Twin spray dryer installation. (By courtesy of Niro Atomizer.) CHEMICAL AND PROCESS ENGINEERING SERIES Spray Drying An Introduction to Principles, Operational Practice and Applications K. MASTERS LEONARD HILL BOOKS LONDON AN INTERTEXT PUBLISHER Published by Leonard Hill Books a division of International Textbook Company Limited 158 Buckingham Palace Road, London SWI W9TR, and 24 Market Square, Aylesbury, Bucks © K. Masters 1972 All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, recording or otherwise, without the prior permission of the copyright owner. First published 1972 ISBN 0 249 44093 8 c Printed in Great Britain by J. W. Arrowsmith Ltd To My Loving Wife, Ben to for her patience and understanding during the many long months of writing, and for her crowning the completion of the book with a supreme gift, Caroline, a sister for Stephen. Preface The importance of spray drying, as illustrated by the rapid expansion of spray drying facilities in all regions of industry, has not been reflected in literary coverage of developments in industry: I have long felt a book dealing specifically with the spray dryer operation is long overdue, In all standard text books and handbooks on chemical and mechanical engineering, spray drying has been restricted to limited coverage under the section headed 'Drying', and in most of these cases coverage consists of a few paragraphs following detailed handling of the more traditional drying operations, for example, tray, rotary and drum drying. This, tdo';Carii be said of books dealing specifically with drying where the text on spray rying is general in nature. * The true status of spray drying has not been truly voice of applications being varied—ranging from low prodUction - rates,m the most delicate pharmaceutical operations to high tonnage- Procinction :;:t1 inorganic chemicals. The purpose of this book is toprovide' a:sre erence ., medium covering spray drying principles, equiprnent, operatiOnat practice and applications. By discussing these aspects in various degreeS Ofdetai I hope to focus more attention on spray drying as a highly specialized operation, fully established in many fields of inthistry. The script has been prepared for both personnel associated with spray drying and students of industrial drying. 1 have tried to relate the current knowledge of the subject in practical terms, with worked examples to show that theoretical principles, when backed up by practical experience, can be often applied to predict, assess, and optimize spray dryer performance, to * (a) Publications devoted solely to spray drying: see Marshall (35), Lykov and Lenochik (478;) (b) recent publications containing chapters on spray drying: see Dombrowski and. Munday (30), Williams-Gardner (376), Nonhebel and Moss (479); (c) literature reviews"on spray drying: see Masters (I), McCormick (494). ix X PREFACE select the most suitable dryer designs for a particular application, and to show how limitations in existing designs can be rectified through equipment modification. Theoretical models used to describe the spray dryer operation are not discussed in detail. The majority of important equations are just stated, and not derived. To those readers who wish to study aspects of spray drying in greater depth, adequate references are given. The choice of units for this book presented a difficult decision. In my experience of spray drying installations, personnel concerned with their operation do not use or have not as yet become familiar with the SI units system due to become standard in the mid-seventies, Based upon the practical emphasis intended for the script I decided to maintain existing units, joining in line with the latest editions of standard chemical and mechanical engineering textbooks and handbooks. Many of these established books are either American or English in Origin, thus based upon the British unit systems. However, there are numerous personnel with spray drying interests operating in areas using metric systems. As a compromise I have tried to utilize both systems, by duplicating data where convenient, and by presenting worked examples in either one set of units or the other, Perhaps this is far from ideal, and I expect comment on this decision but I feel this approach will familiarize the text to a greater number of people than had I used one set of units throughout. Most people are familiar with both sets of units, but feel more competent in one than the other, although they possess the ability to convert units quickly. Worked examples have been included in the text to illustrate use of theoretical principles, empirical equations and operation of equipment. Calculations throughout have been conducted using a slide rule or logarithmic tables, items that are readily available to personnel from management to plant operator levels. Only in chapter 7 (example 7.4) dealing with droplet motion in air was a computer used to eliminate the need to rework constantly a given equation. The writing of this book would not have been possible without the cooperation of the management of Aktieselskabet Niro Atomizer, Copenhagen, (N.A.), and permission to use much of the pictorial material owned by N.A. I wish to put on record my indebtedness to the late Dr. K. Nielsen, who as Head of the Research and Development Department of N.A. encouraged the commencement of the project, and who made available to me an extensive literature survey on spray drying. I also wish to acknowledge the help of so many of my colleagues, whose critique of the text proved so useful in the final preparation of the text for the publisher. All I duly thank. Certain of my colleagues assisted so generously that special thanks are due ; Dr. S. Hovmand, Mr. M. Petersen, for their assessment and suggestions in the first eleven chapters, Mr. Aa, PREFACE xi Moller for his opinions on atomization, Mr. M. Troldborg, whose experience in the field of auxiliary equipment and operational practice I drew heavily upon, Mr. J. Due Jensen for his unselfish assistance in tabulating patent coverage of spray drying, Messrs. E. Houghton-Larsen, H. Justesen, and J. Storm for their invaluable suggestions for improving the section on spray drying operations, last but not least Mr. J. Pilegaard for the services of the Information Department. I wish to express my thanks to my wife and sister who assisted with the preparation of the text, and to all the secretaries, who typed the text so well, no mean task dealing with a tongue far removed from their native Danish. My thanks also go to the ladies who assisted in preparing drawings, especially Mrs. Lundgaard on whom the bulk of the work fell. While acknowledging such assistance, I must emphasize that the interpretation of spray drying presented here is solely mine, and does not necessarily agree with the official view of my employer (N.A.). It is hoped that my handling of the script encourages greater use of the spray drying operation and that, by providing a reference book, I have helped fill the literature gap that exists as far as spray drying is concerned. If these goals are achieved, the energies expended will be fully rewarded, since there can be no disputing that spray drying today is a subject in its own right. Spray drying is a relatively new technique, but is already broad in scope. The selection of material had to be a matter of personal choice. However, to those readers who feel the text could be enhanced by clarification of any part, or by further addition, I would be grateful to hear their suggestions. K. Masters Skovlunde Denmark 1972 Contents Preface List of figures List of tables Introduction ix xxv xxxiii 1 SECTION 1—BASIC PRINCIPLES, DEFINITIONS I SPRAY DRYING FUNDAMENTALS 2 REPRESENTATION OF SPRAYS 2.1 Terminology 2.1.1 Droplet 2.1.2 Particle 2.1.3 Agglomerate 2.1.4 Size 2.1.5 Particle shape 2.1.6 Size distribution 2.1.7 Mean size 2.2 Methods of Data Presentation 2.2.1 Tabular form 2.2.2 Graphical form (a) histograms (b) size frequency curves (c) cumulative plots 2.3 Analysis of data 2.3.1 Mean diameters (a) most frequent diameter (b) arithmetic mean diameter 11 23 23 23 23 23 25 25 25 25 26 27 27 27 27 28 28 28 29 29 X1V CONTENTS (c) geometric mean diameter (d) harmonic mean diameter (e) median diameter 2,3.2 Distribution functions (a) normal distribution (Gaussian) (b) log-normal distribution (c) square root normal distribution (d) empirical distribution functions (i) Nukiyama–Tanasawa distribution (ii) Rosin–Rammler distribution (iii) upper limit function 2.3.3 Mean droplet diameter transformations 3 DRYING TERMS AND PRINCIPLES 3.1 Common Terms and Principles 3.2 Applying the Psychrometric Chart to the Spray Drying Process 4 PERFORMANCE OF SPRAY DRYERS 4.1 Introduction 4.2 Heat and Mass Balances over Spray Dryers 4.3 Dryer Efficiency 4.4 Residence Time in Drying Chamber 5 EQUIPMENT INCORPORATED IN SPRAY DRYERS 5.1 Introduction 5.2 Passage of Air and Product through a Spray Dryer 5.3 Equipment Items Making up a Spray Dryer Layout 5.3.1 Equipment comprising the feed system 5.3.2 Atomizer 5.3,3 Equipment comprising the supply air system 5.3.4 Air disperser and drying chamber 5,3.5 Equipment for separation and recovery of product from exhaust air 29 30 30 33 33 34 34 35 35 35 37 38 42 42 47 54 54 55 59 62 65 65 65 66 66 68 70 72 78 SECTION II—THE PROCESS STAGES OF SPRAY DRYING 6 ATOMIZATION 6.1 Introduction 6.2 Basic Mechanism of Atomization 6.3 Classification of Atomizers 6.4 Application of Basic Mechanisms to Commercial Atomizer Conditions 6.5 Rotary Atomization 6.5.1 Introduction 6.5.2 Flat smooth disc atomization (vaneless) 87 87 87 91 92 93 93 93 6.6 CONTENTS XV (a) flow over smooth flat vaneless discs (b) droplet size from smooth flat vaneless discs 6.5.3 Wheel atomization (atomizer wheels) (a) introduction (b) flow over a vaned wheel (i) radial velocity (ii) tangential velocity (iii) resultant release velocity (iv) angle of liquid release (c) effect of operating variables on droplet size (i) effect of liquid feed rate on droplet size (ii) effect of peripheral speed on droplet size (iii) effect of liquid viscosity on droplet size (d) prediction of mean droplet diameter and spray size distribution (i) mean droplet diameter (ii) size distribution (iii) weight distribution of sprays (e) atomizer wheel performance during spray drying (i) air pumping effects (ii) drying air entry (iii) particle shape change (f) atomizer design requirements (i) atomizer drive (ii) liquid distributor (iii) atomizer wheels (g) applications of atomizer wheels 6.5.4 Disc atomization (vaneless bowls, cups, plates) (a) introduction (b) fluid flow over vaneless discs —radial velocity —tangential velocity (c) droplet size prediction (d) performance of vaneless discs (e) applications of vaneless discs Nozzle Atomization 6.6.1 Introduction 6.6,2 Centrifugal pressure nozzle (a) theoretical principles (b) spray patterns (c) fluid flow from centrifugal pressure nozzles (d) nozzle operating characteristics 97 100 100 100 102 103 104 104 104 105 108 109 112 113 114 118 126 127 127 129 130 135 135 141 142 148 148 148 150 151 151 152 154 157 158 158 159 159 162 165 170 XV1 CONTENTS (i) relation between flow rates, pressure and density (ii) spray angle (iii) effect of operating variables on droplet size —effect of capacity on droplet size —spray angle and droplet size —effect of pressure on droplet size —effect of feed viscosity on droplet size —effect of surface tension on droplet size —effect of orifice size on droplet size (iv) droplet size distribution (e) prediction of nozzle performance (f) prediction of mean droplet size of sprays from centrifugal pressure nozzles (g) nozzle operating features and nozzle applications (h) nozzle assemblies for commercial use 6.6.3 Pneumatic (two-fluid) nozzle atomization (a) theory (b) design features (c) droplet release and spray angle (d) spray characteristics (e) effect of variables on droplet size (i) effect of air–liquid ratio (ii) effect of relative velocity on droplet size (iii) effect of viscosity on droplet size (iv) effect of air density on droplet size (f) prediction of mean droplet size (i) Nukiyama–Tanasawa equation (ii) Gretzinger–Marshall equation (iii) Kim–Marshall equation (iv) Kim–Marshall equation (three-fluid nozzle atomizer) (g) comparison between the spray characteristics of two- and three-fluid nozzles (h) pneumatic nozzle assemblies and their operation (i) advantages and disadvantages of pneumatic nozzles (j) applications 6.6.4 Rotating pneumatic cup atomizers (a) introduction (b) effect of variables on droplet size (c) prediction of mean droplet size 170 170 171 171 172 172 173 174 174 174 175. 182 188 193 196 196 197 199 200 201 201 202 202 202 202 206 211 217 221 221 222 227 228 229 229 231 232 CONTENTS XVii (d) prediction of droplet size distribution 6.7 Sonic Atomization 6.8 Atomizer selection 7 SPRAY-AIR CONTACT (MIXING AND FLOW) 7.1 Introduction 7.2 General Principles 7.3 Droplet Trajectory Characteristics 7.3.1 From rotary atomizers (atomizer wheels) 7.3.2 From nozzle atomizers 7.4 Droplet Moverhent in Drying Chambers 7.4.1 Droplet release velocities 7.4.2 Droplet deceleration (a) from rotary atomizers (b) from nozzle atomizers 7.4.3 Terminal velocity (spherical droplets) 7.4.4 Droplet movement : distance–time relationships (a) droplet movement in non-rotating air (i) motion from rotary atomizers (ii) motion from nozzle atomizers (b) droplet movement in rotating air (i) large diameter chambers (ii) small diameter chambers 7.4.5 Product deposition on chamber wall (a) in small chambers (b) in large chambers 8 DRYING OF DROPLETS/SPRAYS 8.1 Introduction 8.2 Evaporation of Pure Liquid Droplets 8.2.1 Evaporation of single droplets (a) droplet evaporation under negligible relative velocity conditions (b) droplet evaporation under relative velocity conditions (c) evaporation under high air temperature conditions 8.2.2 Evaporation of sprays of pure liquid droplets 8.3 Evaporation of Droplets Containing Dissolved Solids 8.3.1 Evaporation of single droplets (a) vapour pressure lowering effect (b) effect of dried solid formation in droplets (c) droplet evaporation times 8.3.2 Evaporation of sprays containing dissolved solids 8.4 Evaporation of Droplets Containing Insoluble Solids 233 234 235 241 241 247 249 249 251 251 251 252 252 253 256 261 261 261 267 271 271 273 274 275 276 279 279 281 282 282 284 293 297 302 302 302 303 305 309 310 XViii CONTENTS 8.5 9 Drying in Media Other than Air 8.5.1 Drying in gases 8.5.2 Drying in superheated vapours 8.5.3 Drying in superheated steam 8.6 Dried Product Properties on Completion of Drying 8.6.1 Effect of operating variables on product properties (particle size and bulk density) (a) effect of feed rate (b) effect of feed solids (c) effect of feed temperature (d) effect of surface tension (e) effect of inlet drying temperature (f) effect of spray/air contact velocity 8.6.2 Formation of hollow particles 8.7 Size Differences between Product before and after Drying 8.7.1 Procedures to predict dried particle size distribution (a) graphical method (b) mathematical method 8.8 Size Distributions of Wet Sprays and Resulting Dried Particles SEPARATION AND RECOVERY OF DRIED PRODUCT FROM AIR 9.1 Introduction 9.2 Selection of Equipment for Separating Powder from Exhaust Drying Air CONTENTS 313 314 314 315 316 11 316 316 316 316 317 318 319 319 319 320 320 320 322 324 324 327 10 CONTROL SYSTEMS 1 0, 1 Control System (based upon feed rate regulation) 10.2 Control System (based upon heat input regulation) 10.3 Feed System Controls 10.3.1 Systems for rotary atomizers 10.3.2 Systems for nozzle atomizers 10.4 Interlocks 10.5 Fully Automatic Spray Dryers 10.5.1 Programmed start-up 10.5.2 Full automation of spray dryer and feed pretreatment 10.6 Precaution Against Fire and Explosion 10.7 Control Systems for Preventing Fire/Explosion Conditions in Deposit Formations 335 336 338 339 339 339 340 341 341 344 347 349 352 352 352 356 357 357 364 365 371 378 378 380 384 385 385 386 388 390 392 393 398 SECTION IV—SURVEY OF AUXILIARY EQUIPMENT 12 SECTION III—OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS 11.1 Determination of Air Flow 11.1.., Supply air to dryer 11.1.2 Exhaust air leaving dryer 11.2 Measurement of Air Velocity in Ducts 11.2.1 Pitot tube measurement 11.2.2 Orifice/venturi measurements 11.2.3 Anemometer measurements 11.3 Determination of Powder Loading in Air Flows 11.3.1 Manual sampling (a) cyclone probe (B.C.U.R,A.) method (b) internal filter thimble method (c) external filter thimble method 11.3.2 Continuous sampling (a) light intensity methods (b) electrostatic methods (c) CEGRIT sampler 11.3.3 Determination of dried product losses from mass balance techniques 11.3.4 Reducing powder losses from spray dryer exhaust systems 11.4 Assessing Acoustic Environment (Noise Levels) 11.5 Measurement of Droplet and Particle Size xix SURVEY OF AUXILIARY EQUIPMENT 12.1 Air Heaters 12.1.1 Steam air heaters 12.1.2 Fuel oil air heaters 12.1.3 Gas air heaters 12.1.4 Electric air heaters 12.1.5 Liquid phase air heaters (thermal fluid heaters) 12,2 Fans 12.2.1 Fan requirements on a spray dryer layout 12.2.2 Fan parts and principles 12.2.3 Fan characteristics 12.2.4 Fan laws 12.2.5 Fan efficiency 12.2.6 Fan horsepower 12.2.7 Effect of altitude on fan performance 12.2.8 Fan mounting 12.2.9 Fan noise 401 401 401 404 406 406 406 407 408 408 410 411 414 415 418 418 418 XX CONTENTS CONTENTS 12.2.10 Fan selection Mechanical Powder Separators 12.3.1 Dry collectors (a) dry cyclones (i) cyclone performance (ii) overall cyclone efficiency (iii) pressure drop over cyclones (iv) cyclone layouts (b) bag filters (i) principles (ii) bag filter designs (iii) bag filter performance (iv) pressure drop over bag filters (v) bag filter fabrics (vi) use of bag filters (vii) bag filter layouts (c) electrostatic precipitators (i) principles (ii) performance of electrostatic precipitators (d) gravity settlers 12.3.2 Wet collectors (a) wet scrubbers (i) principles (ii) wet scrubber designs 12.3.3 Powder removal from mechanical separators (dry collectors) (a) hoppers (b) powder removal valves 12.4 Pneumatic Powder Conveying 12.4.1 Principles 12.4.2 Pneumatic conveying systems in practice 12.4.3 Operational difficulties with pneumatic conveying systems 12.5 Pumps 12.5.1 Pump duties in spray dryers 12.5.2 Pump types and uses 12.6 Washing Equipment 12.3 419 419 420 420 422 424 427 431 432 432 432 435 436 436 436 437 437 437 438 439 440 440 440 443 445 445 445 451 451 455 456 458 458 460 460 SECTION V—APPLICATIONS OF SPRAY DRYING IN INDUSTRY 13 14 APPLICATIONS OF SPRAY DRYING (A LITERATURE SURVEY) APPLICATIONS IN THE CHEMICAL INDUSTRY 465 498 Plastics, Resins 14.1.1 Polyvinylchloride (P.V.C.) 14.1.2 Resins 14.1.3 SBR lattices 14.2 Ceramic Material 14.2.1 Wall tile and floor tile ceramics 14.2.2 Oxide ceramics 14.2.3 Plastic bodies 14.2.4 Glass 14.2.5 Carbides 14.3 Washing Powder 14.3.1 Heavy duty detergents 14.3.2 Light duty detergents 14.3.3 Soap powder 14.3.4 Soda products 14.3.5 Bleach powders 14.3.6 Optical brighteners 14.3.7 Perfumes for washing powder 14.4 Pesticides 14.4.1 Herbicides 14.4.2 Fungicides 14.4.3 Insecticides 14.5 Dyestuffs—Pigments 14.5.1 Titanium dioxide 14.5.2 Kaolin (china clay) 14.6 Fertilizers 14.6.1 Ammonium nitrate 14.6.2 Ammonium phosphate 14.6.3 Superphosphates 14.7 Mineral Ore Concentrates 14.7.1 Sulphide ores 14.7.2 Iron ores 14.7.3 Cryolite 14.8 Inorganic Chemicals 14.9 Organic Chemicals 14.10 New and/or Specialized Applications in the Chemical Industry 14.10.1 Abrasives 14.10.2 Catalysts 14.10.3 Cement 14.10.4 Metal powders 14.10.5 Sodium carbonate 14.1 XXI 499 499 501 502 502 505 506 509 510 510 511 512 514 515 515. 517 517 518 518 520 521 521 521 522 523 526 526 528 530 533 535 535 537 537 537 538 539 539 540 542 543 xxii 15 CONTENTS 14.10.6 Sodium hydroxide 14.10.7 Titanium tetrachloride APPLICATIONS IN THE FOOD INDUSTRY 15.1 Milk Products and Eggs 15.1.1 Milk products (a) skim milk (b) whole milk (c) whey (d) fat-enriched milk (milk replacer) (e) sodium caseinate (f) baby foods (g) coffee/tea whiteners (h) cheese (i) ice-cream mix (j) high fat powder for bakery use (also butter) (k) buttermilk 15.1.2 Eggs 15.2 Beverages, Flavouring Compounds, Meats, Protein from Vegetable Sources 15.2.1 Beverages (a) instant coffee (b) instant tea 15.2.2 Flavouring compounds 15.2.3 Meats 15.2.4 Edible protein from vegetable sources (a) soya beans (b) peanuts (c) potato fruitwater 15.3 Fruits and Vegetables 15.3.1 Fruits (a) tomatoes (b) banana (c) citrus fruits (d) soft fruits (e) other fruits 15.3.2 Vegetables (a) beetroot (b) asparagus (c) peas (d) mashed potato 15.4 Carbohydrates 15.4.1 Corn products CONTENTS 543' 543 545 545 545 547 553 556 560 562 564 564 564 565 565 565 566 568 568 568 572 572 573 573 573 575 575 576 576 577 581 583 583 583 584 584 584 584 584 585 585 16 17 18 15.4.2 Wheat gluten 15.4.3 Sugar products APPLICATIONS IN THE PHARMACEUTICAL-BIOCHEMICAL INDUSTRY 16.1 Introduction 16.2 Enzymes 16.3 Antibiotics 16.4 Sera, Vaccines, Plasma and Substitutes 16,5 Micro-organisms 16.6 Yeast 16.6.1 Production of food yeast from sugar cane molasses 16.6.2 Active yeast (brewers') 16.6.3 Barley powder 16.7 Vitamins 16.8 Pharmaceutical Gums APPLICATIONS IN INDUSTRIES UTILIZING CHEMICALS FROM TIMBER 17.1 Applications in the Tannin Industry 17.1.1 Manufacture of tannin from woods 17.1.2 Manufacture of tannin from barks 17.1.3 Manufacture of tannin from fruits 17.2 Applications in the Cellulose Industry 17,2.1 Concentrated sulphite waste liquor 17.2.2 Li gn osulphonates APPLICATIONS IN THE OFFAL AND FISH INDUSTRIES 18.1 Spray Drying of Slaughterhouse By-products 18.1.1 Blood 18.1.2 Glands and tissues 18.1.3 Gelatin and glue 18.1.4 Excreta 18.2 Spray Drying of Fish Wastes 18.2.1 Stickwater (fish solubles) 18.2.2 Whole fish meal 18.2.3 Normal fish meal 18.2,4 Edible fish flour 18.2.5 Fish hydrolysates SECTION VI—APPENDICES, NOMENCLATURE, REFERENCES, INDEX 19 APPENDICES A.1 Conversion Factors XXiii 586 586 587 587 592 594 595 597 597 598 600 600 600 600 602 602 602 603 604 604 604 604 606 606 606 609 609 609 609 609 611 612 612 612 617 617 XXiV CONTENTS A.2 Temperature Conversion Tables A.3 Properties of Dry Air A.4 Vapour Pressures of . Water A.5 Psychometric Charts 1. Normal temperatures 2. Elevated temperatures A.6 Humid Heat-Humidity Relation for Air-Water Vapour System at Atmospheric Pressure A.7 Temperature-Latent Heat of VaporizationTemperature Relation (Water) A.8 Liquid Flow over Vaned Atomizer Wheel A.9 Thermal Conductivity of some Insulation Materials A.10 Sieve Sizes A.11 Particle Size Distributions of Standard Powder Grades for Use when Optimizing Cyclone Product Loading 20 NOMENCLATURE 21 REFERENCES 22 hsTDEX 620 622 623 624 624 625 626 List of Figures 627 628 630 631 633 634 640 654 Frontispiece Twin spray dryer installation 0.1 The process stages of spray drying 0.2 Layouts of spray dryers and associated suspended particle processing equipment involving atomization 0.3 Dried powder forms produced by spray drying 1.1 The features of the process stages involved in spray drying 1.2 Equipment involved in a standard spray dryer layout 1.3 Atomizers in operation 1.4 Product-air flow in spray dryers 1.5 Air temperature distributions in co-current and counter-current flow spray dryers 1.6 Product discharge from co-current flow spray dryers with a rotary atomizer 2.1 Range of droplet/particle sizes obtained in spray drying operations 2.2 Size distribution of droplets and particles 2.3 Droplet size distribution represented in histogram form 2.4 Frequency and cumulative curves showing mean droplet diameter values in example 2.1 2.5 Log normal distribution on probability paper 2.6 Droplet size distribution of a centrifugal pressure nozzle (grooved core swirl) conforming to a square root normal distribution 2.7 Rosin-Rammier size distribution 2.8 Comparisons of log normal, square root normal and upper li mit distributions for a centrifugal pressure nozzle Size data for example 2,2 2.9 3.1 Graphical relation between common drying terms XXV 3 5 7 12 13 15 17 18 20 24 26 27 30 35 36 37 38 41 43 XXVI LIST OF FIGURES 3.2 Two applications of the psychrometric chart in spray drying 3.3 Drying characteristics of droplets during spray drying 4.1 Effect of feed solids content on dryer heat load 4.2 Dryer data for calculation of heat and mass balances 4.3 Drying process represented in example 4.2 5.1 Product and air passage through a spray dryer 5.2 Spray dryer layouts with rotary and nozzle atomization 5.3 Feed system involving a feed preheater 5.4 Basic types of atomizers 5.5 Atomizer positioning in drying chamber 5.6 Co-current flow dryers 5.7 Air disperser types creating rotary air flow around atomizer 5.8 Counter-current flow dryer 5.9 Mixed flow dryers 5.10 Primary product discharge from drying chambers 5.11 Total product discharge from drying chambers 5.12 Drying chamber wall cooling 5.13 Equipment for separation and recovery of airborne powders 5.14 Dry product conveying systems on spray dryers 6.1 Ohnesorge chart showing liquid jet disintegration as a function of Reynolds number 6.2 Classification of atomizers 6.3 Mechanisms of atomization 6.4 Mechanisms of atomization (represented photographically) 6.5 Atomization mechanism for rotating discs 6.6 Liquid flow to and from edge of atomizer wheel 6.7 Effect of feed rate on mean droplet size for atomizer wheel 6.8 Effect of atomizer wheel peripheral speed on mean droplet size 6.9 Effect of atomizer wheel speed of rotation on mean droplet size (aqueous sprays) 6.10 Effect of feed viscosity on wheel atomization 6.11 Curves for prediction of spray size distributions from atomizer wheels after the Herring-Marshall relation 6.12 Size relationship between droplet and particle in example 6.4 6.13 Spray weight distribution from rotary atomizers 6.14 Air flow through vaned atomizer wheel due to air pumping effects 6.15 Pressure distribution at vaned atomizer wheel due to air pumping effects 6.16 Arrangement for supplying cool air to atomizer wheel 6.17 Positioning of rotary atomizer in relation to air disperser LIST OF FIGURES 48 49-50 55 56 61 66 67 69 70 71 73 74 75 76 77 79 80 81 83 89 91 95 96 98 102 108 109 111 113 119 125 126 128 129 130 131 XXVii 6.18 Atomizer drives 136 6.19 Rotary atomizer drives for atomizer wheels 139 6.20 Rotary atomizer with variable speed control through a fluid coupling 140 6.21 Spindle pressurizing 141 6.22 Positioning of liquid distributor with atomizer wheel 142 6.23 Liquid distributor designs 143 144 6.24 Designs of vaned atomizer wheels 6.25 Abrasive wear on vaned atomizer wheel 146 6.26 Atomizer wheel with bushings for abrasive and corrosive 147 feeds 6.27 Disc atomizer (plate type, multiLtier) 149 6.28 Disc atomizer (cup type) 149 155 6.29 Effect of feed rate on mean droplet size from disc atomizer 6.30 Effect of atomizer disc speed on mean droplet size 156 6.31 Effect of number of plate tiers of a disc atomizer on particle size distribution 157 158 6.32 Size distributions from atomizer wheels and discs 6.33 Centrifugal pressure nozzles 160 6.34 Inserts for generating liquid rotation within centrifugal 161 pressure nozzles 161 6.35 Centrifugal pressure nozzle construction 162 6.36 Spray angle characteristics 6.37 Velocity diagram for liquid flow from a centrifugal pressure 166 nozzle 168 6.38 Variation of feed rate with square root of nozzle pressure 6.39 Feed rate, feed pressure, feed density ratios for centrifugal pressure nozzles 171 6.40 Effect of variables (feed rate, feed viscosity) on Sauter mean 172 diameter 173 6.41 Effect of feed viscosity on spray droplet size distribution 6.42 Typical droplet size distribution of a centrifugal pressure 174 nozzle used in spray drying 175 6.43 Nozzles with tangential feed entry 176-7 6.44 Nozzle dimensioning relations after Doumas and Laster 6.45 Nozzle dimensioning relations after Dombrowski and Hasson 180-1 6.46 Range of orifice sizes per given nozzle body for optimum 189 atomization conditions 6.47 Performance of centrifugal pressure nozzles (rated on 192 aqueous feed) on 42 % TS skim milk concentrate 194 6.48 Positioning of nozzles in relation to air disperser 198 6.49 Designs of pneumatic nozzle heads XXViii LIST OF FIGURES 6.50 Effect of nozzle operating variables on spray mean droplet size 6.51 Nozzle designs used in pneumatic nozzle investigations 6.52 Nukiyama-Tanasawa plot for converging two-fluid nozzles operating on aqueous feed 6.53 Nukiyama-Tanasawa distribution (a typical plot) 6.54 Gretzinger-Marshall plot for converging two-fluid nozzles 6.55 The Gretzinger-Marshall droplet size relation expressed as a nomograph 6.56 Plot of film thickness against feed rate 6.57 Dimensions of nozzle design in example 6.15 6.58 Size distribution for two-fluid nozzle (after Kim-Marshall) 6.59 Piping connections for pneumatic nozzles 6.60 Feed systems for pneumatic nozzles (two-fluid) 6.61 Feed and air distribution rings for pneumatic nozzles 6.62 Two-fluid paste nozzle with screw feeder 6.63 Atomization mechanism for a pneumatic cup atomizer 6.64 Pneumatic cup atomizer head 6.65 Pneumatic cup atomizer and air disperser positioning in drying chamber 6.66 Particle size distributions of rotary and nozzle atomizers operating on silica and alumina based catalysts 6.67 Modifications of the atomizer drive to handle liquid, powder or liquid-powder feeds 7.1 Air disperser for rotary atomizers (in co-current flow dryers) 7.2 Ceiling air disperser with rotary (vaned wheel) atomizer in co-current flow dryer 7.3 Air disperser for nozzle atomizers in co-current flow dryers 7.4 Air disperser for counter-current flow dryers 7.5 Air dispensers and atomizers in mixed flow dryers 7.6 Plot of R f I pv 2 against Reynolds number for spherical particles 7.7 Plot for CD Re 2 against Re for spherical particles 7.8 Plot of drag coefficient against Reynolds number 7.9 Areas of likely wall impingement of partially dry product in small dryers 7.10 Impingement area control by air disperser adjustment in large dryers with rotary atomization 8.1 Drying rate curve 8.2 Configuration of droplet evaporating in high temperature surroundings 8.3 Estimation of temperatures of droplets containing dissolved solids LIST OF FIGURES XXiX 203 204 207 208 211 212 214 217 220 223 224 225 226 230 231 232 236 239 243 244 245 246 247 250 257 260 277 278 280 295 302 Effect of crust properties on evaporation times Characteristics of droplet undergoing drying (drying air above boiling point) 8.6 Characteristics of droplet undergoing drying (drying air below boiling point) 8.7 Temperature profile in example 8.4 8.8 Temperature of droplet undergoing evaporation in air and superheated vapour 8.9 Effect of feed concentration on bulk density of spray dried products 8.10 Effect of inlet drying air temperature on bulk density of spray dried products 8.11 Graphical determination of size distribution of dried product from that of wet spray 9.1 Product discharge from conical and flat chamber bases 9.2 Exhaust ducts layouts with primary product discharge from conical chamber base 10.1 Outlet air temperature chart for dryer operation under manual and automatic control 10.2 Control system A: outlet temperature control by regulation of feed rate, inlet temperature control by regulation of fuel combustion rate 10.3 Control system B: outlet temperature control by regulation of fuel combustion rate, manual regulation of feed rate 10.4 Control system for pressure nozzles (control system A) 10.5 A combined block and schematic diagram for a fully automated spray dryer 10.6 Automatic feed solids content measuring equipment used in fully automatic spray drying plant in the dairy industry 10.7 Block diagrams for automatic control of combined evaporator and spray dryer systems 11.1 Pitot tube with inclined manometer 11.2 Positions for velocity measurement by pitot tube in circular duct (equal duct areas) 11.3 Positions for velocity measurement by pitot tube in rectangular ducts (equal duct areas) 11.4 Pitot tube pressure difference (P D )-air velocity nomograph 11.5 Permissible positions in ducts for pitot tube measurements and air sampling 11.6 Location of venturi and orifice meters in inlet drying air duct 11.7 Positions selected in spray dryer layout for various air flow measurements illustrated in example 11.2 8.4 8.5 304 306 307 312 315 317 318 321 325 326 336 337 339 340 342 344 346 357 359 360 361 363 364 366 XXX LIST OF FIGURES 11.8 Inlet duct zoning for anemometer measurements in example 12.2 367 11.9 Flow conditions at sampling nozzle 372 11.10 Effect of incorrect sampling rate on observed powder loading in air stream 373 11.11 Basic layout for sampling powder laden air 373. 11.12 Velocity distributions and profiles existing in ductwork arrangement 375 11.13 Layout of B.C.U.R.A. cyclone probe for sampling powder laden air 378 11.14 Layout for measuring powder loadings in air flows using the filter thimble sampler with orifice plate for sampling rate control 382 11.15 Filter thimble sampler for measuring powder loadings in air flow 383 11.16 Layout for measuring powder loadings in air flows using the filter thimble sampler with gas meter for sampling rate control 384 11.17 Layout for external filter thimble equipment 385 11.18 Measuring powder-air loadings by light intensity methods 386 11.19 Layout for sampling equipment based upon contact electrification 387 11.20 The CEGRIT sampler for measuring powder loading in air flows 389 11.21 Sound pressure level against frequency plot for assessing acoustic environment of equipment 395 12.1 Relation between saturated steam pressure and temperature 402 12.2 Indirect air heaters 404 12.3 One- and two-fan spray dryer layouts 407 12.4 Principle parts of a centrifugal fan 409 12.5 Performance curves characteristics for radial, forward curving, and backward curving blades 410 12.6 Fan performance chart for example 12.1 411 12.7 Relation between fan horsepower and installed fan motor horsepower 415 12.8 Basic designs of industrial cyclones 421 12.9 Theoretical and actual grade efficiency curves 423 12.10 Grade efficiency curve for cyclones specified in example 12.7 424 12.11 Measuring pressure drop over a cyclone 427 12.12 Cyclone layout in parallel 431 12.13 Grade efficiency curve for a standard bag filter 432 12.14 Designs of bag filters 434 LIST OF FIGURES xxxi 12.15 Electrical power system for an electrostatic precipitator 438 12.16 Grade efficiency curve for a dry electrostatic precipitator 439 12.17 Gravity settler 440 12.18 Designs of wet scrubber 441 12.19 Grade efficiency curves for wet scrubbers 442 12.20 Hoppers 446 12.21 Powder removal valves 448-9 12.22 Vortex air-lock 451 12.23 Powder removal from cyclones, equipment in practice 452 12.24 Pneumatic conveying layouts 453 12.25 Determination of air rate and duct size for pneumatic conveying 455 12.26 Classification of pumps 458 12.27 Feed system layouts 459 12.28 Automatic washing equipment 461 14.1 Examples of unit operations associated with wet preparation as compared with spray drying process 502 14.2 Spray dryers for ceramic pressbody 503 14.3 Micro-photographs of pressbody 504 14.4 Particle size distributions of wall tile material produced by atomizer wheel and pressure nozzle atomization 505 14.5 Spray dried steatite 506 14.6 Flow diagram for production of ferrite by spray drying 508 14.7 Flow diagram for preparation of spray dried jiggering bodies 510 14.8 Flow diagram for spray drying carbides in closed cycle 511 14.9 Flow diagram for spray drying of detergent formulations 516 14.10 A semi-closed cycle spray dryer for herbicides 520 14.11 Flow diagram for spray drying titanium dioxide 523 14.12 Flow diagram for producing kaolin by spray drying 524 14.13 High tonnage spray dryers on kaolin in Georgia, USA, each producing 15-25 tons per hour 525 14.14 Production of ammonium nitrate prills by spray cooling 528 14.15 Flow diagram for production of mono-ammonium phosphate by spray drying 529 14.16 Flow diagrams for the production of double superphosphate fertilizers 532 14.17 De-watering operations for flotation concentrates 533 14.18 Flow diagram for spray drying flotation concentrates 534 14.19 Twin spray dryer complex in Western Australia, producing 536 bone dry nickel-concentrate 14.20 Flow diagram for manufacture of cement utilizing spray 541 drying XXXii LIST OF FIGURES 15.1 Products derived from milk 15.2 Spray dryer layouts for dairy products 15.3 Forms of spray dried skim milk powder 15.4 Rewet instantizer (shown with agglomerating tube mounted) 15.5 Spray dryer with vibro-fluidizer for instant skim milk, whole milk, milk replacer, ice-cream mix, cheese, cream powders 15.6 Processing stages in the spray drying of whey 15.7 Spray dryer producing non-caking whey powder 15.8 Flow diagram for the production of spray dried sodium caseinate 15.9 Processing diagram for production of egg powders 15.10 Flow diagram for production of instant coffee powder by spray drying 15.11 Process stages in the production of protein from vegetable sources using spray drying 15.12 Flow diagram for the production of potato protein by spray drying 15.13 Flow diagram for the production of tomato powder by spray drying 15.14 Dehumidified enclosed band conveyor for cooling spray dried tomato powder 15.15 Processing stages in production of banana powder by spray drying 16.1 Single stage aseptic spray drying system 16.2 Two stage aseptic spray drying system 16.3 Flow diagram for aseptic spray drying plant with two-fluid atomization 16.4 Spray dryer with rotary atomizer for aseptic drying 16.5 Flow diagram for the production of fodder yeast from molasses 18.1 Stages in the processing of animal blood by spray drying 18.2 Flow diagram for the production of dried fish solids A.5 Psychrometric charts for air-water vapour system at atmospheric pressure A.6 Humid heat-humidity relation for air-water vapour system at atmospheric pressure A.7 Latent heat of vaporization-temperature relation (water) A.8 Liquid flow over vaned atomizer wheel 546 548 550 554 555 557 559 List of Tables 563 566 569 574 576 578 580 582 589 591 593 595 599 607 610 624-5 626 627 628 2.1 Calculation of mean diameters in example 2.1 2.2 Mean diameters based upon number, surface and volume 2.3 Distribution functions 2.4 Mean diameter transformation 2.5 Data for example 2,2 2.6 Calculation of Sauter mean diameter in example 2.2 5.1 Advantages and disadvantages of dry and wet powder recovery 6.1 Prediction of droplet size following liquid jet disintegration 6.2 Droplet size prediction for smooth flat vaneless discs 6.3 Values of A = 0*(1) 2 ) 112 6.4 Values of radial velocity and liquid film thickness at edge of vaned atomizer wheel (example 6.1) 6.5 Operating conditions covered by investigators in drawing up equations (6.26-6.31) to predict spray characteristics from atomizer wheels/discs 6.6 Effect of operating variables on droplet size from atomizer wheels 6.7 Relation between mean droplet size and wheel speed for different van loadings for low viscous feeds 6.8 Sauter mean diameter predicted from viscosity data (13, 42) (figure 6.10) (a comparison with experimentally determined values) 6.9 Relations to predict spray characteristics from atomizer wheels 6.10 Comparison between experimental and predicted Sauter mean droplet sizes 6.11 Values of constant in equation (6.30) for given dryer size 32 33 34 39 39 40 82 90 101 103 105 106 107 111 113 114 115 116 XXXiV LIST OF TABLES LIST OF TABLES 6.12 Range of operating variables applicable to curves A-E in figure 6.11 6.13 Relations to predict droplet size from vaneless discs 6.14 Correlations to predict mean droplet size from centrifugal pressure nozzles 6.15 Nozzle recommendation: enquiry form 6.16 Key to figure 6.48 6.17 Typical performance of internal mixing type nozzles 6.18 Correlations for predicting droplet size from converging pneumatic nozzles 6.19 Experimental conditions covered by pneumatic nozzle droplet size correlations 6.20 Relationship between dispersion coefficient, Sauter mean diameter and slope of the Nukiyama-Tanasawa plot (6) 6.21 Values for example 6.15 6.22 Values for example 6.16 6.23 Comparison of predicted mean droplet sizes 6.24 Tabulated data showing pneumatic nozzle flexibility 6.25 Correlations for predicting droplet size from pneumatic cup atomizers 6.26 Relation between Sauter mean diameter and maximum spray droplet size 7.1 Relation between Reynolds Number (Re) and drag coefficient (CD ) (for spherical droplet) 7.2 Spray trajectory relations for rotary atomizers 7.3 Values of K factor 7.4 Theoretical droplet trajectories in example 7.3 (from rotary atomizer) 7.5 Theoretical droplet trajectories in example 7.4 (from nozzle atomizer) 8.1 Proposals for the equation Nu (or Sh) = 2.0 + K(Re)x(Pr or Sc) 9.1 117 153 11.1 205 11.2 206 11.3 11.4 209 215 219 220 228 233 12.1 12.2 12.3 12.4 12.5 12.6 13.1 234 13.2 249 251 255 14.1 267 14.2 15.1 16.1 16.2 270 286 Values of the integral f in equation (8.23) J C D Re l * 5 288 Fractional evaporation of aqueous droplets undergoing decelerated motion in dry air (379°F) 8.4 Evaporation times for pure liquid droplets 8.5 Values of fl for different temperature driving forces 8.6 Spray evaporation history 8.7 Evaporation of aqueous droplets in atmospheres of air and superheated steam 289 291 291 300 8.3 on 9.3 9.4 184-5 190 195 200 d(Re) 8.2 9.2 316 XXXV Collection efficiency of primary separators on low and high 328 powder/air loadings Suitability of powder-air separation equipment in spray 330 dryer installations 331 Relative costs of separation equipment in spray drying Dimensions of separation equipment to handle 70 000 m 3 /hr 332 air at 80°C Effect on Pd reading of pitot tube misalignment in the air 360 stream Equipment for determination of powder loading in ducted 377 air flows 379 Efficiency of B.C. U R.A. cyclone Available methods of measuring droplet size distribution of 397 sprays and particle size distribution of dried product 405 Efficiencies of indirect fuel oil air heaters 414 Typical fan efficiencies 425 Data for example 12.7 430 Dimensions of industrial and model cyclones 435 Recommended face velocities for bag filter designs 437 Properties of bag filter fabrics Products suitable for suspended particle processing systems, 471-5 involving atomization Recent patents and patent applications dealing with products 476-97 to which spray drying or spray cooling is applied Particle size distribution of oxide ceramics according to 507 atomizer used 530 Methods of double superphosphate manufacture 553 Properties of ordinary and instant milk powders 594 Uses of spray dried enzymes 598 Relative compositions of fodder yeast and muscular protein Introduction Spray drying is by definition the transformation of feed from a fluid state into a dried form by spraying the feed into a hot drying medium. It is a one step continuous suspended particle processing operation. The feed can be either a solution, suspension or paste. The resulting dried product conforms to powders, granules or agglomerates, the form of which depends upon the physical and chemical properties of the feed and the dryer design and operation. Spray drying is a procedure which in many industries meets dried product specifications most desirable for subsequent processing or direct consumer usage. Intensive research and development during the last two decades has resulted in spray drying becoming a highly competitive means of drying a wide variety of products (1). The range of product applications continues to expand so that today spray drying has connections with many things that touch our daily lives. The extent of this will become apparent during the course of this book. Spray drying has moved into all major industries ranging from production in the most delicate of conditions laid down in food and pharmaceutical manufacture right through to the high-tonnage outputs within such heavy chemical fields as mineral ores and clays. There are many products and articles in use around us each day to exemplify the extensive usage of spray drying. This is apparent if we consider just one aspect of common interest to us all, namely our home living. From foodstuffs to home fittings, spray drying has many associations. Each product requires different powder requirements to be met during manufacture. For example, the housewife may be concerned only with the taste and price of the foodstuffs she buys and the quality of the household aids she uses, but it is most likely one would find a wide range of foodstuffs, equipment and fittings within her home having direct and indirect connections with the spray drying operation. Foodstuffs may well be instant 2 INTRODUCTION coffee, coffee whitener, dried eggs, milk, soups, babyfoods, perhaps even powdered cheese and fruits. These are examples of products with direct connections. Spray dried foodstuffs appeal to the eye, retain nutritive contents and are easy to use, through being readily dry mixed and reconstituted. This is irrespective of their dried forms which are highly diverse. Milk powders can be in agglomerated (instant) form, whereas eggs, soup, coffee whitener have powdery, and fruits granular, forms. Apart from dried foodstuffs that are consumed directly, there are a variety of spray dried products used in cuisine. Examples include condiments (garlic, pimento), flavouring compounds, rennet, and ingredients in biscuits and cakes. Meat, vegetables and fresh fruit are foodstuffs with indirect connections with spray drying. Meat may be from a slaughtered animal reared on feeds based upon spray dried skimmilk, whey or fat enriched milk (replacer). Whereas appearance might not be so crucial here, particle size and consistency must be conducive to animal digestion. All vegetables and fruit can be connected with spray dried fertilizers and pesticides used in cultivation. Here good spreading characteristics are the powder requirements, placing emphasis on particle size distribution and moisture content of the powder. Passing from foodstuffs to general household commodities, many examples can be cited. Perhaps the best known spray drying application is household detergents; but also spray dried soaps and other surface active agents and optical brighteners are available. In the bathroom cabinet spray dried pharmaceutical products, and even cosmetics, are likely to be found. Pharmaceuticals, e.g. antibiotics, are produced under the most aseptic of conditions as finely divided powders, which are often tableted prior to marketing. The spray dried powder form is ideal for rapid assimilation into the body organs. Many cosmetics rely on spray drying to provide constituents in such articles as face powders and lipsticks. Applications to home fittings and furnishings are also extensive. Wall tiling is formed by pressing coloured spray dried clays. Paints contain spray dried pigments. Electrical insulation material is spray dried prior to pressing into parts for electronics and electric power supplies. Also in the electronics field spray dried ferrites enjoy wide use, being found in pressed form in telephones, radio, television, etc. Many household aids are powered by an electric motor with a ferrite rotor. All these pressing operations demand strict particle size distributions that can be met by the spray drying operation. No such survey of spray dried products in the home is complete without mention of (a) plastics, as many household plastic utensils originate from a manufacturing process that includes a spray drying stage; (b) fabrics, as spray dried dyestuffs provide the vivid colours of furnishings and clothing; (c) stationery, as spray drying provides many materials for printing while spray dried kaolin is used in paper making itself ; (d) shoes, bags and leather INTRODUCTION 3 wear as spray dried tannin is closely associated with the curing of leather ; (e) starches, as the extensive processing of this, one of mankind's most basic materials, often includes a spray drying stage. Spray dried starch and its derivatives (sugar, syrup) are widely used in ice cream, confectionary, desserts, jellies, preserves, frozen fruit, soft drinks. In non-food manufacture, spray dried starch is used in textiles, papermaking, printing and adhesives. Examples could go on, but the point has surely been made. The variety of spray dried products illustrates the ability of spray drying equipment to meet a wide range of powder product requirements. Spray drying involves atomization of feed (hereafter aqueous unless stated otherwise) into a spray, and contact between spray and the drying medium (hereafter termed air unless stated otherwise) resulting in moisture evaporation. The drying of the spray proceeds until the desired moisture content in the dried particles is obtained, and the product is then recovered from the air. These four stages are illustrated in figure 0.1. I STAGE I 'ATOMIZATION L _J IR 1 0 AIR STAGE 2 SPRAY-AIR LcONTACT r r - 1 STAGE 4 DRIED POWDER RECOVERY STAGE 3 !MOISTURE EVAPORATION FROM SPRAY - DRYING CHAMBER L .1 U L Figure 0.1, The process stages of spray drying. 4 INTRODUCTION INTRODUCTION The word 'atomization' can be confusing initially. 'Atomization' has no association with atoms and nuclear physics but covers the process of liquid bulk break-up into millions of individual droplets forming a spray. The energy necessary for this process is supplied by centrifugal, pressure, kinetic or sonic effects. During spray—air contact, droplets meet hot air and a rapid moisture evaporation takes place. If the spray drying plant is properly designed the outcome will be dried particles suspended in the drying air, from which an efficient particle removal is essential. Explaining the process through viewing an actual installation can be unrewarding as the spray drying operation cannot be separated into distinct processes for individual viewing. Any form of dryer provides means of moisture removal by the application of heat to the feed product and control of the drying medium humidity. A spray dryer is no exception. Heat is applied as a heated atmosphere and evaporation is promoted by spraying the feed into this atmosphere. Humidity control is by air flow and temperature regulation. Although the vast majority of cases employ hot atmosphere to drive moisture from each spray droplet, there are cases where the delicacy of the operation demands that the drying medium is just warmed over atmospheric temperatures. This is a variation of the basic spray drying concept, and is termed low temperature spray drying. A further variation is to spray the product into freezing air, whereupon the individual droplets are frozen for subsequent moisture removal through sublimation under vacuum. This variation of spray drying is termed spray freeze drying. Should the temperature of the air permit only solidification of the spray droplets, the process is termed spray cooling. A still further variation is to utilize the chamber as a spray reactor. For liquids that react chemically with a given gas to form a new compound, the contacting of gas with liquid in an atomized state gives rise to fast reaction rates because of the large surface area of the droplets. The process is termed spray reaction. The spray drying chamber need not only be used to produce dry products; use as a spray concentrator has long been recognized. In fact the use of drying and concentrating liquids by atomizing techniques can be traced back to a one hundred year old patent (2). The historical background of spray drying has been recently described by Hatfield (130). While most of the spray drying operations utilize a drying medium of air and exhaust the air to atmosphere (open cycle), there are cases where an inert gas, e.g. nitrogen, is used as the drying medium instead of air. The inert gas prevents risk of explosion where flammable or .explosive solvents are involved. The inert gas is constantly re-used in the drying process through re-cycling within a closed system. The evaporated liquid absorbed 5 into the drying gas in the drying chamber is recovered in a scrubber— condenser system. Organic solvents and diluents can thus be evaporated and recovered. For products that form potentially explosive powder—air mixtures in the chamber of an open cycle drying system or where the exhaust air contains pollutants or odours, the semi-closed drying system can be used. In the former case, explosions are prevented by lowering the 0 2 content in the drying chamber by control of the combustion air to a direct air heater and exhaust air bleed (see page 522). In the latter case the pollutants and odours in the exhaust air bleed, which forms a small percentage of dryer air requirement, are deactivated prior to atmospheric emission. The spray drying layout and its possible modifications to closed cycle and semi-closed spray drying, spray cooling, spray reaction and spray freeze drying are illustrated in figure 0.2. In introducing the subject, emphasis has been given to the ability of the spray drying process to handle a wide range of products, and meet the combustion air ine t gas make-up hot heater DRYING CHAMB ER DRYING CHAMBER p A OPEN CYCLE B CLOSED CYCLE C SEMI-CLOSED CYCLE SPRAY DRYING otIT.05ph0dC air COOLING REACTION FREEZING CHAMBER CHAMBER CHAMBER SPRAY COOLING SPRAY REACTION SPRAY FREEZING KEY: f—feed, p--product, s—scrubber/condenser/cooler. Figure 0.2. Layouts of spray dryers and associated suspended particle processing equipment involving atomization. 6 INTRODUCTION specifications laid down by diversified industries. Such range of application has led to dryer designs becoming less standardized as each product has to be treated individually and handled in specialized ways to meet the dried product specifications. Whatever dryer design the product demands, the advantageous features of spray drying are retained. These advantages can be listed as : (1) Continuous in operation. (2) Adaptable to full automation. (3) Dried product specifications met through dryer design and operational flexibility. (1) Required product form (particles as spheres, cenospheres, fines, agglomerates) (figure 0.3). (ii) Required product properties (dusty or dustless, degree of flowability, wettability, etc., also see below). (4) Applicable to both heat sensitive and heat resistant materials. (5) Economic in operation. Dried product specifications are related to the properties of : (a) Particle size distribution. This governs product appearance, packing, and subsequent processing requirements. (b) Bulk density and particle density. This is closely related to packing container requirements. Spray drying maintains constant product density and eliminates the need for batch mixing to meet specified densities. (c) Appearance. This is vital from the consumer angle. (d) Moisture content. This governs powder quality, colour, flowability, shelf life, packing and subsequent processing requirements. (e) Friability. This is related to handling and packing. (f) Dispersibility. This is related to rate of solubility on reconstitution. (g) Colour, aroma, taste. This is related to overall powder quality. (h) Activity. This is related to any heat degradation occurring with biochemical products. Economic operation is closely associated with drying temperatures and solids content in the feed. The higher the drying temperatures and solids content, the greater the thermal efficiency' of the process. For example, based on an ambient and outlet drying air temperature of 68°F (20°C) and 185°F (85°C), increase in inlet drying air temperature from 275°F (135°C) to 1202°F (650°C) increases the overall dryer efficiency from about 44 to 90 Z. Increase in feed solids (for a given production rate) from 50 % to 60 % reduces the heat load by nearly 50 %. However, many spray dryers operate at low feed solids and comparatively moderate drying temperatures as these conditions are dictated by the feed properties. In these cases, successful operation is based not so much on thermal efficiency but on the ability of the process to dry delicate products without degradation. INTRODUCTION 7 (a) (b) (c) Figure 0.3. Dried-powder forms produced by spray drying. (a) Fine particles (dusty) (noninstant skim milk). (b) Spheres (Aluminium oxide). (c) Agglomerates (instant skim milk). 8 INTRODUCTION • The book is divided into five sections. Section I contains five chapters on basic principles and includes important definitions. Section II deals with the process stages of spray drying, where individual chapters are given to atomization, spray—air contact (mixing and flow), drying of sprays, and dried product recovery. Section III, entitled 'Operational Practice', describes control systems and common operational measurements. Section IV briefly surveys some of the equipment used on spray dryers. Section V concludes the book with descriptions of established, new or interesting products that are spray dried nowadays. Products are classified according to their induStry. A literature survey, including recent patents covering spray drying applications, is given at the beginning of section V (chapter 13). Section I BASIC PRINCIPLES, DEFINITIONS 1 Spray Drying Fundamentals Spray drying consists of four process stages (figure 0.1): (A) Atomization of feed into a spray. (B) Spray—air contact (mixing and flow). (C) Drying of spray (moisture evaporation). (D) Separation of dried product from the air. Each stage is carried out according to dryer design and operation, and, together with the physical and chemical properties of the feed, determines the characteristics of the dried product. The spray homogeneity following atomization and the high rates of moisture evaporation (spray—air mixing and flow) enable the temperature of the dry product to be considerably lower than the drying air leaving the drying chamber. The product is thus not subjected to high temperatures, and when separated from the drying air is devoid of any heat degradation. The basic physical principle of `evaporation causes cooling' is very pertinent to the operation. Figure 1.1 shows diagrammatically what features each process stage has. Figure 1.2 indicates the actual equipment involved to carry out each stage in a standard layout, represented by a rotary atomizer, cyclone separators and pneumatic product conveying. Feed is pumped from the product feed tank (1) to the rotary atomizer (5). The atomizer is located within a ceiling air disperser (12), through which drying air enters the drying chamber (15). The air is drawn from atmosphere by a supply fan (8) and is steam heated (10). Following the drying of the spray in the chamber, the majority of dried product falls to the base of the chamber and enters a pneumatic conveying system (20) via a powder offtake (18). Conveying air is filtered (19). The product fines remain entrained in the air and pass (27) to cyclones (28) for separation. The fines enter the pneumatic conveying system. Exhaust air passes to atmosphere via the exhaust fan (31), Dried powder in the SPRAY DRYING FUNDAMENTALS BASIC PRINCIPLES, DEFINITIONS pff f7 d ULLl SPRAY EVAPORATION ;61, SPRAY-AIR L) Figure 1.1. The features of the process stages involved in spray drying (shown diagrammatically). PRODUCT SEPARATION h, oax z 13 ao Sti FEED -ATOMIZATION 12 Equipment items Feed system 1. Product feed tank. 2. Water feed tank for use during dryer start-up and shut down. 3. Three way valve and filter. 4. Feed pump. Atomizer system 5. Rotating vaned wheel atomizer. 6. Atomizer motor drive. Supply air and spray-air contact system 7. Filter at drying air intake. 8. Air supply fan. 16. Insulated chamber wall. 17. Chamber pressure detector. Product recovery system 18. Powder discharge unit at chamber base. 19. Filter at conveying air intake. 20. Pneumatic conveying system duct. 21. Transport cyclone. 22. Powder hopper. 23, Rotary valve. 24. Pneumatic conveying system exhaust duct. 25. Conveying air fan (transport fan). 26. Outlet drying air temperature measuring element. 27. Exhaust drying air duct. 28. Main powder recovery cyclone. 29. Rotary valve. 30. Exhaust air duct from cyclone. 31. Exhaust drying air fan. 32. Exhaust air flow damper. 33. Exhaust air stack. 34. Air hood. 35. Spray dryer control panel. 9. Air flow damper. 10. Air heater (here shown as a steam-air heater). 11. Inlet drying air temperature measuring element. 12. Air disperser. 13. Cooling air outlet (air disperser cooling), 14. Air disperser cooling fan. 15. Spray drying chamber. Figure 1.2. Equipment involved in a standard spray dryer layout. (By courtesy of Niro Atomizer.) pneumatic transport system is collected at the base of the transport cyclone (21). Instrumentation items include air temperature measurement (11) (26), chamber pressure measurement (17) and dampers (9) (32) for adjustment of air flows. 14 BASIC PRINCIPLES, DEFINITIONS SPRAY DRYING FUNDAMENTALS 15 (A) Atomization of Feed into a Spray The formation of a spray (atomization) and the contacting of the spray with air are the characteristic features of spray drying. The selection and operation of the atomizer is of supreme importance in achieving economic production of top quality products. The atomization stage must create a spray for optimum evaporation conditions leading to a dried product of required characteristics. Rotary atomizers and nozzles are used to form sprays. With rotary atomizers centrifugal energy is utilized. There are two categories of rotary atomizers : (a) atomizer wheels, (b) atomizer discs. Wheel designs are available to handle feed rates up to tens of tons feed per hour. With nozzle atomization, pressure, kinetic or (less common) sonic energy is utilized. There is a wide range of nozzle sizes and designs to meet spray drying needs. Feed capacities per nozzle are lower than per rotary atomizer, leading to nozzle duplications to meet high feed rate requirements. The selection of the atomizer depends upon the nature of the feed and the desired characteristics of the dried product. In all atomizer types, increased amounts of energy available for liquid atomization result in sprays having smaller droplet sizes. If the available atomization energy is held constant but the feed rate is increased sprays having larger droplet sizes will, result. The degree of atomization depends also upon the fluid properties of the feed material, where higher values of viscosity and surface tension result in larger droplet sizes for the same amount of available energy for atomization. (i) Rotary Atomizers (Utilization of Centrifugal Energy) Feed is introduced centrally on to a wheel or disc rotating at speed. The feed flows outwards over the surface, accelerating to the periphery. Feed, on leaving the periphery, readily disintegrates into a spray of droplets. Rotary atomizers form a low pressure system. A wide variety of spray characteristics can be obtained for a given product through combinations of feed rate, atomizer speed and atomizer design. Designs of atomizer wheels have vanes or bushings. Vanes are high, wide, straight or curved; bushings circular or square. Vaned atomizer wheels are used in many and varied industries, producing sprays of high homogeneity. Atomizer wheels with bushings are used in more specialized fields, e.g., for handling abrasive feeds. Wheels can be operated to produce sprays in the fine to medium coarse size range (see figure 2.1). Peripheral velocities reach 550 ft/sec (154 m/sec) in industry. Designs of disc include vaneless plates (discs), cups, and inverted bowls. Discs are used to meet coarse spray requirements. Rotary atomization is discussed in detail in chapter 6. The spray form leaving a rotary atomizer (vaned wheel) is shown in figure 1.3(a). Rotary atomizers are reliable, easy to operate and can handle varying loads. (a) (b) Figure 1.3. Atomizers in operation. (a) Rotary atomizer (vaned wheel). (b) Nozzle atomizer (pressure nozzle). 16 BASIC PRINCIPLES, DEFINITIONS (ii) Pressure Nozzles (Utilization of Pressure Energy) The feed concentrate is fed to the nozzle under pressure. Pressure energy is converted to kinetic energy, and feed issues from the nozzle orifice as a high-speed film that readily disintegrates into a spray as the film is unstable. The feed is made to rotate within the nozzle resulting in cone shaped spray patterns emerging from the nozzle orifice. Sprays from pressure nozzles handling high feed rates are generally less homogeneous and coarser than sprays from vaned wheels (see figure 2.1). At low feed rates spray characteristics from nozzles and wheels are comparable. Duplication of nozzles allows fine sprays to be obtained in nozzle dryers, but nozzles are generally used to form coarse particle powders having good free flowability. The spray form leaving a pressure nozzle is shown in figure 1.3(b). Variation of pressure gives control over feed rate and spray characteristics. Pressure nozzles have operating pressures up to 10 000 p.s.i. (680 atm). Pressure nozzles are described in detail in chapter 6. (iii) Two-fluid Nozzles (Utilization of Kinetic Energy) The feed concentrate and atomizing gas (usually air) are passed separately to the nozzle head. High air velocities are generated within the nozzle for effective feed contact which breaks up the feed into a spray of fine droplets. Sonic velocities are often generated. The air stream is rotated within the nozzle, and feed is contacted either within the nozzle (internal mixing) or as the liquid emerges from the orifice (external mixing). The nozzles operate successfully at low pressures (up to 100 p.s.i. (7 atm)). The feed system includes pressure pumps, although at low feed rates the suction caused by the air flow ejector effect will be sufficient to draw liquid into the nozzle. Adjustment of the air flows controls the degree of atomization at constant feed rate. Two-fluid nozzles have the advantage of handling high viscous feeds and produce sprays of medium coarseness, but of poor homogeneity. For low viscous feeds, fine particles can be produced, although the resulting dried powder may be of agglomerates. There is much likelihood for high occluded air content within the particles. Two-fluid nozzles are discussed in chapter 6. Two-fluid nozzles are generally applied in small diameter chambers where fine atomization is required. However, they are expensive to operate and low production per dryer unit is obtained. Atomizing air can be combined with a rotary atomizer to form a pneumaticcup atomizer. (8) Spray-Air Contact (Mixing and Flow) The manner in which spray contacts the drying air is an important factor in spray dryer design, as this has great bearing on dried product properties by influencing droplet behaviour during drying. Spray-air contact is SPRAY DRYING FUNDAMENTALS 17 AIR OUT PRODUCT IN ATOMIZER AIR PRODUCT IN IR IN ATOMIZER ATOMIZER PRODUCT IN AIR OUT AIR PRODUCT OUT OUT PRODUCT ial CO- CURRENT FLOW DRYER Al IN Al R IN PRODUCT OUT b COUNTER-CURRENT FLOW DRYER AI R AND — PRODUCT OUT MIXED FLOW FLOW DRYER Figure 1.4. Product—air flow in spray dryers. determined by the position of the atomizer in relation to the drying air inlet. Many positions are available. The spray can be directed into hot air entering the drying chamber as shown in figure 1.4(a). Product and air pass through the dryer in 'co-current' flow,* so called after the inlet-outlet layout for air, feed, and dried products (3) (35). This arrangement is widely used, especially in cases of handling heat sensitive products. Spray evaporation is rapid, the drying air cools accordingly, and evaporation times are short. The product is not subject to heat degradation. Product temperature is low during the time the bulk of the evaporation takes place as droplet temperatures approximate to wet bulb temperature levels. When the desired moisture content is being approached, each particle of the product does not rise substantially in temperature as the particle is then in contact with much cooler air. In fact, low temperature conditions prevail virtually throughout the entire chamber volume, in spite of very hot air entering the chamber. This is shown in figure 1.5(a), which illustrates a typical air temperature distribution within co-current flow dryers. Both rotary and nozzle type atomizers can be used in co-current flow dryers. With the former type, the radial trajectory of droplets from the atomizer periphery can be controlled, so excessive product deposits on the drying chamber wall are prevented. * Quotation marks are used as spray—air movement in reality is often far from co-current, e.g. at the point of actual spray—air initial contact and in any areas of back mixing in the drying chamber. 18 BASIC PRINCIPLES, DEFINITIONS SPRAY DRYING FUNDAMENTALS Alternatively, the spray can be contacted with air in 'counter-current' flow (figure 1.4(b)). Spray and air enter at the opposite ends of the dryer (3) (35). This arrangement offers dryer performance with excellent heat utilization, but it does subject the driest powder to the hottest air stream (see air temperature distribution, figure 1.5(b)). It readily meets granular powder requirements of non heat-sensitive products. Counter-current flow is commonly used with nozzle atomization, since an upward streamline flow of drying air reduces the fall velocity of the large droplets in the spray, enabling sufficient residence time in the drying chamber for completion of evaporation, AIR 120 FEED AIR 230 1 I I 220 160 40 I 220 60 130 FEED th 60 150 180 FEED 180 130 100 120 120 40 60 240 100 90 270 90 100 BO BD 300 100 300 80 80 100 \ 100 —14.-AIR 330 AIR 350 AIR PRODUCT a. CO-CURRENT DRYER (C) Drying of Spray (Moisture Evaporation) 240 90 110 105 PRODUCT the hot areas around the air disperser. Air flow in the drying chamber is discussed in chapter 7. The selection of how best to contact the spray cloud with drying air is dependent upon the product involved. For example, in the 'countercurrent' arrangement, the hottest drying air contacts the driest particles as they are about to leave the chamber. If the dried product can withstand presence in a very high temperature, and a high bulk density product is required, this layout is highly suitable. The product particles will be of low porosity due to the reduced tendency of the droplet to expand rapidly and fracture during evaporation. If the particle cannot withstand such high temperature conditions alternative contacting methods must be employed and the `co-current' system may be suitable. The hottest drying air contacts droplets at their maximum moisture content. The rapid evaporation prevents high droplet temperatures. However, the droplets undergoing such a high evaporation rate may well expand or fracture to give non-spherical porous particles, and the product will often have a low bulk density. 100 40 50 110 110 210 230 AIR 100 19 350 AIR PRODUCT b. COUNTER - CURRENT DRYER Figure 1.5. Air temperature distributions in co-current and counter-current flow spray dryers. (AU temperatures in degrees centigrade.) There are dryer designs that incorporate both `co-current' and 'countercurrent' layouts, i.e. mixed flow dryers, figure 1.4(e). In this type coarse free flowing powder can be produced in dryer chambers of relatively small size. In all cases, the movement of air predetermines the rate and degree of evaporation by influencing (a) the passage of spray through the drying zone, (b) the concentration of product (particle population) in the region of the dryer walls, and (c) the extent to which semi-dried droplets re-enter As soon as droplets of the spray come into contact with the drying air evaporation takes place from the saturated vapour film, which is quickly established at the droplet surface. The temperature at the droplet surface approximates to the wet bulb temperature of the drying air. Evaporation takes place in two stages. At first there is sufficient moisture within the droplet to replenish that lost at the surface. Diffusion of moisture from within the droplet maintains saturated surface conditions and as long as this lasts, evaporation takes place at a constant rate. This is termed the first period of drying. When the moisture content is reduced to a level, where it is insufficient to maintain saturated conditions, the so-called critical point is reached and a dried shell forms at the droplet surface. Evaporation is now dependent upon the rate of moisture diffusion through the dried surface shell. The thickness of the dried shell increases with time causing a decrease in the rate of evaporation. This is termed the falling rate period or second period of drying. Thus a substantial part of the droplet evaporation takes place when the droplet surfaces are saturated and cool. Drying chamber design and air flow rate provide a droplet residence time in the chamber, so that the desired droplet moisture removal is completed and product removed from the dryer before product temperatures can rise to the outlet drying air temperature of the chamber. Hence there is little likelihood of heat damage to the product. 20 BASIC PRINCIPLES, DEFINITIONS SPRAY DRYING FUNDAMENTALS During evaporation, the atomized spray distribution will undergo change. Different products exhibit different evaporation characteristics. Some tend to expand, others collapse, fracture or disintegrate, leading to porous irregular shaped particles. Others remain a constant spherical shape or even contract, leading to denser particles. The extent of any particle shape change and hence the dried powder characteristics is closely connected to the drying rate, and it follows that meeting desired powder characteristics requires close consideration to the drying chamber design. Drying of sprays forms the subject matter for chapter 8. 21 System (2). Total recovery of dried product takes place in the separation equipment (figure 1.6(b)). This system places great importance on the separation efficiency of the equipment, but the system is often utilized, as it does not need a product conveying system. Separation of dried product from the air influences powder properties by virtue of the mechanical handling involved during the separation stage. Excessive mechanical handling can produce powders having a high percentage of fines. Separation effects in drying chambers is discussed fully in chapter 9. Separation and recovery equipment is covered in chapter 12. ( D) Separation of Dried Product from the Air Product separation from the drying air follows completion of the drying stage, when the dried product remains suspended in the air. Two systems are used to recover the product. These are illustrated in figure 1.6 for the case of co-current flow dryers with a rotary atomizer and cyclones. System (1). Primary separation of dried product takes place at the base of the drying chamber (figure 1.6(a)). During operation, the majority of product falls to the base of the chamber, while a small fraction passes out entrained in the air and is recovered in the separation equipment. Such equipment is usually cyclones, Bag filters are also installed as are electrostatic precipitators and wet scrubbers. The choice of equipment is dependent upon the powder loading of the air leaving the drying chamber, and accept,able efficiencies of recovery. With this system, a classification of powder is achieved, as the coarse particles are recovered at the chamber base and the finer particles from the separation unit. This form of powder classification can be utilized. However, normally the two powder offtakes are combined and conveyed to a single discharge area. PRODUCT Ill AIR IH AIR IN ATOMIZER AIR ovr AJR AND ENTFtA INED POWDER U. b. PRIMARY PRODUCT DISCHARGE SECONDARY PRODUCT DISCHARGE TOTAL PRODUCT DISCHARGE Figure 1.6. Product discharge from co-current flow spray dryers with a rotary atomizer. Meeting Dried Product Requirements in Spray Drying The meeting of dried product requirements calls for close attention to all four process stages. All stages effect dried product properties to a degree. Atomization technique and feed properties will have a bearing on particle size distribution, bulk density, appearance, and moisture content. Spray— air contact and resulting evaporation, in fact the drying operation, will have a bearing on bulk density, appearance, moisture content, friability and retention of activity, aroma and flavour. Techniques for product—air separation will determine the degree of comminution the powder undergoes following completion of drying. Many operational variables associated with atomization and the drying operation offer means of altering dried product characteristics. The important variables are summarized below. (1) Energy Available for Atomization Increase in energy available for atomization will create smaller droplet sizes at constant feed conditions. Increase in rotary atomizer speed, nozzle pressure, or air—liquid flow ratio in two-fluid nozzles will decrease mean spray droplet size. The spread of droplet sizes in the spray distribution may not be appreciably changed. Producing greater amounts of fine particles can often form a product of higher bulk density. The greater numbers of smaller particles fill the voids between the larger, and smaller particles may well be more dense. (2) Feed Properties Increase in feed viscosity through increase in feed solids or reduction in feed temperature will produce coarser sprays on atomization at fixed atomizer operating conditions. Surface tension effects appear minor. Increase in feed solids effects evaporation characteristics where generally an increase in particle and bulk density results. (3) Feed Rate Increasing feed rate at constant atomizer operating conditions will produce coarser sprays and dried products. 22 BASIC PRINCIPLES, DEFINITIONS (4) Atomizer Equipment Selection Rotary atomizers and nozzles exhibit different spray forming characteristics, which can be utilized to meet necessary product requirements. Selection can only be made with reference to the product concerned. However, modern rotary atomizer and nozzle designs are flexible and can produce similar spray characteristics over a wide range of industrial products and dryer capacities, although there are applications where certain atomizer techniques are so established that they are considered standard. (5) Atomizer Equipment Design This is closely connected with item (1) above. If the energy available is made to act on reduced feed bulk, finer sprays will result. Many spray properties can be achieved by alteration to the vane design of an atomizer wheel, where number, height, width, length will determine the amount of liquid at the point of atomization at the wheel periphery. Similarly, duplication of nozzles, at fixed pressure will create finer sprays through reduced liquid bulk per nozzle. (6) Air Flow Air flow rate controls to a certain extent product residence time in the drying chamber. Increased residence time leads to greater degree of moisture removal. Reduction in air velocity assists product recovery from drying chamber. Air flow has bearing on product handled and its dried properties. (See earlier, (B) Spray—Air Contact.) (7) Drying Temperature Inlet. Increase in inlet temperature increases the dryer evaporative capacity at constant air rate. Higher inlet temperatures mean a more economic dryer operation. Increased temperature often causes a reduction in bulk density, as evaporation rates are faster, and products dry to a more porous structure. Outlet, For a fixed moisture content and dryer design, outlet temperature must be kept within a narrow range to maintain the powder packing and flow requirements. Increase in outlet temperature decreases moisture content at constant air flow and heat input conditions. Operation at low outlet temperature to produce powder of high moisture content is used, where agglomerated forms of powder are required. This is often utilized in making special 'instant' powders. Auxiliary equipment (e.g. fluid-bed) is required to handle the high moisture powder leaving the dryer. 2 Representation of Sprays Spray droplets and dried particles are an inherent part of spray drying. It is vitally important that droplets and particles can be represented in a manner for easy reference. Accepted terminology is available to express mean size and size distributions. Particle size distribution features as a most important dried product specification. Particle size is closely related to droplet size, but is rarely equal, due to droplet behaviour during drying. Ranges of droplet and particle sizes met in spray drying are shown in figure 2.1. 2.1. Terminology 2.1.1. Droplet This refers to the state of subdivision of feed on being sprayed from the atomizer. As long as the surface moisture remains in the spray, the spray is said to be composed of droplets. 2.1.2. Particle This refers to the state of subdivision of dried product. The shape of the particle depends upon how the droplet was formed during atomization and how the droplet/particle behaved during drying. 2.1.3. Agglomerate An agglomerate is composed of two or more particles adhering to each other. Agglomeration is often desired in the spray drying operation as agglomerated particles show improved dispersibility characteristics. Agglomerates can be formed through two or more droplets coalescing in the proximity of the atomizer and drying in this state, or through partially dried droplets adhering to each other in the lower regions of the chamber, due to their sticky surfaces. Agglomerates when specifically desired are created in the drying chamber by (a) contacting the evaporating spray 24 BASIC PRINCIPLES, DEFINITIONS REPRESENTATION OF SPRAYS 25 with dry product fines, or (b) installing special agglomerating equipment directly to the drying chamber (e.g. fluid-bed instantizer). 2.1.4. Size The size of a particle/droplet/agglomerate is the representative dimension that expresses the degree of comminution. For spherical particles the diameter represents its size. For non-spherical particles, its size can be represented by an 'apparent' diameter. This is the mean distance between extremities of the particle measured through the particle centre of gravity. Size can also be based on area, volume or weight (see below 'Size Distribution' and 'Mean Size'). 2.1.5. Particle Shape The complexity of the atomization mechanism and the distortions a droplet undergoes during drying result in the majority of spray-dried products being comprised of non-spherical particles. Wide variations in shape are often evident The ratio of measured maximum to minimum particle diameters often defiii -e hape. To express divergence from sphericity a shape factor is used, defined as ifie-rattobetween the actual surface or volume of the particles and the total surface or volum-d-obtaiffed from size measurement techniques, e.g. microscopic analysis or sieving, where spherical particles are assumed. 2.1.6. Size Distribution Droplets and particles comprising sprays and dried products are never of one size. The atomizer cannot form totally homogeneous sprays. Spray droplets are subjected to different shape distortions depending upon their drying characteristics and travel within the dryer. Dried particles and droplets from a spray have a range of sizes termed their size distribution. A great number of methods have been devised over the years for measuring size distributions. Microscopic analysis (with manual or automatic counting), sieving, sedimentation, elutriation, light absorption and automatic sensing equipment (e.g. Coulter Counter analysis) are the established methods. Counting procedures express the number of droplets or particles within a suitable size group (increment). Size distributions can be represented by a frequency or cumulative distribution curve. If occurrence is given by number, a number distribution results, or if given by area-volume-weight corresponding to a given diameter, area-volume-weight distributions result. Number size distribution is the outcome of microscopic analysis— weight distribution the outcome of sieving. Methods of size analysis are reviewed in chapter 11. Droplets forming a size distribution of a spray from a centrifugal pressure nozzle, and particles forming a size distribution of a spray dried ceramic material are shown in figure 2.2. 2.1.7. Mean Size The mean droplet or particle size represents a single value, most suited to be representative of the whole distribution. No value is adequate to express - 26 BASIC PRINCIPLES, DEFINITIONS •• •• • • • • 1. ;•• • ■ . • ■ • • • • • • OS • • ■ •• . • • 11'0 '• •• • • • • .11 • ■ •• • • • ' • •• '•• • •• • • .0 • • • • '. :. : •• ■ • • ■ • ••• • • * - •• • 500p (a) SDX centrifugal pressure nozzle type SE-622 300 p.s.i.g., 26.5 U.S. gal/hr water Sauter mean diameter = 65 micron (b) Figure 2.2. Size distribution of droplets and particles. (a) Droplet size distribution. (By courtesy of Delavan Manufacturing Company.) (b) Dried particle size distribution (ceramic material). (By courtesy of Niro Atomizer.) a size distribution, and the mean size must be used with other parameters to define more fully size characteristics. There are many types of mean diameter parameters. The type selected depends upon the information required about the spray or product, i.e. length, area, volume, shape, etc. The pertinent characteristic varies according to how the droplet or particle data is to be used. Details on mean size parameters and their calculation follow in this chapter. SIZE RANGE • • • 27 For a comprehensive account of spray data presentation, the reader is referred elsewhere (4) (5) (6) (35). 2.2.1. Tabular Form This is the most precise and general method of presenting droplet size data. Tables can show a listing of size against one or more ways of expressing their distributions, e.g. size frequency or size cumulation. However, large amounts of data can make tabular form unwieldy and difficult to interpret. 2.2.2. Graphical Form The use of graphical presentation offers many advantages in spite of the accuracy of tabular presentation. Graphs present data in a form whereby approximate values of deviation and skewness of data from a given mean can be assessed quickly. Furthermore, graphs are more manageable than long lists of data in tabular form. Graphs also provide constants that describe the size distribution. The relationship of a size distribution to a certain mathematical function can be seen at a glance from graphical representation. (a) Histograms The histogram is the simplest way of representing size distribution of a spray. It is a plot of the percentage number of droplets or particles in a given size range (size increment). The histogram gives an immediate indication of the droplet size, which constitutes the majority of the distribution. A typical histogram is shown in figure 2.3. OCCURRENCE OF DROPLETS • REPRESENTATION OF SPRAYS w o_ D. min DROPLET SIZE (D Figure 2.3. Droplet size distribution represented in histogram form. 2.2. Methods of Data Presentation There are two basic forms of representation available to express the characteristics of size and size distribution. These forms are summarized below. (b) Size Frequency Curves Curves are more practical when a large number of size increments are used to express the size distribution. Size frequency curves can be considered 28 BASIC PRINCIPLES, DEFINITIONS REPRESENTATION OF SPRAYS a smoothed out form of histogram (figure 2.3) and give the relative frequency of a variable within a certain group of data (measurements of diameter, volume, surface area, etc.). The frequency curve shown in figure 2.4 is a plot of the number of droplets with a diameter within certain size increments (fN (D)) against diameter (D). The subscript N indicates a frequency of occurrence according to number. Droplet frequency is generally stated as a percentage diameter. The frequency curve is expressed as f fN (D) d(D) = 100 % (2,1) p, If the ordinate of the plot is the volume or surface area corresponding to a given diameter the resulting curve is skewed due to the weighting influence in the large-diameter range. (c) Cumulative Plots A further method of representing size distribution is the cumulative distribution plot formed by plotting the cumulative frequency percentage of particles or droplets greater or less than a given size, against the size. Cumulative percentage can be represented on linear or probability paper. Cumulative plots are shown in figure 2.4 and figure 2.5. Particle or droplet diameter, surface, area, volume, weight can form the basis of the curve. 2.2.3. Mathematical Form This is the representation of data in a manner most suitable for size prediction. Mathematical functions express the form of distribution (see table 2.3). 29 duly calculated have a number basis. These are described below. Calculation of mean diameters is illustrated in example 2.1. (a) Most Frequent Diameter (DO The most frequent diameter often characterizes a spray or dried powder sample satisfactorily. This size can be seen from tabular results. When represented graphically Df corresponds to the highest value on the frequency curve. It also appears as the point of inflection for data represented on a cumulative curve. Dr is shown in figure 2.4. (b) Arithmetic Mean Diameter (D AM ) The arithmetic mean diameter (D AM ) is defined as the sum of the diameters of separate particles/droplets divided by the number of particles/droplets. This mean diameter is most significant when the particle or droplet size distribution is not overbalanced by either very large or very small particles— droplets. DAM can be defined in terms of the frequency curve, where D rnax -J— D AM — 100 • Dmi„ D • fN (D)d(D) (2.3) The arithmetic mean can be readily calculated from sampling data (see example 2.1), since DAM = ED . fN (D)AD EfN (D)AD (2.4) where 2.3. Analysis of Data A distribution function and two parameters can be used to represent spray data. These parameters consist of a mean diameter of some form, and a measure of the size range of particles involved. 2.3.1. Mean Diameters A mean diameter is a mathematical value that represents the complete spray. This value can be a measure of number, length, area, or volume. A general equation that defines a mean diameter is given by (Dpoa _p fN (D)A(D) EDP . fN (D)A(D) (2.2) where D is the mean diameter and p q are integers (or zero). f (D) is the function representing the spray size. For number (arithmetic) mean : p = 0, q = 1: surface mean p. = 0, q = 2: volume surface mean p = 2, q = 3. AD is the size class increment and is usually taken as uniform. When analysing sprays from atomizers, microscopic counting of a given spray sample is the technique most commonly used. The mean diameters ED . fN (D)(AD) = summation of every given size (range) multiplied by its percentage occurrence; • EfN (D)(AD) = summation of given size occurrence, which is 100 for sampled data. (c) Geometric Mean Diameter (DGM) The geometric mean diameter (D GM ) is defined as the nth root of the product of the diameters of the /7 particles/droplets analysed. D GM is always smaller than DAM . The geometric mean for droplet and particles according to their sizes D 1 , D 2 ,. , D„, (where fN (D) is the percentage occurrence of a given size in a sample) is represented by DGm — 10..sly(Dfi N(DI) DJ' DiiN(D.)) (2.5) DGM is of particular value since in the log-normal distribution the geometric mean is the diameter having the highest frequency. Defined in terms of logarithms log DGM = ffiEfN(D) (log D) (2.6) 30 REPRESENTATION OF SPRAYS • 31 BASIC PRINCIPLES, DEFINITIONS (d) Harmonic Mean Diameter (D HM ) The harmonic diameter is defined as the number of particles/droplets divided by the sum of the reciprocals of the diameters of individual particles/ droplets. It is related to specific surface, and is of value where surface area is the important product characteristic. D HM is always smaller than DGm For occurrence of a given size stated as a percentage, - the harmonic diameter is represented by 100 Dflm = (2.7) IfN(D)/(D) (e) Median Diameter (D M ) The median diameter is defined as the diameter above or below which 50 % of the number of droplets/particles lie. The median diameter divides the area under the frequency curve into two equal parts. It is represented by the 50 % line on the cumulative curve (figure 2.4). D M is especially useful when an excessive number of very large and very small particles are present. The mean diameters defined above are divergent. The parameter selected is appropriate to the circumstances of sampling. In general D,,m DM (2.8) DAM The relation between the mean diameters follows no definite rule, as any relation depends upon the skewness or bias of the distribution. The calculation of the mean diameters defined above is illustrated in example 2.1. EXAMPLE 2.1 Spray from a nozzle atomizer is sampled and analysed by microscope. The numbers of droplets occurring in size increments of 20 micron were determined. 500 droplets were counted. The resultant distributions are given in table 2.1, column 4. Calculate : 1. Most frequent diameter 2. Arithmetic mean diameter 3. Geometric mean diameter 4. Harmonic mean diameter 5. Median diameter The computations required are shown in table 2.1 and the distribution is shown graphically as a frequency and cumulative curve in figure 2.4. 1. The most frequent diameter as seen on the frequency curve or in table 2.1, column 4, is 70 micron. 2. The arithmetic mean diameter as defined in equation (2,4) becomes, for uniform size increments Column 7 9608 = Column 5 100 96.08 micron 3. The geometric mean diameter as defined by equation (2.6) becomes log DGM Column 8 190.38 — 19038 100 100 D Gm = 80 micron 4. The harmonic mean diameter as defined by equation (2.7) results in o 9n 7 E < 22 100 20 18 80 16 - 0 1412- 60 10 40 a 6 4 20 20 40 60 80 100 120 140 160 180 200 220 240 CUMULATIVE PERCENT LESS THAN DROPLET SIZE (b) 7 co. DROPLET SIZE CD) MICRONS Figure 2.4. Frequency and cumulative curves showing mean droplet diameter values in example 2.1. 100 100 — — 67 micron DHM _— Column 9 1 486 5. The median diameter (i) corresponds to the 50 % line on figure 2.4 = 83 micron (ii) from table 2.1, column 6: less than 90 micron, greater than 70 micron Apart from mean diameters based on the frequency of size occurrence other mean diameters based on surface, volume or mass are available. For each chosen basis, the appropriate values of integers (p . q) as given in equation (2.2) must be used. Table 2.2 shows four such mean diameters. REPRESENTATION OF SPRAYS BASIC PRINCIPLES, DEFINITIONS 33 Table 2.2. Mean Diameters Based upon Number, Surface and Volume AD CD AD 0 AD Net CD oo eN eN oo m CD AD 00 et DON oo • c.,.4 (-14 ,-. CD CD CD CD CD c, et C7 CD 6 6 e5 6 6 c5 c) cp ati r (4p (471 rq • •D AD ct AD- oo UD - •D et et ion N 00 UD 0' CD er et 00 c7 ,-. 00 on (.0 • oo r4-- r- rl r- cN 00 .1 --, ( 1 -4 ( ) - i e5 m rl ob tr) cn on Mean diameter D Surface mean D d c? cu u? u? op c? u? up c? oo ,t r- O. ep r- -Li • C7 ,t r- oo oo CN CN CD 9 r4 et vn r 4 , O 0 N : N op 4 r- tfl 1—c r ,?m ,0t r- vl ,?N 0 9-1 CD CD CD \AD r4 oo r4 VD VD Do CD r4 • Nr r et DO N rt CN c) N 00 N on AD ') et N (-4 rcq r4m •D m VD oo qs, LE NcV NN NNN c7 r, cry 0 N Cq 00 - C7 r- en ,t ,r) c? CD • - 0 CD CD 0 0 CD CD CD 0 CD CD 0 • rn vn r- CN w (-1 Min w. r- N N CD CDCD CD CD CD CD CD AD 00 CD rl CD CD CD CD CD (-4 cg Ng c - c; c; "c .cT rCg Cr) AD 00 CD N 1 UD 00 ° AM sm CN 0 0 PI, 0 r4 00 C7 0 - CD et UD UD < 4 (7 N - CD CD r- C. vn 00 CD DO N r- CD uD ( V r- r4 et et rn C7 oa AD of CN • Mathematical definition Arithmetic mean (linear) Volume mean Table 2.1. Calculation of Mean Diameters in Example 2.1 32 r cg N O Volume—surface (Sauter) mean D vm D vs ED . fN (D)AD EfN (D)AD (2.4) LD 2 fN (D)AD1 112 EfN(0)AD (2.9) ED 3 fN(D)AD EfN (D)AD (2.10) (D 3 fN(D)AD) D2fN(D)AD (2.11) Analysis of spray dried powder using sedimentation or sieving techniques results in mean diameters based on volume or weight. Where the latest light absorption techniques are used, diameters are based on surface. The volume mean diameter (D VM ) usually exceeds the Sauter mean diameter by 15-20 %. The two mean diameters commonly used in the spray drying operation are the median diameter (D M ) and the Sauter mean diameter (D„) (equation 2.11). The median diameter is that diameter above or below which lies 50 % of the number or volume of droplets/particles. The Sauter mean diameter is that droplet or particle having the same surface-to-volume ratio as the entire spray or powder sample. The parameters pre-suppose spherical droplets or particles. 2.3.2. Distribution Functions Many authors have prepared mathematical relationships to represent size distributions. The existence of varying forms illustrates that no one mathematical distribution fits the size range of droplets or dried particles produced in the spray dryer operation. The more common distributions are given below. Their mathematical definition is given in table 2.3. d(N) is the number of droplets or number fraction in size increment. d(D), B and C are constants. (a) Normal Distribution (Gaussian) Several distributions are based on the normal (Gaussian) distribution. The mathematical form is given in table 2.3, equation (2.12). Plotting the number of droplets or frequency against their size results in a 'bell-shaped' curve. The distribution is of limited use in spray drying. (S N is the number standard deviation.) 34 BASIC PRINCIPLES, DEFINITIONS REPRESENTATION OF SPRAYS Table 2.3. Distribution Functions d(N) = . exp i (2.12) Nog D - log D Gm ) 2 1 2,s. (2.13) [(,/D - V D Gm ) ] (2.14) r d(D) SN , 02m) Log-normal 1 d(N) _ d(D) - D . S G V(27E) . exP Square root normal I d(N) = d(D) 2 . V(27c . D . SG). exP Upper limit d(N) = 99.599 - _ _ 95 - _ _ - Df 1 1 d(N) = B . D 2 . e -(c •' ) Nukiyama-Tanasawa d(D) vi) = 100 - twii5R)q) Rosin-Rammler 2S G rlog ((D rii.„ - D)/D Gm l ' . ex d(D) D . S G V(27r) L 2,5?, P L 2. A z I- 90 as 70 60 50 40 - _ _ _ (2.15) 20 (2.16) (2.17) (b) Log-normal Distribution The log-normal distribution has a theoretical relation to droplet formation and is applicable to the spray drying process. The distribution has two parameters, the geometric mean size (D G ,) and the geometric standard deviation (S G ). The mathematical form is given in table 2.3, equation (2,13). The 'distribution gives a straight line on a plot of size (D) as abscissa on log-scale against the number per cent oversize or undersize as ordinate on probability scale (figure 2.5). The geometric mean diameter corresponds to D at the 50 % line. The geometric standard deviation is the size ratio at , the corresponding oversize values of 50 % and 15 9 % or the size ratio at the corresponding undersize values of 84.1 % and 50 %. Use of the undersize plot to determine geometric mean size and geometric standard deviation is shown in example 2.2. The log-normal distribution enables determination of the geometric mean size and deviation, and with this data other mean diameters (shown in table 2.4) can be calculated. This is possible since the nature of the lognormal distribution law means the geometric standard deviations on number, weight, surface area bases are equal. The log-normal distribution is applicable to represent sprays from rotary (vaned wheel) atomizers. (c) Square Root Normal Distribution The square root normal distribution equation (2.14) is similar in form to the log-normal distribution (equation 2.13). Both distributions have a mean and standard deviation. (VD) merely replaces (log D). The square root normal distribution is used with centrifugal pressure nozzles, as the CUMULATIVE Normal Equation No. Form Distribution 35 'v_. 10 5- _ 1 0.5 - _ 005 DROPLET SIZE (0) MICRONS 100 Figure 2.5. Log-normal distribution on probability paper. distribution often represents spray size data with greater accuracy than the log-normal distribution. A spray of a centrifugal pressure nozzle is shown represented by the square root normal distribution in figure 2.6. (d) Empirical Distribution Functions (i) Nukiyama—Tanasawa Distribution. The distribution (equation (2.16)) is proposed as suitable for representation of sprays from pneumatic nozzles. For the distribution to apply, a plot of (log 1/D' . d(N)/dD) against D' will be a straight line, the slope of which gives the value of the constant (C). Values of the dispersion coefficient (q) can vary between e and 2, depending upon nozzle design. For a given spray sample, values of q are selected by trial and error to determine the value that gives the actual spray distribution the closest agreement with a linear relationship. The higher the value of q, the narrower the size distribution. For small capacity nozzles, q can be taken as unity : the distribution is described in more detail under the section on pneumatic nozzle atomization (chapter 6) where it is plotted. Procedure on applying the distribution is given by Lewis et al. (7). (ii) Rosin—Rammler Distribution. The Rosin-aammler distribution is widely quoted to express size distributions especially from nozzle sprays. 36 REPRESENTATION OF SPRAYS BASIC PRINCIPLES, DEFINITIONS 10 37 -3 CUMULATIVE PERCENT BY WEIGHT LESS THAN D 99.9 99.5 99 95 90 99 10 70 60 50 40 30 20 10 5 10 0.0 0.1 0 2 4 6 8 10 1 1 11 (DROPLET DIAMETER 1'1/2 1 ( : ) 12 14 16 R MICRONS Figure 2.6. Droplet size distribution of a centrifugal pressure nozzle (grooved core swirl) conforming to a square root normal distribution. Feed rate: 120 kg/hr (aluminium silicate). Feed pressure: 50 atm. Orifice diameter : 1.1 mm. Spray angle: 45p. Grooved core swirl insert. 10° 10 100 DROPLET DIAMETER It is empirical, and relates the volume per cent oversize (V D ) to droplet diameter (D), It is a special case of the Nukiyama—Tanasawa Distribution. The mathematical form is given in table 2,3, equation (2.17). Rearranging equation (2.17) we obtain 100. ( =D VD (2.18) ( MICRONS ) Figure 2.7. Rosin—Rammler size distribution. Thus it follows that the value on the ordinate of figure 2.7 corresponding to Li equals log 100 36.8 = log 2.75 = 0.43 L/ R or log In /100\ VD q ID ./T) (2.19) For a spray distribution to follow this function, the plot of log (100/V D ) against (D) will give a straight line on log-log paper. This is shown in figure 2.7. The slope represents the dispersion coefficient (q). The higher the value of (q), the more uniform the distribution. The Rosin—Rammler mean (D R ) can be obtained directly from the curve as it is the droplet diameter above which lies 36.8 % of the entire spray volume. (iii) Upper limit function. This is a development of the log-normal distribution. The distribution is expressed in equation (2.15). Proposed by Mugele and Evans (6), it contains a third parameter, the stable maximum droplet size, which permits greater flexibility in fitting experimental data. The upper limit distribution is considered justified as all sprays are made up of droplet sizes that have a maximum size, i.e. the upper limit size. Nelson and Stevens (8) discussed the merits of the distribution in relation to the normal and square root normal distributions. The upper limit distribution places practical limits on the minimum and maximum droplet sizes, unlike the square root distribution, which gives meaningless values in the maximum 38 BASIC PRINCIPLES, DEFINITIONS REPRESENTATION OF SPRAYS size range. A comparison of the three distributions has been made (8) for the case of a centrifugal pressure nozzle. This is shown in figure 2.8. The upper limit and square root distributions approximate typical experimental droplet size distributions for a centrifugal pressure nozzle. 99.95 99.9 - I 1 i T - 99.5 _ d 0.51n 2 SG (2.20) _ D SM (Surface mean) ln DGm 2 1.01n SG (2.21) :- --3 --- - D vm (Volume mean) In DGm + 1.5 lri 2 SG (2.22) 95 I- 90 PERCENT LESS I 80 70 60 50 40 30 _ 1 - Dvs (Volume—surface (Sauter) mean) 2 in DGm In SG (2.23) The spray was sampled, the droplets counted and sized. Data is given in table 2.5. Calculate the Sauter mean diameter. Table 2.5 z _ 10 Measured size (micron) 3 , il 2 - ▪ 5 - 1 / 0•5 - 3 /2 1 / / • - 1 - 0.1 0 20 40 Number counted - / 20 9 Transformation (expressed in natural logarithms) Mean diameter 111 DGm 2 99 Table 2.4. Mean Diameter Transformation DAM (Linear or arithmetic mean) i 39 60 80 100 DROPLET SIZE ID) 120 140 Less than 5 5-15 15-25 25-35 35-45 45-55 55-65 65-75 75-85 3 18 130 220 105 48 16 11 6 160 MICRONS ) Figure 2.8. Comparisons of log-normal, square root normal and upper limit distributions for a centrifugal pressure nozzle (based upon Nelson and Stevens (8)): I. log-normal distribution; 2. upper limit distribution; 3. square root normal distribution (shaded area represents typical experimental data for the centrifugal pressure nozzle). 2.3.3. Mean Droplet Diameter Transformations If the size distribution of a sampled atomized spray obeys (or is in close agreement with) the log-normal distribution, the transformation between mean diameters can be used. This is shown in table 2.4. Example 2.2 illustrates the use of the transformation (table 2.4). EXAMPLE 2.2 An atomizer in a pilot plant unit is spray drying a low viscous liquid at a feed rate of 1 lb/rnin. A resultant spray is found satisfactory as the dried product meets the specifications. Data is required on the spray distribution, so that the atomization conditions 'can be selected for a scaled-up unit. Method 1: (use of equation 2.11) The computation steps are given in table 2.6. For uniform size increments Column 8 DVS = Column 7 129 983 x 10 3 ) = 43.4 micron 6889 5 x 102 . Method 11: (use of equation 2.23) This method prevents the tedious computations leading to columns 7 and 8 in Method I. Draw the cumulative per cent undersize curve from data in columns 2 and 6 respectively. This is shown in figure 2.9. Spray distribution lies on a straight line, hence following the log-normal distribution. From curve Geometric mean diameter (D GM ) = D = 24.2 micron 84.14 39 Geometric standard deviation (S G ) = D 50 = 1.62 24.2 = REPRESENTATION OF SPRAYS BASIC PRINCIPLES, DEFINITIONS 41 999 "e), 00 -do,—.c op 2? x 8 CD CD efl 8 P. cri; 00 Lu Ni 0 r— CD 8 8 • 0r 9 47 4? 7' O a 9 r- on 0 N N MD DO CN CP, CN CD ,r CD 00 00 MD N CD ‘ID CT CD CD 6,■ Cn pi) rq r.•- ) 995 99 95 • 0 90 • 80 70 60 84.14% ▪ 50 w - 40 30 CUMUL ATIVE PERCENT 0 0 on co op r op 0 6 ob 6 6 ken .0 on cn 71on oo • r4 00 ro.1 vn cn N 00 Table 2.6. Calculation of Sauter Mean Diameter in Example 2.2 40 20 . 24.2 microns 10 5 y ..••••• •••••• 0.1 2 3 4 6 8 10 DROPLET SIZE 101 on ',ID • rn c, rvn vn vn vn 39 microns 50% 20 30 40 60 80 100 MICRONS Figure 2.9. Size data for example 2.2, conforming to a log-normal distribution (cumulative per cent undersize curve for calculating geometric mean diameter and geometric standard deviation). Using equation (123) and substituting In D vs = in 24.2 + 2.5 In' 1.62 C H VD erl 00 CD CD ken 00 - rn. Cl CD .4 log io D vs = log„ 24.2 + 2.5 . 2-303 logi o 1.62 = 1.3838 + 0.255 vn N CD CD CD CD CD CD CD CD vn ,47 Q n N = 1.638 therefore Dvs --- 43.5 micron a) • E o2a (:) lfl in V-) 4-1. rn 1 • 1 .4 ) kr) vn V-1 1 vn vn N 00 1 vno t N m Cr vn MD N DRYING TERMS AND PRINCIPLES 3 Drying Terms and Principles of the droplet depend upon whether bound or unbound moisture is evaporated, as each has distinct features. As long as unbound moisture exists, drying proceeds at a constant rate, and will continue while the rate of moisture diffusion within the spray droplet is fast enough to maintain saturated surface conditions. When diffusion and capillary flow can no longer maintain these conditions the critical point is reached, and the drying rate will decline until the equilibrium moisture content is attained. The equilibrium moisture content will remain unchanged while product is exposed to the same atmospheric humidity and temperature. Figure 3.1 relates these terms to the drying of a spray droplet in a constant humidity air medium. Other terms used frequently in describing mechanisms are outlined below. 100 In the spray drying operation, the liquid to be removed is invariably water, although the removal of organic solvents in closed cycle operations is becoming more widespread. The drying principles involved for both water and non-water systems are the same, and thus in this chapter, the case of water evaporation into air will be taken to illustrate the drying principles involved. 3.1. Common Terms and Principles The removal of water from a feed to the extent of leaving its solids content in a completely or nearly moisture-free state is termed drying. The moisture in the feed can be present in two forms : bound and unbound moisture. The nature of the solids and accompanying moisture determines the drying characteristics. The bound moisture in a solid exerts an equilibrium vapour pressure lower than that of pure water at the same temperature. Water, retained in small capillaries in the solid, adsorbed at solid surfaces, as solutions in cell or fibre walls, or chemically combined with the solids (product water of crystallization) falls in the category of bound moisture. The unbound moisture in an hygroscopic material is that moisture in excess of the bound moisture. All water in a non-hygroscopic material is unbound water, which exerts an equilibrium vapour pressure equal to that of pure water at the same temperature. The equilibrium moisture is the moisture content of a product when at equilibrium with the partial pressure of water vapour of the surroundings. The free moisture is the moisture in excess of the equilibrium moisture and consists of unbound and some bound moisture, Only free moisture can be evaporated. The mechanism of moisture flow through a droplet during spray drying is diffusional, supplemented by capillary flow. The drying characteristics 43 0 BOUND MOISTURE 0 UNBOUND MOISTURE ›0 z T 0 EOUILIBRIU LI] 1.10ISTUR or 0 MOISTURE REMOVED DURING EVAPORATION MOISTURE CONTENT (free moisture) wt moisture unit wtdrysolid SPRAY DROPLET FROM ATOMIZER Figure 3.1. Graphical relation between common drying terms. Dry air is atmospheric air exclusive of accompanying water vapour, as apart from wet air, which is inclusive of water vapour. The water vapour content varies considerably from day to day and from place to place. Properties of dry air are given in Appendix 3, Properties of wet air are given by humidity (psychrometric) charts. Psychrometric charts relate air temperature and humidity, or air enthalpy and humidity. The former is the more commonly used. The abscissa is the dry bulb temperature (DB), the ordinate absolute humidity (H a ) and the parameter relative humidity (H„,). Air volumes, total heat content and wet bulb (WB) temperature (adiabatic saturation (AS) temperature) are also indicated. Parentheses are used here since the air—water system is unique, as for all practical purposes the (WB) and (AS) temperatures can be considered the same, and the wet bulb and adiabatic cooling lines coincide. The (WB) exceeds the (AS) temperature in all other systems. Psychrometric 44 DRYING TERMS AND PRINCIPLES BASIC PRINCIPLES, DEFINITIONS charts for air—water vapour systems covering normal to elevated temperatures are given in Appendix 5. Humidity defines the moisture content of the air. The amount of water vapour present in the air is independent of the air pressure (P T ) but it does depend upon the temperature of the air with which it is mixed, i.e. according to Dalton's Law. Thus for air—water systems, the absolute humidity (H a ) is related to the partial pressure (A y ) of the water vapour in the air in the following way 45 force it provides resisting drying. Vapour pressure is governed solely by temperature, and is directly related to drying rates. The vapour pressure of water at any temperature provides the forward driving force for drying. For- the air—water systems, the vapour pressure at a saturated surface (PwB ) is related to that of water in the surrounding air (P,,) by equation (3.4). The equation can be used to calculate wet bulb temperatures, see example 3.2 P,03 =P+ 29 C,PT A AT (3.4) 18 18( p w 29 PT — pw (3.1) Ha = C, = specific heat of vapour at constant pressure, 1 = latent heat of vaporization at wet bulb temperature, AT = temperature difference between surface and air (i.e. wet and dry bulb temperatures) where H a is expressed as weight of water vapour i lb \ gr unit weight of dry air \ lb lb or (g kg Absolute humidities for air—water systems at atmospheric pressure are read directly from psychrometric charts. Absolute humidities at pressures other than atmospheric, i.e. H a at pressure B, are given approximately by : 1 Ha(B) = Ha{cA-) + 0.622P4 1 1 PT — P‘,) (760 — (3.2) Pressure A = 760 mmHg where Pp' = vapour pressure of water at wet bulb temperature. Relative humidity (H„,) is the water vapour content expressed relative to the water content at saturation at the temperature of the mixture. The mixture humidity at saturation is designated 100 %. Alternatively the relative humidity can be expressed as the ratio. Ti re' = 100 partial pressure of water in air at temp (T) vapour pressure of water at temp (T) where (3.3) The addition of heat to a wet droplet is insufficient by itself to promote satisfactory drying. Removal of moisture depends upon the humidity of the surrounding drying air. To maintain high drying rates cool humid air must be moved from around a droplet and replaced with hot low humid air. The partial pressure of water in air is the pressure it would exhibit if existing alone in the same volume and at the same air temperature. The sum of partial pressures of components in a gaseous mixture equals the total mixture pressure. The partial pressure of vapour is the vapour pressure at dew point temperature (see equation (3.3)). Alternatively from Dalton's Law, the partial pressure is the multiple of total pressure and mol fraction of vapour. The significance of partial pressure concerns the reverse driving The dew point (saturation temperature) is the temperature to which wet air must be cooled at constant pressure before liquid will form through condensation. At the dew point, the saturation vapour pressure equals the partial pressure of water vapour in the air mixture. The dew point is not the temperature where all water vapour is condensed to leave dry air. If the air is cooled below the dew point, condensation continues. The amount of condensation depends upon the degree of cooling. The air is at a state of saturation at lower temperatures and the absolute humidity decreases by the quantity of water condensed. The dew point is related to vapour pressure data where the vapour pressure at dew point equals Pw . = P,.s x lire, ( 3.5) where Pw = vapour pressure at dry bulb temperature humidity expressed as a decimal Hrei relative = The dry bulb temperature of air is recorded by an ordinary thermometer when in thermal equilibrium with the air surroundings. The wet bulb temperature is recorded under steady state conditions by a thermometer, whose surface is saturated with liquid water and simultaneously exposed to a mixture of air and water vapour. The usual technique is to place a clean cloth around the thermometer bulb and thoroughly moisten the cloth. The thermometer must be placed in a strong air current (velocity > 900 ft/min (4.5 misec)) (379). The wet bulb temperature is lower than the dry bulb temperature. The difference (or depression) is proportional to the moisture evaporation from the wet cloth surface. The wet-bulb temperature in fact, corresponds 46 BASIC PRINCIPLES, DEFINITIONS DRYING TERMS AND PRINCIPLES to the temperature at which the air would normally be saturated without any change in its heat content. The upper limit of wet bulb temperature is the dry bulb temperature. The lower limit is the dew point. For saturated mixtures of air, wet and dry bulb and dew point temperatures are the same. The wet bulb temperature does not represent conditions of thermal equilibrium. It represents simultaneous heat and mass transfer the dynamic equilibrium between the rate of heat transfer to the thermometer bulb and the rate of mass transfer from the bulb. The driving force for moisture evaporation from a saturated surface is the difference between the water vapour pressure at the temperature of the surface and the partial pressure of water vapour in the surrounding air A y ). The driving force can equally well be expressed in terms of the difference in humidity at the saturated surface (H„) and the humidity of the air (H a ), i.e. H, — H a . Equation (3.1) relates the partial pressure of water vapour in the surrounding air to H a . At the saturated surface, the partial pressure of water equals its vapour pressure and thus substitution of p, for P„, in equation (3.1) gives the expression for H. The rate of mass transfer from a saturated surface equals : dW dt k A(H — H a ) = kgA(PwB Pw) g (3.6) w For dynamic equilibrium the rate of heat transfer is equal to the multiple of the rate of mass transfer and latent heat of vaporization. The rate of heat transfer from a saturated surface equals dQ dt W h A(T )= A (3,7) — T, B ) = k g (Hw H a )A (3.8) a Tw B dt combining equations (3.6) and (3.7) The coefficients h„ k g are incorporated with the humid heat (C s ) in the Lewis Number. This is unique in being unity for air—water vapour systems and results in the adiabatic cooling line and wet bulb line being the same on the psychrometric chart. This greatly simplifies dryer calculations of water containing solids dried in air. The humid heat (C s ) is the heat required to raise the temperature of a unit mass of air and its vapour one degree at constant pressure. It is expressed by C s = 0.24 + 0.45H a (3.9) The humid heat is used to calculate the heat for raising the temperatures of air—water vapour mixtures where Q a = ifiC s AT 47 (3.10) Equation (3.10) is valid so long as condensation or vaporization does not take place. The relationship between humid heat and humidity for air—water vapour systems at atmospheric pressure is given in Appendix 6. The enthalpy (heat) of a mixture of air and its water vapour is the sum of the air enthalpy and vapour enthalpy. Enthalpies are relative to a given reference level (Tr ) taken as air and saturated liquid water at 32°F (0°C). For air—water vapour systems (3.11) Q a = (0.24 + 0.45H a )(T — 7) + ~.H a where A is the value at the reference temperature. The relationship between temperature and the latent heat of vaporization of water is given in Appendix 7. Drying characteristics of droplets during spray drying are best illustrated by plotting the variations in evaporation rate and accompanying changes in droplet temperature and vapour pressure as droplet moisture decreases. Figure 3.3(a) illustrates the droplet temperature change for a droplet containing 50 % moisture contacted with hot air 290°F (143°C) (humidity 50 gr/lb (7 g/kg), equivalent WB temperature = 105°F (40°C)). The plot shows that although a spray dried product comes into contact with hot air, at no stage during the process does the product temperature become excessive to cause product degradation. The product is removed from the dryer long before the product temperature has time to rise to approach the temperature of the exhaust drying air. Figure 3.3(b) shows the vapour pressure change during the droplet drying. The vapour pressure during the initial drying period is that at the WB temperature 105°F (40°C), which is 2.24 in Hg (see Appendix 4). Figure 3.3(c) shows the rate of drying curve. The ordinate expressed in weight moisture evaporated per unit time per unit area is often termed the drying flux. The falling rate curve shown shows the basic phases. Different shapes are obtained for different products and different conditions. For more detailed treatment of drying principles the reader is referred to Perry (91), Coulsen and Richardson (98), Blackadder and Nedderman (500), and Cremer (501). 3.2. Applying the Psychrometric Chart to the Spray Drying Process The psychrometric chart provides all data pertaining to a wet product in contact with air. Common applications include determining the evaporative capacity of a dryer, droplet/particle temperatures and necessary air conditions for product conveying and handling packing. •▪ - 48 ZE cc ci BASIC PRINCIPLES, DEFINITIONS DRYING TERMS AND PRINCIPLES DRY BULB TEMPERATURE AT DRYER OUTLET 160- 300 —1 cc Z• t )_ 800 49 LL LI_ 600 TEMPERATURE 150- 700 MOISTURE CONTENT AT DRYER OUTLET 140- 0 cc la- 500 cc 300 I CRITICA PO I N r L 130- DROPLET ENTERS DRYER EVAPORATION AT DECREASING RATE 120- EVAPORATION AT CONSTANT RATE 110 25 3 2 u_ i=} 100 1— = DRY BULB TEMP 15 20 25 5 TEMPERATURE °F 55 60 30 35 40 45 50 MOISTURE CONTENT PERCENT IN DROPLET EQUILIBRIUM MOISTURE CONTENT IU WET BULB o a o. HUMID HEAT 378 c0180 Lu cc iri D ci 1418 ;< cc z¢ oc)140 7 cc )ci ( ris 2.6 c .._ 1_ a.1 AIR AT DRYER OUTLET 160' F 0,8 15 R H 4CeF D.P 2.4 - 0 I- ci WO Lu Z .4,-. Ee 105.5 rx U °- 12 L_ =.0 a. -135 cox uct_ D LI 0 2-24 _ ❑ 2.2 - EVAPORATION AT CONSTANT RATE 2.D - ❑ yr to a' L. a -130 ix EVAPORATION AT DECREASING RATE 1-6 1 1 MOISTURE CONTENT LEAVING DRYER VAPOUR PRESSURE OF MOISTURE IN AIR AT DRYER OUTLET lu 1422 14` 0 30 50 55 60 65 70 DRY BULB TEMPERATURE (°F) 75 80 85 95 90°F DRY BULB 100 DROPLET ENTERS DRYER CRITICAL POINT 1-0 - 1• 2 5 10 15 20 25 30 35 40 45 50 55 Moisture content of droplet % b. Figure 3.2. Two applications of the psychrometric chart in spray drying. (a) Estimating droplet surface temperature, (b) Conveying air conditions. b. Figure 3.3. Drying characteristics of droplets during spray drying. (a) Variation of droplet temperature during drying. (b) Variation of droplet vapour pressure during drying. 50 DRYING TERMS AND PRINCIPLES 51 BASIC PRINCIPLES, DEFINITIONS EXAMPLE 3.1 The dew point of air sampled at the base of spray dryer is 115°F (46°C), If the chamber pressure is 10 mm of water below atmospheric, what is the air humidity in this region? Data : Barometric pressure 29.92 in Hg (760 mm Hg), vapour pressure of water (Pw ) at 115°F = 2.995 in Hg (from Appendix 4). Now er 0 a. u.1 U cc CC FD2 1 2 CONSTANT RATE INTERNAL MOVEMENT CRITICAL OF MOISTURE POINT CONTROL'LIN G UNSATURKHED SURFACE DRYING crz cob u0_ UZ DRYING RATE FALLING RATE 0 0 25 1 mm water = 0.0029 in Hg chamber pressure = 29.92 — (10 x 0.0029) 29.891 in Hg DROPLET ENTERS DRYER , PT = 29.891 in Hg H MOISTURE CONTENT OF DRIED PARTICLE LEAVING DRYER I 15 20 25 30 35 40 45 b The humidity is calculated from equation (3.1) by substitution of (at Dew Point) Pw p,, = 2.995 in Hg T I = 0.066 lb water lb dry air EXAMPLE 3.2 50 MOISTURE CONTENT.( PERCENT) C. Figure 3,3 continued. Drying characteristics of droplets during spray drying. drying curve. 2.995 18F L29.891 — 2.995 a= (c) Rate of The determination of the theoretical moisture removal from a spray dryer is illustrated in example 3.2. The droplet surface temperature is shown in figure 3.2(a) by a droplet contacted with air 262°F (128°C) containing 35 gr/lb moisture, It is that temperature where the adiabatic (wet bulb) cooling line (which passes through the drying air conditions) intersects the dew point line. Data on air conveying conditions are often essential where dried product specifications impose stringent control of wet air in contact with product, i.e. where product is highly hygroscopic. Figure 3.2(b) illustrates how the dew point (DP) 69°F (20.5°C) of conveying air 90°F (32°C) DB, 75°F (24°C) WB can be obtained, so as to ascertain whether this DP is likely to be reached during plant operation, and whether an air heater will ever be necessary to prevent condensation conditions. The figure also shows the total humidity to be 106.5 gr/lb (15.2 g/kg), If experience has shown the dry product to rapidly take in moisture from such wet air, some form of air conditioning must be used to lower the absolute humidity. Droplets of aqueous slurry are sprayed from a nozzle into air at 240°F (116°C). An air sample is drawn off the atomization zone and the dew point determined. Assuming the droplet surfaces are still saturated at the point of air sampling, calculate the droplet temperature. Barometric pressure = 2992 in Hg. With the above assumption, the droplet temperature is the same as the wet bulb temperature. Equation (3.4) can be applied using a trial and error method to calculate the temperature (T s ), where P,„ = 3.446 in Hg PT = 29.92 in Hg C, = 0.24 BTU/lb °F AT = (240 — Ts ) °F Substituting values in equation (3.4) A 3.446 = P„ 11.6 7: Trial and error method. Let TS = 140°F 2 = 1014 BTU/lb AT = 100°F PwB (from Appendix 4) = 5.881 in Hg 52 BASIC PRINCIPLES, DEFINITIONS DRYING TERMS AND PRINCIPLES Substituting in equation (3.4) 3.446 = 5.881 — 1.144 3.446 0 4.737 By further trial and error, the value of is = 131°F gives satisfactory equality of the equation Ts = 131°F = 1019 BTU/lb P„ = 4.647 in Hg 3.446 4.647 — 1.242 = 3.405 droplet temperature = 131°F (55°C). EXAMPLE 3.3 A spray dryer is supplied from atmosphere with air containing 50 gr/lb dry air (7 g/kg). Air enters the dryer at 300°F (149°C). For maintenance of the specified moisture content in the product, the humidity of air leaving the dryer is maintained at 15 % relative humidity. Calculate the theoretical quantity of moisture that can be removed in the dryer, and the temperature drop through the dryer. Although the air is heated to 300°F, it still retains a moisture loading of 50 gr/lb. The maximum theoretical amount of moisture that can be taken up by the dryer is the amount required to saturate the drying air. in practice, saturation is never achieved, and for most spray dryer operations, where outlet temperatures are well above atmospheric temperatures, the relative humidities are kept low to enable rapid completion of product drying. Hence, using Appendix 5.2. For inlet air, T = 300°F, H a = 50 gr/lb, the corresponding wet bulb temperature is 106°F (41°C). Now : 106°F WB is equivalent to 360 gr/lb. Moisture required to saturate drying air = 360 — 50 = 310 gr/lb (44 g/kg), For an outlet relative humidity of 15 %, the final air conditions can be obtained from the chart (Appendix 5.2). For the ideal case, the total heat in the air is the same initially as it is finally, if the product is considered not to receive heat or release heat to the air during the drying. Therefore, reading along adiabatic cooling line : at 15 % RH, the corresponding dry bulb temperature is 166.5°F (75°C) having a dew point of 96°F (36°C). For dew point of 96°F, equivalent moisture loading = 260 gr/lb (37 g/kg). Therefore (a) Theoretical moisture removal in the dryer = 260 — 50 = 210 gr/lb of dry air (30 g/kg). (b) the temperature drop through the dryer = 300 — 166.5 = 133.5°F (56°C). 53 In reality to achieve the above moisture removal, inlet drying temperatures above 300°F are required to supply the added heat to raise the temperature of the product within the dryer, and to allow for the heat losses from the dryer structure. The calculation accounts for heat supplied by the drying air for moisture evaporation. The additional product temperature requirements can be calculated from the specific heat data of the dried product. Heat losses from the dryer can be calculated from standard procedures involving convection, and radiation losses from the dryer structure. Such procedures are to be found in standard heat transfer textbooks (9, 10). EXAMPLE 3.4 Air at 96•5°F (36°C) and 30 % RH enters a cooler which supplies air to the base of a spray dryer. The presence of cooled air completes product crystallization. The product leaves the spray dryer with a sticky texture, although at low moisture content. What is the temperature the cooler exit air must exceed to prevent saturated air passing to the dryer base? Method I (From Appendix 4) Vapour pressure of water at 96.5°F (36°C) = 1.74 in Hg Substituting in equation (3.5) Vapour pressure at dew point = 1.74 . 0.3 = 0.522 in Hg (13.25 mm Hg) Dew point corresponding to this vapour pressure = 60°F Method II The above result can be read directly off the psychrometric chart. At the intersection of the dry bulb temperature line of 96.5°F (36°C) and relative humidity curve of 30 %, draw the horizontal line to intersect the saturation line. Point of intersection is the point 60°F. The cooler exit air temperature must exceed 60°F (16°C). 55 4,1. Introduction Spray dryer performance is an expression of the thermal efficiency of the process and in practical terms defines the ability of the dryer to produce the desired product specification economically. Dryer design is directed towards achieving desired dried product properties at highest possible thermal efficiencies. The thermal efficiency of a spray dryer depends upon the operation temperatures. It is defined as the ratio heat used in evaporation heat input As it is normal practice not to recover the heat content in the air exhausted from the drying chamber, the thermal efficiency is increased by increasing the temperature of the air entering the chamber and operating the dryer at an outlet temperature as low as the process allows. The whole basis of economic operation is the utilization of heat passed into the dryer, i.e. the dryer heat load, or the heat input required for producing a unit weight of dry product. The heat load is proportional to the evaporation rate, and for a given rate is greatly affected by the solids content in the dryer feed. As seen from figure 4.1 it is economically important to operate at as high a solids content as possible. For a given production rate, increase in feed solids content from 10 to 25 % will result in a 66.6 % reduction in heat load. Even increasing the solids content from 25 to 50 % will result in a similar heat load reduction. For feeds of high solids content (50 % and over) substantial reductions in heat load can still be obtained by continued solids content increase. Increase from 50-60 % will result in a reduction of heat load of nearly 50 %. To utilize these savings atomizer development seeks designs to atomize feeds of higher solids content satisfactorily at high feed rate. MOISTURE FOR EVAPORATION HEAT LOAD 4 Performance of Spray Dryers UNIT WT OF BONE DRY SOLIDS IN•FEED PERFORMANCE OF SPRAY DRYERS 10 6 6 4 2 0 0 20 40 60 80 100 PERCENTAGE SOLIDS IN FEED Figure 4.1. Effect of feed solids content on dryer heat load. 4.2. Heat and Mass Balances over Spray Dryers Air—product flow and temperature data for assessing dryer performance are obtainable from heat and mass balance data. For continuous operation with negligible product hold-up in the drying chamber, the mass input of air and feed per given time equals mass outputs of air and product. Heat input of air and feed equals heat output of air and product plus the heat losses from the drying chamber. For semi-continuous operation, shu down if often due to build-up of product in the dryer. The difference i product input and output equals the accumulation. Heat and mass balances are drawn up below with reference to figure 4. For calculation of air feed and product enthalpies, a reference temperatur of the water freezing point is used. It is common to base moisture balance on a unit weight of bone dry product. Suppose M s wt units/hour of dry soli enter the spray dryer in a feed (solution, slurry or paste) containing (W s ) i w units moisture/unit dry solid. The feed is dried to give solids leaving th dryer with a moisture content of (Ws ), wt units moisture/unit dry solid. The feed temperature when atomized is (Ts ), and product is discharged at a temperature of (Ts ), . Drying air is supplied to the dryer at a rate of G a wt units dry air/hour at temperature (71. The inlet absolute air humidity is 56 57 PERFORMANCE OF SPRAY DRYERS BASIC PRINCIPLES, DEFINITIONS Heat input = heat outlet + heat loss (%) (Td ( )(1) (4.4) thus Ga(Qa)i + M5(Qs)1 = Ga(Qa)2 + WW2 + QL (4.5) where (T)( 0° ( 1-12 ) ) Q L = heat losses from the dryer outer cladding and structural supports. The heat loss is expressed by the standard heat transfer equation _ Q L = UAAT ( Ms ) ( 5)2 ( Gs ) ( Ws ) Figure 4,2. Dryer data for calculation of heat and mass balances. H 1 , and increases during the dryer operation to H2 . The air leaving the dryer is (Ta ) 2 (4.6) For well-insulated drying chambers heat losses are low. For non-insulated drying chambers, or chambers designed with cooling air jackets to maintain cool dryer walls (when handling many hygroscopic and heat sensitive products) heat losses from the dryer are high. Q L becomes a significant term in equation (4.5). The enthalpy of the feed (42 5 ) 1 as it enters the atomizer is the sum of the enthalpy of the dry solid and the moisture as liquid. Thus (4.7) (Qs)1= CDs(AT) + (Ws)iCwAT where Moisture balance Moisture entering in feed Moisture entering in hot air Moisture leaving the dryer in the dried product Moisture leaving in the exhaust drying air CDS = heat capacity of dry solid (MS) (141s)1 C w — heat capacity of moisture (in liquid form) AT = difference in temperature between feed temperature and the reference temperature level (water freezing point) (G a)H, Ms(W5)2 GaH 2 For no product accumulation in the chamber input = output (4.1) m5( 14701 + G.(111) = Ms ( W)2 + Ga H2 (4.2) thus or Ms((W)1 (Ws)2) = Ga(H2 H1) By similar procedure. Enthalpy or heat balance Enthalpy of air entering dryer -- G a (Q a ) 1 Enthalpy of feed entering dryer = M 5 (Q S ) 1 Enthalpy of exhaust drying air = G a (Q a ) 2 Enthalpy of dried solid = M5(Q02 (4.3) The enthalpy of the drying medium (Q a ) whether entering or leaving the dryer is expressed in terms of the humid heat, absolute humidity, and the latent heat of vaporization of water at freezing point, where Q a = QA T) + (4.8) If additional air is added to the chamber either in the form of cooling or conveying air, the enthalpy of this air flow must be added to the left-hand side of equation (4.8). The equivalent weight of air must be added to the value of (G a ) on the right-hand side of equation (4.5). EXAMPLE 4.1 2060 lb/hr of dried product (4 % moisture) is produced from a co-current flow spray dryer incorporating a rotary atomizer. Atmospheric air (75°F) (50 % RH) is heated to 350°F before entering the dryer. Air is exhausted from the chamber at 176°F. Feed (45 % solids by weight) is pumped to the 58 BASIC PRINCIPLES, DEFINITIONS PERFORMANCE OF SPRAY DRYERS atomizer at 80°F. Dried product temperature is 115°F. What is the air rate if heat losses from the dryer are estimated at 95 000 BTU/hr? 2060 x 96 Feed rate to dryer M, = Enthalpy balance Enthalpy entering dryer 100 89.2G a + 1980(77.8) BTU/hr x - = 4400 lb/hr 45 100 Enthalpy leaving dryer Moisture in feed (1470, = 55 45 = 1.22 lb/lb dry solid Moisture in driedproduct (WO , 4 59 36.7(1980) + G a (34.6 + 1140H 2 ) From equation (4.5) -- 0.042 lb/lb dry solid 89.2G a + 1980(77.8) = 36.7 x 1980 + G a (34.6 + 1140H 2 ) + 95 000 Heat capacity of dry solids C ps = 0.4 BTU/lb °F Absolute humidity of inlet air H, = 0.0095 lb/lb dry air (75°F, 50% RH) Enthalpy of inlet air (equation (4.8)) (reference temperature 32°F) Combining equations (A) and (B) 54.6G a - 13 700 1140 (C) G a H 2 = 2340 + 0.0095G a (D) G a H2 = (Qa)i = (0.24 + 0.451-1 1)(aD1 - 32) + 1075.2(H 1 ) = 77.7 + 10.2 = 89.2 BTU/lb Enthalpy of outlet air (exhaust) (B) 54.6G a - 1140H,G a = 13 700 From equations (C) and (D) (Qa)2 = (124 + 0.45H 2 )(176 - 32) + (1075.2H ) 54.6G a - 13 700 = 1140(2340 + 0.0095G a ) 2 = (34.6 + 1140H 2 ) BTU/lb 54.6G a - 13 700 = 2 670 000 + 10.8G a Enthalpy of feed entering dryer (equation (4.7)) G a = 60 600 lb/hr (Q s )i = 0.4(80 - 32) + 1.22. 1. (80 - 32) Humidity of outlet air (H2) = 19.2 + 58.6 = 77.8 BTU/lb 11 2 Enthalpy of dried product leaving dryer 2340 + 0.0095G a - Ga 2340 60 600 + 0.0095 (Q s ), ---- 0.4(115 - 32) + (0.042)1 . (115 - 32) = 33.2 + 3.5 = 36.7 BTU/lb = 0.0386 + 0.0095 = 0.0481 lb/lb (337 gr/lb dry air) Moisture balance at 176°F-relative humidity = 15 %. NB. If operation had been adiabatic, i.e. no heat loss from the dryer, the required air rate for the given conditions becomes 58 600 lb/hr. Basis Dry solids dried per hour = 2060 x 96 = 1980 lb/hr 00 Moisture entering in feed Moisture leaving in product .'. Moisture evaporated Moisture gained by air = 1980 x 1.22 1b/hr = 1980 x 0.042 lb/hr = 1980 x (1.178) = 2340 lb/hr = moisture lost from feed 4.3. Dryer Efficiency From equation (4.3) G a (H 2 - 0.0095) = 2340 (A) Hot air enters the dryer chamber, and due to moisture evaporation from the spray, the air temperature falls during air passage through the drying chamber. If the chamber is well insulated, the heat losses to the surroundings can be assumed negligible, and the fall of air temperature follows the 60 BASIC PRINCIPLES, DEFINITIONS PERFORMANCE OF SPRAY DRYERS adiabatic cooling line, as depicted on the psychrometric chart (Appendix 5) and figure 4.3. Maximum possible evaporation from a given air flow is obtained, if the air is exhausted in its saturated state. This never occurs in actual spray dryer practice, although there are cases when producing very moist powders, when approach to saturation can be close. Relative humidity is generally low at the dryer outlet. Example 3.3 (page 52) shows calculation of the theoretical moisture that can be removed in a spray dryer for a given set of air conditions. If the air is considered to enter a spray dryer at a temperature T 1 after being heated from atmospheric temperature To , and that during the drying process the air temperature falls and air is exhausted at a temperature of T2, the efficiency of process can be expressed as follows EXAMPLE 4.2 Atmospheric air at 74°F (23°C) and 30 % RH is heated to 300°F (149°C) and passed to a spray dryer. The air is exhausted at 180°F (82°C) and 9 % RH. Determine : (a) maximum thermal efficiency (ideal case), (b) overall thermal efficiency, (c) evaporative efficiency, (d) degrees of heat and percentage heat not used for evaporation. The drying process can be represented on a psychrometric chart, figure 4.3. cr) z 0) LD (a) Overall thermal efficiency (n o „ raii ) is defined as the fraction of total heat supplied to the dryer used in the evaporation process. It can be approximated to the relation [T, — I /overall = z 0 T21 T, — T o 61 100 (4.9) • 350 where T2 = the outlet temperature if the operation was truly adiabatic. Inspection of equation (4.9) shows a rapid increase in overall efficiency on increase in inlet temperature for fixed outlet and ambient conditions. For outlet and ambient temperatures of 185°F (85°C) and 68°F (20°C) the overall efficiency is 43.5 % at an inlet temperature of 275°F (135°C); 74 % at 518°F (270°C) ; 87.5 % at 1004°F (540°C); and 89.5 % at 1202°F (650°C). (b) Evaporative efficiency (ri e „,) is defined as the ratio of the actual evaporative capacity to the capacity obtained in the ideal case of exhausting air at saturation. It can be approximated to the relation Lu I— I-0 210 0 38 55 74 T. 105 300 TT 160 189 TEMPERATURE ° F l evap T, [ Ti — T2 Tat_ 100 (4.10) where Tsai = the adiabatic saturation temperature corresponding to the inlet air temperature (T1 ). Although high efficiencies are obtainable for higher inlet air temperatures, there are limitations to how high temperatures can be raised and yet still obtain better performance. Firstly there is a temperature level above which the heat effects on the atomized spray become too severe and where product will degrade. Secondly extra cost of air heating beyond a certain level may not be justified and thus the inlet air temperature may reach a maximum from an economic viewpoint. Figure 4.3. Drying process represented in example 4.2. (a) Maximum thermal efficiency (ideal case) is obtained by exhausting the drying air in a saturated state. The air temperature at saturation is obtained from the intersection of the adiabatic cooling line through (T 1 ) and the 100 % relative humidity line. From figure 4.3 wet bulb temperature of drying air = 105°F (41°C), hence : heat used in evaporation heat input 300 — 105 100 = 300 — 74 195 100 86 .4% 226 1 This is given by equation (4.9). T2 is (b) Overall thermal efficiency (n,ove calculated as follows : The absolute humidity of exhaust air is 210 grulb 62 BASIC PRINCIPLES, DEFINITIONS PERFORMANCE OF SPRAY DRYERS (30 g/kg), corresponding to 180°F (82°C) at 9 % RH. For adiabatic conditions, absolute humidity level in the exhaust air remains the same, and the required temperature is where the absolute humidity line intersects the adiabatic cooling line used in (a) above. From figure 4.3 this temperature is 189°F (87°C). Thus the equation (4.9) [ 300 — 181 //overall 111 100 = [-- 300 --74 1891 = "" 300 L — 105 100 = [ 111 1100 = 57 % 195 300 — 180] 9 [ [ 9 -= 7.5%. 120 4.4. Residence Time in Drying Chamber Drying chambers are designed to handle an air volume containing sufficient heat for drying the spray droplets, and to provide an air residence time sufficient for droplets to be dried to particles of desired moisture content. Initial drying rates are very high in the first period of drying when the majority of moisture is evaporated in very short time intervals, but during the second period of drying, rates fall off quickly and more time is required to evaporate product down to low moisture content. Many extra seconds are required to evaporate the last few percentages of moisture to bring the final moisture down to the desired moisture content. Drying rate curves for a droplet can give information on residence times necessary in drying, but due to difference in evaporation characteristics of single droplets and sprays, residence time requirements are usually established on pilot plant dryer facilities. The minimum residence time of product can be assumed to be the average residence time of air. This is calculated by dividing the chamber volume by the total air rate. Air volume at the outlet temperature is used. Chamber designs incorporate cylindrical, conical or rectangular forms, and chamber volumes (V) can be calculated from : Cone Cylinder (4.13) where D c h is chamber diameter, b = breadth, L = length, h height. For conical based drying chambers of cylindrical height (h') and cone angle (60°) the volume can be expressed as (dimensions in ft) V = 0.7854DL(h' 0.2886k h ) 100 = 49.2 (d) (i) degrees of heat lost to evaporation due to the heat losses from chamber and product heating = 189 — 180 = 9°F (5°C) (ii) percentage heat lost = V = bLh (4.14) 2261 (c) Evaporative efficiency (n evap,) • This is given by equation (4.10). The saturated air temperature is 105°F. Thus substituting in equation (4.10) 11 Rectangular (box) 63 V = A-hD c2, (4.11) hD 2h c (4.12) = 4 Most of the product during passage through the •dryer has a residence time much higher than the average air residence time. This is due to (a) particles enter recirculating air flow regions in the chamber, (b) particles remain suspended at the chamber wall or fall at lower velocities due to air velocities being lower than the average air velocity through the chamber. For drying chambers with primary product discharge from the chamber and secondary separation from the powder recovery section, only the fines fraction passing to the recovery section will experience the minimum residence time. This fraction contains fine particle sizes, and their size will enable drying to be completed to the moisture content of the product recovered from the primary product discharge point, even though the primary product will have experienced greater residence times. For drying chambers with total product discharge at the recovery section, a greater proportion of the product will experience residence times in the order of the average air residence time. Drying chambers must be sized, therefore, to provide a residence time optimum for a given product. The optimum residence time is the time for completion of desired moisture removal at minimum temperature increase of dried product temperature. It follows that coarse sprays require longer residence times in the dryer than fine sprays for the same inlet air temperature. Where low drying air temperatures are required for highly heat sensitive products, transfer driving forces are low and residence times are very long. This can lead to drying towers of great height. Dryer designs are available that cover the entire range from short (5 seconds) to long (several minutes) residence times. The longer the residence time the larger the structure for a given evaporative capacity. Products that can withstand turbulent air handling and contact with hot air temperatures can be effectively spray dried in mixed flow dryers (cyclone type), see figure 5.9(a), at short residence times. For products that can withstand hot temperatures, but a minimum of air turbulence, tall drying towers of high residence time are required as near free falling droplet velocities conditions are achieved in the dryer. For the many products that are dried in co-current flow dryers with rotary air flow, intermediate residence times (20-40 seconds) prevail. 64 BASIC PRINCIPLES, DEFINITIONS EXAMPLE 4.3 126 000 lb/hr air pass through a co-current flow conical based spray dryer (60° cone) of 24 ft diameter and 20 ft cylindrical height. If the outlet drying temperature is 176°F what is the minimum residence time in the chamber? Volume of chamber given by equation (4.14). Substituting in values V = 12 200 ft 3 5 Equipment Incorporated in Spray Dryers Air rate = 126 000 lb/hr 000 359 Volume at 176°F = 126 x 636= 33 700 ft 3 /min 60 29 x 492 Minimum residence time = 12 200 x 60 = 217 sec 33 700 5.1. Introduction Many spray dryer designs are available to cover the wide range of product applications. Although designs are diversified, each design contains standard equipment, which can be classified into four categories : A. Heating of the drying air ; air heaters with accompanying fans, air filters, dampers and ducts. B. Atomization of feed into a spray; atomizer with feed supply system of pumps, tanks and feed pretreatment equipment. C. Contacting of air and spray, and drying of spray ; drying chamber complete with air disperser, product and exhaust air outlets, D. Recovery of dried product ; complete product recovery system with product discharge, transport and packing. Air exhaust system with fans, dampers and ducts. Equipment items are discussed generally in this chapter. More detailed discussion of the more important equipment items is given in section IV (chapter 12). 5.2. Passage of Air and Product through a Spray Dryer The passages of air and product through a spray dryer are shown diagrammatically in figure 5.1. The air intake is from atmosphere, unless the spray dryer is operating under closed cycle with a special gaseous medium, when recycling is employed. The air is first filtered, then heated. The filter can be dispensed with, if entry of atmospheric dust into the heater and drying chamber does not jeopardize dried product quality. Direct or indirect air heating can be used depending upon the product spray dried. 66 EQUIPMENT INCORPORATED IN SPRAY DRYERS BASIC PRINCIPLES, DEFINITIONS 67 AIR EXHAUST OLOINE FEE D FILTER PUHP ATOMIZER 0- PRODUCT AIR DISPERSER ATOMIZER (rotary ) L- FEED SYSTEM AIR HEATER LID .ED AIR AIR FILTER AIR DRIARR HEATER CHAMDER AIR PRODU4 RECOVERY FEN i RTA'RE —P- EEPUIPMENT EXHAUST FAN FAN FILTER FEED TANK AIR SUPPLY SYSTEM CYCLO'vE AIR EXHAUST SY51EN Figure 5.1. Product and air passage through a spray dryer. D PUMP FILTER Flow of air through the heater is by a supply air fan located at the heater inlet. In some dryers especially those of smaller capacity, the exhaust fan is sized to draw sufficient supply air through the heater. In a one fan system, the drying chamber operates under a higher negative pressure than when a two fan system is used. A supply fan can balance the pressure in the chamber. The dryer feed, i.e. a solution, suspension or paste is pumped or gravity fed to the atomizer located within the drying chamber. The feed must be strained. The atomized spray readily undergoes drying within the chamber. Dried product of required moisture content is discharged at the base of the chamber or borne away with the exhaust air for recovery in the product recovery system. Air is drawn from the chamber and through the product recovery system by the exhaust fan. The product recovery system separates out entrained powder prior to venting the air to atmosphere. The exhaust air can contain much heat, and a heat recuperator can be installed before the air passes to atmosphere. The temperature of the outlet air is controlled through adjustment to the inlet air temperature at constant feed rate, or through adjustment of feed rate at constant inlet air temperature (see chapter 10 on dryer control). - Equipment items mentioned in figure 5.1 are standard to basic spray drying layouts. Two such layouts, featuring rotary atomization (figure 5.2(a)) and nozzle atomization (figure 5.2(b)) illustrate the position of equipment items in relation to the drying chamber. PRODIJE T RECOVERY a, AIR ExFIALLST AIR DISPERSER ATOMIZER (nozzle) AIR NEATER FAN F AN FILTER :yc LONE FEED TANK 1=1 PUMP FILTER 5.3. Equipment Items Making Up a Spray Dryer Layout 5.3.1. Equipment Comprising the Feed System The feed system comprises of suitable holding and feed tanks, strainers or fine filters, and feed pumps. A feed pump transfers the product to the ERY b. Figure 5.2. Spray dryer layouts with rotary and nozzle atomization. (a) Layout with rotary atomizer, (b) Layout with nozzle atomizer. --0-.10-- atomizer either directly or via a constant head feed tank. The holding tanks are of sufficient volume to enable continued plant operation, even though supply of product to the tanks may be intermittent. It•is quite usual for two holding tanks to be used alternatively thus assuring constant product supply to the dryer. The feed strainer or filter is important as all matter likely to jeopardize the performance of the dryer through partial or total blockage of the atomizer must be removed. The feed system is designed to enable easy cleaning and maintenance, Piping is normally laid out to enable recycling of product or washing fluids through the complete feed system via the holding tanks. Choice of metallic piping depends upon the feed. With food products, for example, stainless steel is used throughout. Applications in the chemical field often require specially lined holding tanks and corrosion resistant pumps, pipes and pipe fittings. The pumps are sized and selected for each application. Pumps most widely used are the rotary positive displacement type. Diaphragm pumps are suitable when feeds contain irregular shaped insoluble solids. Further details on pumps and pump selection are given in chapter 12. There are cases where pretreatment or preheating of the feed is required prior to atomization. Pretreatment can be the blending in of additives, or feed dosification to maintain required feed properties, such as a pH value. Preheating invariably is conducted to lower the feed viscosity in order to ensure required atomizer performance. Preheaters can be of the plate, shell and tube, scraped surface or spiral tube type. The type is selected according to the feed, heat transfer rates, available space and cleaning requirements. Pretreating and preheating equipment is connected into the feed system just before transfer of product to the atomizer. A piping diagram for a feed system involving a preheater is shown in figure 5.3. Feed from holding tanks is transferred through the preheater into a smaller feed tank prior to pumping to the atomizer. Feed from the preheater can be pumped directly to the atomizer, but the inclusion of a small intermediate (atomizer) feed tank aids flexibility in the feed system, by providing possibilities for dosification of products that cannot withstand passage through a preheater, feed recycling and visual control of feed supplies to the atomizer. A water tank for dryer start-up and shut-down is mounted by the atomizer feed pump. 5.3.2. Atomizer The atomizer is often regarded as the heart of the spray drying process. The ability of the atomizer to produce sprays of desired droplet size distribution is a most important factor in determining the success of the process. Two basic types of equipment are used rotary atomizers and nozzle atomizers (figure 5.4). Main design and operation features were introduced to the reader in chapter 1. Atomizer equipment is discussed in greater detail in chapter 6. 69 Figure 5.3. Feed system involving a feed pre eater. EQUIPMENT INCORPORATED IN SPRAY DRYERS BASIC PRINCIPLES, DEFINITIONS CONDEN SATE 68 70 EQUIPMENT INCORPORATED IN SPRAY DRYERS BASIC PRINCIPLES, DEFINITIONS 71 COUPLING TO MOTOR DRIVE FEED PIPE GEARING TOP BASE LIQUID DISTRIBUTOR SIDE BASE W - VANED WHEEL SIDE TOP a. FEED PIPE CONNECTION I FEPIALEI NOZZLE ORIFICE z NOZZLE HEAD END MIDDLE Figure 5.5. Atomizer positioning in drying chamber. Figure 5.4. Basic types of atomizers. (a) Rotary atomizer (atomizer wheel). (b) Nozzle atomizer. Whatever atomization technique is used, the atomizer is positioned within the drying chamber and operated so that the spray has intimate contact with the drying air. Contact can be made as the air flows upwards, outwards or downwards. In each case moisture evaporation from the spray in the vicinity of the atomizer is fast enough to dry the feed sufficiently before the spray comes into the neighbourhood of the chamber wall. Insufficient drying leads to semi-wet deposits on the wall. Atomizer positioning in the dryer is illustrated in figure 5.5. 5.3.3. Equipment Comprising the Supply Air System The supply air system delivers drying air to the chamber. Equipment involved are filters, heaters, dampers, ducts and fans. The supply air is filtered unless possible resulting contamination of the spray dried product by dust in the air can be tolerated. Atmospheric air is the usual supply source. In cases of closed cycle drying, the exhaust drying medium is filtered, re-cycled, passed through conditioning equipment and returned to the heater. Filter media are capable of removing airborne particles above 5 micron. The filter housing can consist of cages in which squares of filter medium are clamped. The filter squares are removed periodically for manual washing. More automatic arrangements are available where the pressure drop over the filter is measured continuously. On reaching a set pressure drop value the filter roll moves forward bringing a clean filter surface into operation thereby reduding the resistance over the filter. The filter rolls are replaceable. 72 EQUIPMENT INCORPORATED IN SPRAY DRYERS BASIC PRINCIPLES, DEFINITIONS Air heaters are either the indirect or direct type. Heating sources can be steam, fuel oil, gas, heat transfer fluids or electricity. Selection depends upon the product being spray dried and fuel availability. Groups of products can be classified according to their heater requirement. Group A. ProduCts that can withstand high temperature and be contacted with products of combustion. Oil or gas fired direct heaters are applicable. Examples of such products include clays, and mineral ore concentrates, and many inorganic materials. Successful use of direct oil heaters in many cases requires clean products of combustion. Burning of high quality oils is essential. Group B. Products that can withstand high temperatures, but must remain free of contact with products of combustion. Oil or gas fired indirect heaters are applicable. Examples of such products include various inorganic salts and fertilizers. Group C. Products that can withstand products of combustion but are subjected to limitations in temperature due to chemical changes or likelihood of ignition. Oil or gas fired direct air heaters are applicable, subject to a built-in automatic high temperature alarm system. Dilution of combustion products is used to maintain suitable air temperatures. Examples of such products include various organic and inorganic salts. Group D. Products which cannot be subjected to high temperature conditions or be contacted with products of combustion. Indirect air heaters must be used. In small units, liquid phase or electrical heating is often applied. Products in this grouping include foodstuffs and many fine chemicals. Heaters are discussed in chapter 12. Supply air fans are of the centrifugal type. Backward curved impellers are used as high volume air movement is achieved at low pressures. Fans are discussed in chapter 12. Dampers are of the butterfly type. 5.3.4, Air Disperser and Drying Chamber Air enters the drying chamber through the air disperser. The function of the air disperser is to provide the required heat for drying, control droplet/ particle travel during drying and remove the vaporized moisture from the chamber. Where the air disperser and atomizer are located together, air flow can influence the droplet size distribution of the spray. The function of the drying chamber is to provide air/particle residence times for obtaining desired dried product moisture levels without heat degradation and unwanted wall deposits. Product discharge must be continuous and the method of discharge conducive to the desired form of dried product. Drying chambers are designed to discharge the majority of the product at the base (primary product discharge) or to convey all the product with the 73 7:n ‘+ Cd a Cd g sir 45 =o a ❑, t„.1 5 74 BASIC PRINCIPLES, DEFINITIONS EQUIPMENT INCORPORATED IN SPRAY DRYERS exhaust air to a product separation and recovery unit (total product discharge). Dryer designs fall into three categories, co-current, counter-current, and mixed flow dryers . (as defined in chapter 1). Figure 5.6 illustrates four types of co-current flow drying chambers. The air disperser and atomizer are located either at the top, base or end of the chamber. Types (a) and (b) are the most common. Type (a) has a downward rotary air flow. The air disperser creates air rotation through tangential entry and/or flow over angled vanes. Spray is quickly drawn into a similar rotary motion. Such air disperser designs are shown in figure 5.7 (see also chapter 7, figures 7.1, 7.2, 7.3). Type (b) has a downward streamline flow. The air disperser creates non-rotary flow by use of perforated plates and/or straightening vanes. The spray acquires a streamline flow motion once the deceleration of droplets from the nozzle is completed. In type (c) the air must prevent dried particles settling out in the upward flow. In type (d) the reverse is required, namely air flow permits dried particles to fall out of the air and fall to the chamber base. In counter-current flow dryers (figure 5.8) the atomizer and air disperser are located at opposite ends of the drying chamber. Counter-current 75 AIR OUT FEED IN PRODUCT OUT Figure 5.8. Counter-current flow dryer. IT Cliornbrr rob! A lomizer ....----. ■.... An,ked win es flow is mainly restricted to nozzle atomization in tall, narrow diameter towers. The air disperser creates various degrees of air rotation on entry into the chamber (see figure 7.4) but due to chamber height, the rotary motion cannot be sustained in the upper region of the chamber. In mixed flow dryers, air and product are subjected to both co-current and countercurrent flow conditions during passage through the drying chamber. This is accomplished by : (i) Air flows in two directions while the product flows in one. The air inlet and outlet ducts plus the atomizer are located at the top of the chamber as shown in figure 5.9(a). a. (ii) Air flows in one direction while the product flows in two. The atomizer sprays up from the chamber base into the incoming drying air. Product discharge is at the chamber base. This is shown in figure 5.9(b). d. Figure 5.7. Air disperser types creating rotary air flow around atomizer. (a) Tangential entry (roof mounted). (b) Angled vanes creating swirl (centrally mounted). (c) Angled vanes; banjo inlet (roof mounted). (d) Tangential entry; double inlet (roof mounted). In figure 5.9(a) high inlet velocities develop a high degree of swirl to obtain high evaporation rate conditions. The residence time within the dryer is very short (5-10 sec). The vigorous cyclonic motion created within the chamber sweeps the walls clean, while at the same time separates out the product from the air. Product is discharged at the chamber base. Due to the high powder—air ratio within the chamber a fair percentage of product remains entrained in the air and is carried out at the top of the dryer. In 76 EQUIPMENT INCORPORATED IN SPRAY DRYERS BASIC PRINCIPLES, DEFINITIONS AIR OUT FEED IN 77 figure 5.9(b) the feed is sprayed upwards into a rotary air flow created by a ceiling air disperser. The spray travels upwards and decelerates to rest. The spray then becomes fully under the influence of the air flow and passes back down the chamber. This type of design is often designated the 'fountain spray dryer'. With the 'fountain' design, product can be either conveyed away with the exhaust drying air, or undergo separation in the conical base of the chamber and be discharged separately. Specialized patented drying chamber designs are covered in references (418) to (433)(514). PRODUCT AND AIR FLOW PRODUCT AND AIR FLOW I I AIR OUT AIR OUT OUT PRODUCT OUT PRODUCT OUT CONVEYOR PRODUCT OUT b. ❑. ASR IN SWEEPER SWEEPER DRIVE PRODUCT AND AIR FLOW SWEEPER AIR OUT \ AIR OUT Ati 111 PROD T OUT SWEEPER DRIVE C. PRODUCT OUT b. Figure 5.9. Mixed flow dryers. (a) Cyclonic. (b) Fountain layout. Figure 5,10. Primary product discharge from drying chambers. (a) From conical base chamber. (c) From double conical base chamber with sweeper. (b) From• flat bottom chamber with sweeper. 78 BASIC PRINCIPLES, DEFINITIONS With the majority of chamber designs, dried product passes to the base, which is equipped for either primary or total product discharge. In primary product discharge (figure 5.10) the greater proportion of dried powder is discharged directly from the chamber base. Only a fines fraction remains entrained in the exhaust air for recovery in the powder separation unit. Figure 5.10(a) shows primary product discharge from a conical chamber base. Air is exhausted from the side of the chamber cone. Figure 5.10(b) shows primary product discharge by a sweeper from a flat-bottom chamber. The swept area is large and product is subjected to mechanical handling. Primary recovery of product is from the conical base due to the separation effect of the cyclonic air flow created within the cone. Primary recovery of product from a flat-bottomed chamber is due to the product settling out from the air flow and falling at a terminal velocity to the floor. Both designs can handle lumpy products. Thermoplastic and high fat content powders are best handled in conical based dryers. There are blockage tendencies with a screw conveyor system in flat bottom designs. The main features of primary product discharge from both conical and flat bottom chambers can be combined to give a conical based design of reduced chamber height. Figure 5.10(c) shows this development of the conical base design where the lower part of the cone is inverted to give a double coned or W-shaped chamber. The chamber has a central exhaust air duct. A sweeper guides product into a rotary valve. Efficient primary product separation is still maintained with the arrangement. Use of a sweeper does subject product to some mechanical handling but this is reduced to a minimum as the actual swept floor area is small in relation to the chamber cross-sectional area. In total product discharge (figure 5.11) the air velocity in the exhaust duct must be high enough to convey the product to the separation unit. Due to the requirement for pneumatic conveying, this form of discharge is not recommended for spray dried products that leave the chamber as sticky lumps, although the conveying of product can be assisted by introducing cooler atmospheric air into the exhaust duct. Refinements to chamber design are used to handle special products ((435) to (441), (502)). For sticky (thermoplastic) products chamber wall temperatures must be kept low. Wall air cooling, (figure 5.12(a)) or introduction of secondary cooled air to sweep the lower chamber walls, (figure 5.12(b), (c)) can be used. For products having the tendency to remain on the chamber wall, electrical hammers or vibrators are mounted on the wall to constantly dislodge the product. 5.3.5. Equipment for Separation and Recovery of Product from Exhaust Air Dried product that is entrained in the air leaving the drying chamber must be effectively separated and recovered to maintain maximum output from the dryer operation and prevent air pollution through excessive EQUIPMENT INCORPORATED IN SPRAY DRYERS a. 79 PRODUCT, AIR OUT SWEEPER PRODUCT, AIR OUT PRODUCT, AIR OUT (i) b, Figure 5.11. Total product discharge from drying chambers. (a) From conical chamber base. (b) From flat chamber base; (i) sweeper side discharge, (ii) sweeper central discharge. powder release to atmosphere. Dry and wet equipment can be used. Product recovered dry is transported to further processing or to the dryer baggingoff area. Product recovered wet may be recycled to the dryer feed pretreatment, or simply considered as waste. Dry equipment of cyclones, bag filters or electrostatic precipitators are used as the main separation/ recovery stage. Generally product quality is not affected, although the comminuting effect of flow throligh cyclones can reduce the particle size of products exhibiting fragile structures. Where air with traces of product BASIC PRINCIPLES, DEFINITIONS EQUIPMENT INCORPORATED IN SPRAY DRYERS 81 CODLING AIR OUT (a) Double wall cooling air jacket. (b)Rotating PRODUCT OUT AIR/PRODUCT OUT leaves the main stage and must be cleaned prior to exhausting to atmosphere, wet equipment, e.g. wet scrubbers, wet cyclones,-irrigated fans are installed as a secondary stage. Often product concentrations in scrubber liquids are too low for economic concentration and re-drying, and thus the liquids are passed to effluent treatment. The range of dry and wet equipment is shown in figure 5.13, and their features are listed in table 5.1. 0 CODLING AIR IN 80 AIRBORNE POWDER WET SEPARATION !AIR CLEANING) DRY RECOVERY E k DRY CYCLONES BAG FILTERS ELECTROSTATIC PRECIPITATORS WET SCRUBBERS WET CYCLONES IRRIGATED FANS Figure 5.13. Equipment for separation and recovery of airborne powders. Cyclones are widely used due to their low cost and virtual total lack of maintenance. Cyclone efficiency is normally high enough with most spray dried products to dispense with the need for a secondary stage. It must be borne in mind, however, that even the highest efficiency cyclone operating under optimum operational conditions cannot reach 100 % efficiency, and if complete separation is required alternative systems must be used. Such a system is often a bag filter which is virtually 100 % efficient. However, the advantage of being a single unit exhausting powder-free air to atmosphere is offset by maintenance difficulties. Should bag rupture occur or product leakage result through incorrectly mounted bag clamps, access into the bag assembly is not too easy. Bag inspection in a dust laden environment makes isolation of the faulty bag(s) a time consuming task, and down-time often proves to be lengthy. In choosing the most suitable separation system, particle size, structure, loading in the air, air rate, required efficiency of separation, available power and space are factors to be considered (see also chapter 9). When all the product leaves the chamber airborne, powder loadings are high and a battery of high efficiency cyclones are required to reach high degrees of recovery. A 99.5 % efficiency, however, still gives a measurable product loss if production rates are high. When complete dry recovery is essential a bag filter might well be added after the cyclones or installed to replace the cyclones entirely. When primary discharge of powder in the chamber is adopted, only the fines fraction remains entrained in the air and passes to the separation unit. If bag filters are used, near total recovery of fines is • Table 5.1. Advantages and Disadvantages of Dry and Wet Powder Recovery Dry powder recovery Wet powder recovery Advantages 1. Powder recovery in useable form. 2. No equipment corrosion. 3. Available equipment capable of removing virtually all the airborne particle sizes from the spray dryer. 4. Simple layout (e.g. cyclones). 5. Hygienic (e.g. cyclones). 6. Capable of removing sub micron powder particles (e.g. bag filter). 7. Operates in a dry floor area. 1. Handles high temperature exhaust air. 2. Handles high humidity exhaust air. 3. Corrosive gaseous medium recovered and neutralized. 4. No explosion dangers. 5. Available equipment small in size compared with dry collectors. 6. Soluble material recovered and pumped back to the dryer. 7. High efficiency of powder recovery. Disadvantages 1. Not suited to hygroscopic materials. 2. Some equipment types have humidity and temperature operating limitations. 3. Powder atmospheres can cause an explosion hazard. 4. Cleaning sequence can be complicated (e.g. bag filters). 5. Equipment can block-up under adverse operating conditions (e.g. cyclones). 6. Strict maintenance required (e.g. bag filter). 7. Equipment wears with abrasive powders (e.g. cyclones). SNOIIINIJR0 `salaiDmuct DISVII oc 1. Insoluble powders are discharged as effluent liquid, unless settling and filtration equipment is available. 2. Scrubber liquid can cause an effluent problem. 3. Small micron sizes are not wetted and thus are lost from the equipment. 4. Greater corrosion risk to the equipment. 5. Scrubber water can freeze in cold weather. 6. Recovery of product in dry form requires further treatment. 7. Flooding can occur, and a drained floor area is required. 8. Unhygienic-unsuitable for many food products. 4 '5, ' P ut ❑ 4, . cr •0 o co m m ci 0 co og 0 0.. -I `6' '5 0 ....... 54 , O C 0 CD co co F - C a> CD V' 0 0 m o 7P n CD ID C) g EQUIPMENT INCORPORATED IN SPRAY DRYERS S. crq 0 0 -4 co •-e C q CX) 84 BASIC PRINCIPLES, DEFINITIONS (e.g. dyestuffs) or (c) are likely to cause an extreme air pollution problem (e.g. herbicide dusts causing flora damage in the surroundings), cyclones may well be followed by bag filters and/or scrubbers to ensure negligible losses. This is done even though primary recovery from the chamber may result in only a small percentage of the powder production entering the recovery section. When primary product recovery is from the chamber, there is more than one place of product discharge within the dryer layout. To assist ease of :product handling for packing it is usual to combine the numerous powder discharge places within a common transport system. The transport system can be pneumatic or mechanical. A pneumatic system is shown in figure. 5.14(a). Powder discharged from both the chamber and cyclone bases feed a common pneumatic system. Product is conveyed to a transport cyclone, from which the final packaging of the product takes place. The conveying air can be exhausted to atmosphere or blown back into the spray dryer system. Figure 5.14(a) shows the conveying air returned into the main ductwork of the exhaust drying air. Alternatively conveying air can be returned to the drying chamber. Pneumatic conveying is discussed further in section IV (chapter 12). Mechanical conveyor belt systems are suitable for granular, non dusting products. The system is shown in figure 5.14(b). It is used to transfer product to silo storage, or additional treatment processes, or to areas for direct bagging-off. Although such systems eliminate the problems of handling conveying air, they tend to result in a dirty operation. They cannot be considered where any degree of hygiene is demanded. Conveyor belt systems are found mainly in the chemical industry. Conveyor belts and other, equipment for mechanical conveying have been recently discussed (1970) by Buffington (11). Section II THE PROCESS STAGES OF SPRAY DRYING 6 Atomization CI. Introduction The atomization stage in spray drying produces from liquid bulk a spray of droplets having a high surface to mass ratio. The dried product that results from moisture evaporation of atomized spray can be made to possess the desired particle size distribution through control of the atomization variables. The ideal spray is one of small individual droplets of equal size. Heat and mass transfer rates and drying times are then the same for all droplets in the spray, ensuring uniform dried product characteristics. Droplets of a spray evaporate quickly and the short drying times involved maintain low droplet temperatures due to the cooling effect that accompanies evaporation. No product deterioration can take place due to heat, if correct atomization is combined with a suitable drying chamber design to give a product residence time just sufficient for completion of moisture removal. The ideal requirement of an atomizer is to produce homogeneous sprays. Such sprays have not yet been obtained at industrial feed rates, although atomizer types are available producing sprays that closely approach homogeneity, when operating with liquids of certain physical characteristics at low feed rates. 6.2. Basic Mechanism of Atomization The mechanism of atomization has been studied by many workers, but remains a controversial subject in spite of much published data. Various theories predominate, each receiving experimental support. The mechanisms now accepted as applicable to commercial atomization conditions are the outcome of work by pioneers on the stability and collapse of simple liquid jet (ligament) systems. A dripping tap or the slow release of liquid from a pipette are examples of the simple jet system initially studied, and on which ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING atomization theories are based. The formation of each drip illustrates that the basic atomization steps of liquid break-up depend upon forces acting on and within the jet. These forces destroy the jet's initial stability. It is gravity in the case of the dripping tap. Simple relationships can express basic break-up. Extension to more complicated conditions enables atomization mechanisms pertaining to spray drying to be deduced. However, conditions occurring in commercial atomization are extremely complex and theoretical relationships cannot be considered adequate. Apart from irregular liquid break-up, due to non-ideal liquid distribution at the atomizer edge, there is the complex interaction between the spray leaving the atomizer and the surrounding air, unknown stresses within each droplet the instance after leaving the atomizer, and the influence of droplets on each other within the spray cloud. The development of a mechanism theory applicable to commercial atomization can readily be followed and one man is credited with the innovation. Lord Rayleigh (12) published in 1878 the mathematical break-up of non-viscous liquid jets under laminar flow conditions. The conclusion drawn at that time stated that a jet becomes unstable and ready to disrupt if its length is greater than its circumference. Although these conditions do not exist in rfiality, an actual liquid jet being turbulent, viscous and subjected to surrounding air influence, the general conclusions were accepted in later theories. Tyler (13) working with mercury jets came very close to Rayleigh 's predictions. Weber (14) extended the predictions to include viscosity, surface tension, and liquid density effects. In the 1930's jet disintegration had reached the stage where the effects of air resistance on jet break-up were being considered. Haeniin (15) reported that orderly wave formation at the jet surface caused by a high velocity air flow become completely irregular on velocity increase. Castleman (16) also analysed high velocity disturbances, and suggested the degree of atomization was controllable by the relative velocity of air and liquid. In direct continuation, jet stability was found to be a function of Reynolds number. Ohnesorge (17) is credited with the Reynolds Number relationship. The tendency of the jet to disintegrate is expressed in terms of liquid viscosity, density, surface tension and jet size. Ohnesorge condensed his findings by suggesting that the mechanism of liquid break-up could be expressed in three stages, each stage characterized by the magnitude of a dimensionless number Z'. The Z' number was the ratio of the Weber/Reynolds numbers : V i p 1 d.) 1 i 2 a x ( Vd n p,) - (P)adr,) 1I2 Vi = jet velocity, p, = liquid density, d o = nozzle (jet) diameter, c = surface tension, I/ = liquid viscosity. Z' is plotted against Reynolds number in 89 figure 6.1. The graph shows three zones : Zone 1. At low Reynolds numbers the break-up of liquid jets shows the Rayleigh mathematical prediction. Zone 2. At intermediate Reynolds numbers, the break-up of liquid jets is by jet oscillations with respect to the jet axis. The magnitude of these oscillations increases with air resistance until complete disintegration of the jet takes place. Zone 3. At high Reynolds numbers, complete atomization occurs at the orifice from which the jet emerges. WEBER NUMBER REYNOLDS NUMBER 88 2 1 10 10 4 3 10 10 6 5 10 10 REYNOLDS NUMBER ( Re) Figure 6.1. Ohnesorge chart showing liquid jet disintegration as a function of Reynolds number. From figure 6.1 atomization mechanisms can be deduced. Atomization mechanism at low Reynolds number is through oscillations created at the liquid jet surface. At intermediate Reynolds numbers, the degree of atomization depends upon the wave motion set-up in the jet. At high Reynolds numbers, the disintegration is so rapid that direct atomization is obtained at the atomizer edge. This is an oversimplification of the process of liquid atomization, since in commercial atomization conditions all mechanisms act simultaneously influencing the spray characteristics to varying degrees. For further details on mechanism of liquid jet disintegration, reference should be made to Giffen and Muraszew (18), Miesse (19) and Richardson (481). The various atomization theories arising from work on liquid jet instability are summarized by Friedman, Gluckert and Marshall (20). A comprehensive survey and critique of atomizer literature, up to and including THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 91 December 1966 has been reported by Lapple, Henry and Blake (25). The dependence of jet instability and disintegration on liquid properties, jet velocity and orifice size is illustrated in table 6.1, which contains correlations proposed by investigators to predict droplet size following jet disintegration. ‘46 ,43 1/40 +43 6.3. Classification of Atomizers Droplet size equation Atomization results from an energy source acting on liquid bulk.* Resultant forces build up to a point where liquid break-up and disintegration occurs and individual spray droplets are created. The different atomization techniques available concern the different energy forms applied to the liquid bulk. Common to all atomizers is the use of energy to break-up liquid bulk. Centrifugal, pressure, kinetic energy are the common forms and each classify the atomizer device. Sonic and vibratory atomizers are less common, with work into possible spray drying applications within the early stage of development. ATOMIZERS . INCORPORATING CENTRIFUGAL ENERGY Droplet size parameter ROTARY ATOMIZERS VANED WHEELS VANELESS DISCS CUPS BOWLS PLATES PRESSURE ENERGY KINETIC ENERGY SONIC ENERGY PRESSURE NOZZLES PNEUMATIC NOZZLES SONIC NOZZLES I CENTRIFUGAL PRESSURE NOZZLES SWIRL CHAMBER GROOVED CORE TWO-FLUID INTERNAL MIXING THREE-FLUIE SIRENS WHISTLES 1 EXTERNAL MIXING ROTARY PNEUMATIC ATOMIZERS Figure 6.2. Classification of atomizers. Merrington, Richardson (24) 90 The classification of liquid atomizers used in spray drying is shown in figure 6.2. Rotary atomizers feature high velocity discharge of liquid from the edge of a wheel or disc. Pressure nozzles feature the discharge of liquid under pressure through an orifice. Pneumatic nozzles feature the break-up * Minimum energy for atomization is the requirement to create new surface. The theoretical power (PK ) can be expressed (18) (29): PK = AO where A = net average area created per unit time, e = surface tension. Based upon thermodynamic considerations, power requirement to create new surface is only a very small proportion of that expended in an atomizer during spray dryer operation. 92 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING 6.5. Rotary Atomization of liquid on impact with high velocity air or other gaseous flow.' Sonic nozzles feature break-up of liquid through sonic excitation. For each class of atomizer, a wide range of designs has been developed to handle the diversity of feed materials and to meet dried product characteristics. 6.4. Applications of Basic Mechanisms to Commercial Atomizer Conditions The mechanisms as stipulated by Ohnesorge (17) apply to the break-up of simple jets. Before these mechanisms at high Reynolds numbers can be tonfidently applied to commercial atomizer conditions, a link between simple jets and the liquid form leaving a rotary atomizer or issuing from a nozzle orifice had to be established. Liquid at the edge of a rotary atomizer or in a pneumatic nozzle is subjected to high velocity contact with air. Castleman's (16) analysis on high velocity disturbances thus applies, and by drawing on his conclusions can relate the mechanism of atomization in these commercial atomizers to simple jet break-up mechanisms of Ohnesorge (17). Liquid issues from a centrifugal pressure nozzle as a conical sheet due to the swirl imparted to the liquid within the nozzle. Experimentation has shown a similarity between the break-up of jets and the disintegration of conical sheets of liquid. Observations on a simple centrifugal nozzle have established that the conical sheet (the dispersion of which is measured as a cone or spray angle) breaks up into droplets a short distance from the orifice, when undulating disturbances in the cone eventually result in its collapse. As pressure is increased, break-up occurs nearer the Orifice, the behaviour of which is analogous to the findings of Ohnesorge for simple jets. The mechanisms applicable to conditions under which commercial atomizers operate can be summarized as the immediate disintegration of liquid at the atomizer edge. Disintegration at the atomizer edge is the result of turbulence in the issuing liquid and the action of air forces, whilst being opposed by viscosity and surface tension forces in the liquid. The readjustment of sheer stresses within the liquid once the droplet is airborne is another factor contributing to further disintegration of the droplet. The atomization mechanisms are still not fully understood. The role played by air friction at the atomizer edge is especially interesting, since successful atomization of liquid in turbulent flow can be obtained in vacuum at low feed rates. Much research (25, 35) has been undertaken on subjects ranging from simple jet disintegration to the atomization characteristics of basic atomizer devices, e.g. low speed rotating discs. Much of the uncertainty results from the experimental difficulties involved. When it comes to the investigation of commercial atomizers, the process of liquid disintegration proceeds too fast to distinguish the individual phases of liquid break-up. The role of each liquid property is thus still obscure. 93 IR 6.5.1. Introduction In rotary atomization, the feed liquid is centrifugally accelerated to high velocity before being discharged into an air—gas atmosphere. The liquid is distributed centrally on the wheel/disc/cup. The liquid extends over the rotating surface as a thin film. Rotary atomization is often termed centrifugal atomization, but this can be a little misleading as centrifugal energy is also utilized to a certain degree in centrifugal pressure nozzles, where liquid is given rotational motion. The degree of rotary atomization depends upon peripheral speed, feed rate, liquid properties and atomizer design. Maximum centrifugal energy is imparted to the liquid when the liquid acquires the wheel/disc peripheral speed prior to discharge. If a flat smooth disc is rotating at high speed and liquid is fed on to its top surface, severe slippage occurs between the feed liquid and disc. The velocity of liquid from the disc edge is much lower than the disc peripheral speed. Conditions of no slippage occur at very low speeds, but the available centrifugal energy permits only the smallest of feed rates to be satisfactorily atomized. To prevent slippage in commercial atomizers, radial vanes are used. The liquid is confined to the vane surface, and at the periphery the maximum liquid release velocity possible is attained. The maximum release velocity is the resultant of radial and tangential components acquired by the liquid. Alternatively slippage can be reduced by increasing friction between liquid and rotating surface. This is often done by feeding liquid on to the lower surface of a disc shaped as an inverted plate, bowl or cup. As the liquid is flung outwards due to centrifugal force, the liquid film is pressed against the disc surface. Both techniques are used to handle large feed rates, although the vaned designs (atomizer wheel) are selected in cases where fine sprays are required. However, many spray dryer operations call for large particle sizes, and thus the inverted disc types enjoy wide usage. Smooth flat vaneless discs (with feed on top surface) are rarely used in spray drying operations. Only a brief description will be given (6.5.2). Their operation, however, goes some way to explain the basic atomization mechanism involved in rotary atomizers. Atomizer wheel designs are dealt with in detail (6.5.3). These are the most widely applied of rotary atomizers. Vaneless discs of the plate and cup type are discussed afterwards (6.5.4). 6.5.2. Flat Smooth Disc Atomization (Vaneless) For a flat smooth vaneless disc, the degree of atomization obtainable will depend upon the magnitude of feed acceleration toward the edge over the smooth surface. The final liquid release velocity depends upon the 94 THE PROCESS STAGES OF SPRAY DRYING slippage between liquid and the rotating surface. The extent of slippage depends upon feed rate and physical properties of the liquid, namely the viscous drag and the ability of the liquid to wet the surface. The disintegration of liquid into droplets from a rotating disc is governed by: (a) the viscosity and surface tension of the liquid, (b) inertia of the liquid at the disc periphery, (c) frictional effects between the liquid droplets and surrounding air at the point of droplet release from the disc, (d) readjustment of shear stresses within the liquid droplet once the droplet is airborne. At low disc peripheral speeds, the liquid viscosity and surface tension are the predominating factors. The higher the disc speed, the more inertia and air friction contribute to the mechanism of droplet formation. Due to liquid slippage over the disc surface, liquid inertia never becomes high and as release velocities are low, air frictional effects are minimized too. Only in the commercial atomizer designs of vaneless discs do inertia and air friction play a dominant role at high feed rates and high liquid release velocities. For smooth flat vaneless discs, when viscosity and surface tension predominate the mechanism of atomization, sprays are formed by individual formation and release of droplets from the disc edge. This is shown diagrammatically in figure 6.3(a), Feed rates and disc speeds are very low. Sprays consist of two or three prominent droplet sizes, i.e. parent droplet and two satellites. With continued disc speed increase and higher feed rates, the direct droplet mechanism changes to one of ligament break-up. The point concentrations of liquid that gave rise to direct droplet formation contain more liquid, and ligaments begin to extend out from the disc edge. The ligaments again disintegrate into sprays of parent and satellite droplets as illustrated in figure 6.3(b). Larger parent droplets are formed from higher feed viscosities and surface tensions. Increases in feed viscosity increase the proportion of satellite droplets in the spray. Spherical droplets are formed irrespective of the surface tension value. The mechanisms illustrated in figure 6.3(a and b) are controlled by the physical properties of the feed liquid. The transition between the predominance of liquid properties and of inertial forces occurs when the liquid ligaments join to form a liquid sheet extending from beyond the disc edge (figure 6.3(c)). The mechanism of liquid atomization at the transition between liquid ligament and sheet formation is shown photographically in figure 6.4. Atomization by liquid sheet formation is often referred to as the velocity spraying mechanism (26). The mechanism is accentuated by ATOMIZATION 95 0 0 0 0 a O 0 O a. 0 ❑ . 6„ 0 .„ o p o a DISC EDGE c. Figure 6.3. Mechanisms of atomization. (a) Direct droplet formation. (b) Ligament formation. (c) Sheet formation. highly viscous liquids. The sheet disintegrates giving a spray of broad droplet size distribution. With further increase of disc speed at constant feed rate the liquid sheet retracts towards the disc edge. If feed rate is increased with disc speed, velocity spraying continues. If slippage over the disc is minimized or prevented, liquid release velocity from disc edge becomes high enough to enable air frictional effects at the liquid—air interface to become the controlling atomization mechanism. The mode of disintegration of the retracting sheet makes the formation of completely homogeneous sprays appear a remote possibility. Use of high viscosity and surface tension 96 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 97 reduces the broad distribution as does increase of disc peripheral speed at constant feed rate. To produce narrow distribution, high speeds are required at low disc loadings. Bauer and Kruger (27) in a recent article (1969) review current knowledge of atomization mechanisms from vaneless discs. Theory pertaining to flow over the disc and release of liquid from the disc edge is discussed. Photographic evidence of the mechanisms involved have assisted visual appreciation of the atomization process. Once the droplets have left contact with the disc edge and are airborne further disintegration can take place due to readjustment of shear stresses set up within the liquid during liquid flow over the disc surface. Droplet disintegration by this mechanism is difficult to distinguish from disintegration by air friction effects, which also causes droplet distortion when droplets are airborne. In spray drying the air friction effects are considered the major mechanism, but atomization in low vacuum has shown the mechanism of shear stress readjustment to occur when liquid flow is turbulent. (a) (a) Flow over Smooth Flat Vaneless Discs The mechanism of liquid atomization has been reported widely on flat vaneless discs. With the degree of atomization dependent upon the velocity of liquid release, which in turn depends upon the slippage between liquid and surface, Frazer (28) defines the occurrence of severe slip by the relation (6.7), where M = mass feed rate (lb/hr), p = feed viscosity (cp) and d = disc diameter (ft) ( M (6.7) 1440 mpd ) Quite high feed rates that can be handled on a disc. For example a 6 in (150 mm) disc operating on water can take 38 lb/min (17 kg/min) before extreme slippage conditions commence. Atomization by spray drying standards would be poor, illustrating the additional factors like air—liquid frictional effects that make for effective liquid disintegration. The time (t) taken for liquid to reach the disc edge under non-slippage conditions at very low feed rates has been expressed mathematically by Seltzer and Marshall (29) (N = disc rotation) t = (b) Figure 6.4. Mechanisms of atomization (represented photographically). tion. (b) Transition between ligament and sheet formation. (a) Ligament forma- 0 27EN (6.8) B is the number of radians a liquid element must pass before disengagement. 0 is defined as the theoretical hyperbolic path travelled by the liquid element where B = cosh' (r d /ro ). Equation (6.8) was evolved from a set of simultaneous non-linear ordinary differential equations proposed by Seltzer and Marshall (29), for disc 98 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION conditions where both slippage and frictional resistances occur under laminar flow conditions. The flow characteristics were defined by d er dt 2 127r1.0\ dr \ 2 Qp, ndt) r (10) 2 0 (6.9a) d dO\ 27;u0 2 1 d& dr 0 (6.9b) La) dt dt Qp, r = disc rotational speed (2IEN), Q = volumetric feed rate, r = radial distance from centre of disc, t = time for element of liquid to move from r o to r, dO/dt = rotational speed of feed. dt r dt ) This can be reduced to equation (6.8) through integration, by substitution of P = dr/dt.* Equation 6.8 applies to the 'ideal' disc, Frazer (28) proposed functions to express flow conditions over an ideal disc surface, where liquid break-up at the disc edge is due to ligament or sheet disintegration. The transition between the two disintegration mechanisms is stated as functions of two dimensionless parameters Az and B' where y \ 1/6 (pcni) d od r 1/2 ) 13' is expressed in terms of the Z' number (see figure 6.1). The parameters show the roles played by viscosity and surface tension on resulting liquid break-up conditions. The transition is represented on figure 6.5 by a line of separation. as checked out by substituting these values in equation (6.9b). If frictional viscous forces are also ignored = 0), equation (6.9a) becomes N72 p = dr d er = dt 2 pd) 1/2 o- A r =Nd - ° [(61i) For conditions of non-slippage dO N =— dt and d ( da ) — — 0 dt dt d e r dP dP dr dP dt 2 = dt = dr = P dr Thus dP P— = (6.10) dr N2r P dP = N 2 r dr Integrating P2 N 2 r 2 + T= 2 C when ATOMIZATION THROUGH LIQUID SHEET FORMATION t = '0, rry r ro C — P2 Ar2( r 2 11 .' Q N dt 001 1 1 1 1 1 41 1-0 Integrating " ce•d ) dr Nt = fro (r2 rD1/2 = cosh' ?1 ( A421 /4) r rD dr dt N(r 2 rW/2 dr dt dr (r 2 rg) 112 P J N2r2 2 or z 0001 dr =0 dt Therefore ATOMIZATION THROUGH LIQUID LIGAMENT FORMATION .0 99 ro 05 Figure 6.5. Atomization mechanism for rotating discs (28). (Relationship between operating variables and atomization mechanism.) for N in rev/min aNt = cosh' (1 ro 100 THE PROCESS STAGES OF SPRAY DRYING Equation number oc N 1-4 tll N Ld Sheet disintegration Ligament break-up cis Oyama, Endou (34) Walton, Prewett (33) N Direct droplet formation where p.q.r.s are respective integers, the values of which depend upon atomizer operating conditions. 6.5.3. Wheel Atomization (Atomizer Wheels) (a) Introduction The mechanism of atomization applicable for atomizer wheels is similar to that discussed for flat smooth vaneless discs in section 6.5.2. Mechanisms are shown photographically by Marshall (35) and Kurabayasi (36). At low speeds and feed rates, viscous and surface tension forces predominate to give direct droplet formation. For intermediate speeds, the disintegration of liquid ligaments extending out from the vane edge is by centrifugal and to a lesser extent by gravitational forces. In the commercial range of conditions (high liquid flows at high wheel peripheral speeds), liquid disintegration occurs right at the wheel edge by frictional effects between air and the liquid surface as liquid emerges as a thin film from the vane. The mechanism does not lend itself to the formation of homogeneous spray formation, although sprays of small droplet sizes can be produced. Increasing the viscosity and surface tension of the liquid will act to increase the spray uniformity, but at the expense of a low mean droplet size. However, for general operational circumstances in spray drying, adjustment to the feed II II II aa by Cl Atomization mechanism D cc N -13 : D cc o- g: D d': D cc QS ATOMIZATION 101 Table 6.2. Droplet Size Prediction for Smooth Fiat Vaneless Discs (b) Droplet Size from Smooth Flat Vaneless Discs Six equations to predict droplet size from smooth flat vaneless discs are given in table 6.2. Other equations in this field are given by Lapple (25) and Dombrowski (30). All are applicable to the simplest of systems involving low feed rates of low viscous liquids. Surface tension and liquid density appear as the only liquid properties of influence, which is misleading as viscosity is of prime importance. This is illustrated in equation (6.13), where the author claimed close agreement between experimental and predicted results for low viscous liquids but not for high viscous liquids. Droplet size appears inversely proportional to the first power of disc speed for these simple systems. The conditions of experimentation produced uniform sprays, although the presence of satellite droplets was evident. The D max value in the Bar (32) equation refers to the parent droplet. Frazer (28), Walton and Prewett (33) and Hege (31) give the average diameter of the spray. Oyama and Endou (34) use the Sauter mean diameter. In table 6.2; D is microns, N is rev/min, 3 3 d is cm, o- is dynes/cm, p is g/cm , Q is cm /sec. The equations of table 6.2 are of limited interest to spray drying conditions. However, the equations indicate the relationships between droplet size and the operation variables; relationships that do hold into commercial atomization conditions. 102 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION liquid properties is not possible or desirable. To obtain optimum droplet size uniformity for a given feed rate the maintenance of the following six conditions is essential : i. Vibrationless wheel rotation. ii. Large centrifugal forces compared with gravitational forces (i.e. high peripheral speeds). iii. Smooth vane surfaces. iv. Uniform liquid feed rates. v. Complete wetting of the vane surface. vi. Uniform distribution of feed to the vaned wheel. (b) Flow over a Vaned Wheel Liquid fed on to a wheel moves across the surface until contained by the rotating vane. Liquid flows outwards under the influence of centrifugal force and spreads over the vane wetting the vane surface as a thin film. At very low liquid vane loadings, the thin film can split into streams. Unlike the flat smooth vaneless disc, no liquid slippage occurs on a wheel once liquid has contacted the vane. The vanes, whether radial or curved, prevent transverse flow of liquid over the surface. Of the basic equations developed in the previous section, equation (6.9a) is not valid. For vaned wheels, only viscous resistance is acting. 103 Droplet travel from a wheel is shown in figure 6.6. The liquid film on leaving the vane edge has radial (XY) and tangential (YZ) velocities giving a resultant component (WY). The angle of release is less than 45° to the wheel edge. For commercial atomizer wheels, the radial velocity component is much smaller than the tangential, and release velocity approximates to the peripheral wheel velocity, and at an angle of release approaching the tangent to the wheel edge. (i) Radial Velocity (14 Radial velocity of the liquid film at the wheel edge is calculated from differential equations derived from consideration of forces acting upon the liquid film (35). Differential equations are derived in Appendix 8. Marshall (35) suggests that for atomizer wheel sizes and peripheral speeds used in industrial spray drying liquid acceleration along the vane has ceased upon reaching the wheel edge. The radial velocity is given by PJav 0)211/3 Vr = (6.18) 3/2h2 The error in this simplification is minimal, but Marshall (35) has stated the error can be reduced further if equation (6.19) is used where X has values greater than 1. DROPLET TRAVEL RELATIVE TO WHEEL EDGE Z = X1/3 1 1 1 9X 27X" 218X 213 (6.19) Where X = r(R*o.) 2 ) LIOWO DISTRIBUTOR and R* = 3/.1h 2 R* 112 DROPLET TRAVEL., RELATIVE TO CHAMBER WALL. v?.1- 1/2 A 5 in (125 mm) 24-vaned wheel atomizing water gives values of X as shown in table 6.3. Equation (6.19) is valid for calculating radial velocities in this case. x FASTENING BOLTS Table 6.3. Values of X = r(R*(o 2 )'I2 Wheel speed (rev min) RESULTANT v LIQUID SLIPPAGE OVER SURFACE UNTIL CONTACT WITH VANE Figure 6.6. Liquid flow to and from edge of atomizer wheel. Feed rate (113/min) 15 750 20 600 24 000 4.0 7.0 10.0 28 16 11 32 18 13 35 20 14 104 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING Frazer (28) has forwarded an estimation of radial velocity (ft/sec) from a vaned atomizer wheel. P i n 2N 2 dQ 2 1/3 (6.20) V, = 0.043 [ m/22112 1 Where d is ft, p. is cP, h is ft, N is rev/min, Q is ft /min, p, is lb/ft . The graph of flow rate plotted against radial velocity is a straight line on log-log plot. (ii) Tangential Velocity (VT ). The vanes prevent slippage and the liquid acquires the peripheral velocity of the wheel on release. (6.21) V, = rdN (iii) Resultant Release Velocity (Tires). The resultant release velocity is the square root of the sum of the squares of the radial and tangential components. Tires (6.22) [ Vi + Vi?.]"2 (iv) Angle of Liquid Release (a). The angle of liquid release follows from equation (6.22) by basic geometry V (6.23) tan VT In practice a is very small, and Tires approximates to the peripheral speed of the atomizer wheel. EXAMPLE 6.1. Radial velocities and film thickness at the edge of a 10 in diameter 20 vaned wheel are required. Vane height is lk in. If the feed specific gravity is 1.5 but the feed liquid viscosity can be varied from 50-100 cP by preheating, calculate values at feed rates of 132, 264 lb/min at viscosities of 50, 80, 100 cP respectively. The wheel speed is 10 000 rev/min. Assumptions : Equal liquid distribution to all vanes. No acceleration of liquid on vane surface at wheel periphery. For operating conditions of 132 lb/min, and feed viscosity 80 cP, substituting values in equation (6.18) Q, 1.18 x 10 -3 ft 3 /sec per vane, w = 1044 rad/sec p i = 93.5 lb/ft' 33.5 ft/sec Film thickness (b) is calculated from the continuity equation (no hold-up on vane) (b = +2,/h Vr) b = 3.5 x 10 -4 ft (0.107 mm) Values of V, and b for other operating conditions are given in table 6,4. Equation (6.20) can also be used. (Note how much smaller the radial velocity is compared with the tangential component.) Table 6.4. Values of Radial Velocity and Liquid Film Thickness at Edge of Vaned Atomizer Wheel (Example 6.1) 3 3 105 Feed rate (lb/min) Liquid viscosity (cP) Radial velocity Film thickness at wheel edge at wheel edge (mm) (ft) (ft/sec) 132 132 132 50 80 100 39 33.5 31 3.0 x 10 -4 3.5 x 10 -4 3.8 x 10 -4 9-15 x 10 -2 1.07 x 10 -1 1-16 x 10 -1 264 264 264 50 80 100 63 53 49.5 3.8 x 10 -4 4.5 x 10 -4 4.8 x 10 -4 1.16 x 10 -1 1.37 x 10 -1 1.47 x 10 -1 430 ft/sec (131 m/sec). Peripheral velocity (c) Effect of Operating Variables on Droplet Size Operational variables that influence droplet size produced from atomizer wheels are speed of rotation, wheel diameter, wheel design (number and geometry of vanes or bushings), feed rate, viscosity of feed and air, density of feed and air, surface tension of feed. The effect of these variables on mean droplet size of a spray is best studied through dimensionless analysis, where variables are grouped to represent basic atomization mechanisms. Forms of Reynolds number (defining the inertial and viscous force ratio on the liquid) and Weber number (defining the inertial to surface energy ratio) are commonly used. Friedman, Gluckert and Marshall (20) used the following groupings where the atomizer wheel speed conveniently appears in one group only (M, = mass feed rate for wetted periphery) D vs r i Ma \ p Ni p b I M p lc I LV \r pNr 2 ) Groups having exponents a . b are related to Reynolds Number, the remainder to Weber number. Effect of liquid properties and liquid release velocity on droplet size has already been introduced under the section 6.5.2. Several investigators have studied the effect of these variables and others, and report that the variables of most influence on droplet size in commercial atomization conditions are peripheral wheel speed, and liquid loading on the vanes (volumetric basis). Atomizer wheel/disc Viscosity (cP) Density (lb/ft 3 ) Surface tension (dynes/cm) Diameter (in) Speed (rev/min) Feed rate (lb/hr) Vane number Vane height (in) , Friedman, Gluckert, Marshall (20) Herring, Marshall (37) Frazer (28) Vaned non-vaned 1-9000 62.4-88 74-100 2-8 860-18 000 8.5-800 2-24 0-015-1.31 Vaned non-vaned 1 62.4 74 2-8 5000-32 500 0.2-50 8-24 0-31-1.28 Vaned non-vaned 1-9000 62.4-88 74-100 2-8 860-18 000 33-4050 8-24 0.31-1-32 Masters, Mohtadi (38) Scot, Robinson, Pauls, Lantz (39) Vaned Vaned 1 62-4 74 5 15 750-24 000 240-600 24 0.25 9.8-199-5 5327-8 2 11 900-41 300 ' ,4.2-37 - 24 . 0.23 THE PROCESS STAGES OF SPRAY DRYING Table 6.5_ Operating Conditions Covered by Investigators in Drawing up Equations (626-621) to Predict Spray Characteristics from Atomizer Wheels/Discs Table 6.6. Effect of Operating Variables on Droplet Size from Atomizer Wheels Wheel speed Wheel diameter Peripheral speed Feed rate Vane height Vane number Feed viscosity Feed density Feed surface tension Herring, Marshall (37) Masters, Mothadi (38) N —°-82 N - ° -6 Q ❑-2 (Nd) —°.83 Q0.24 (Nd) ° Q0.18 - ❑ -1 b-o-1 n -(1-1 b- 0.12 n 0-1 µ— 0.2 p 0.5 )0 — ❑ -5 Frazer (28) N - ❑ -6 d — 0-2 Q -2 ❑ b --o-1 n o•i ❑ N - -6 d - °• 2 d- 0.85 Scott, Robinson, PauIs, Lantz (39) OW -13-54 Q0-17 —0.02 0_ 0-1 NOLLVZCWOIY Operating variable Friedman, Gluckert, Marshall (20) •• • 108 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 109 Table 6.5 lists investigators, and the operating conditions under which their conclusions were drawn. The effects of operating variables on droplet size, concluded from such work are summarized in table 6.6. (i) Effect of Liquid Feed Rate on Droplet Size. Droplet size varies directly with feed rate at constant wheel speed. The variation of Sauter mean droplet size with feed rate is shown in figure 6.7. Droplet size varies between 0.17-0.2 power of feed rate. Friedman, Gluckert and Marshall (20) established a 0.2 power variation for feed rates up to 70 lb/min at constant wheel speeds within the range 3500-14 000 rev/min where maximum peripheral speeds reached 208 ft/sec (63 m/sec). Feed properties ranged from (a) specific gravity (1-1.425), (b) viscosity (1-9000 cP) and (c) surface tension (74-100 dynes/cm). 2 00 1 I I I overage slope = 0.2 150 200 CC Li 1— 77 FT /SEC < 1 00 • 90 — J Ln CL z o 70 Or ct O 60 Z X 7 (270 Kg/hr). Scott (39) studied the particular case of small diameter wheels rotating at very high speeds and with low feed rates and found a 0.17 power variation to apply. (ii) Effect of Peripheral Speed on Droplet Size (including effect of speed of rotation on droplet size). Droplet size is inversely proportional to wheel peripheral speed at constant feed rate. This is shown in figure 6.8. Droplet size varies inversely within a power range of 0.54--483 power of peripheral speed. Herring and Marshall (37) established the 0.83 power relation within a low speed range (50-305 ft/sec, 15-93 m/sec) at constant feed rates (20-50 lb/min, 9-23 kg/min). Masters and Mohtadi (38) showed within a higher speed range (325-496 ft/sec, 100-150 m/sec) using a similar wheel design that an inverse power relation of 0.7 fitted experimental data. Such findings indicate that the rate of decrease of mean size with peripheral speed decreases with increase of speed within the higher speed regions. It follows that, for set feed conditions, there is a minimum droplet size for which further increase of speed has no further effect. 50 ct REST LT S EY FRI EDMAN, 734 FT/SEC ( 20 ) GLU CNER AND MARSHALL 150 RESULTS BY HERRING AHD MARSHALL ISLE! LLI N (7) -.100 U) Z Li] • LI) ( 37) 091) 325 FT/SEC 426 rrissc 49 6 FT/SEC LLJ — 40 30 4.0 AQUEOUS FEED RATE 11: , 7.0 10.0 90 0_ L' 0 — 80 RESULTS BY MASTERS AND MOHTA131 ( 3B ) • 70 LLI 60 15.0 MASTERS AND /min Figure 6.7. Effect of feed rate on mean droplet size for atomizer wheel. Frazer (28) substantiated the 0.2 power variation working over a similar range of variables. Masters and Mohtadi (38) atomized water at constant wheel peripheral speeds in the higher regions up to 496 ft/sec (150 m/sec), and established a 0.18 power variation to be more representative of the feed rate—mean droplet size relation. Feed rates ranged up to 600 lb/hr RESULTS NV MONT AD! i 35) ( SLOPE-041 50 40 200 300 400 500 600 700 PERI PH ERAL SPEED FT/ SEC Figure 6.8. Effect of atomizer wheel peripheral speed on mean droplet size. ATOMIZATION 111 110 THE PROCESS STAGES OF SPRAY DRYING Scott (39) showed the power relation to be even lower than that stipulated by the above investigators. When operating small diameter wheels at very high speeds and low feed rates, the Sauter mean diameter was shown to vary inversely with the 0.54 power of peripheral speed. Peripheral speed is widely accepted as the main variable for adjustment and maintenance of a specified droplet size. However, the precise role played by the variable is still not clear. It has been shown by Wallmann and glyth (40) that droplet size does not necessarily remain constant if equal peripheral speeds are produced in wheel designs of various diameter and speed combinations, operating at equal feed rates and fixed feed solids. The wheel that subjects liquid to the greater centrifugal force produces the s mallest droplets. In fact, plotting droplet size against a centrifugal factor (c) defined as the number of times gravity, results in an inverse function, from which follows D cc (dN 2 ) -1 14 1/min 7.5 l/rnin 4.51/rnin 3.01/min 1.8 I /min (6.25) as rg 42r 2 r 2 N 2 r3600 7r2r/V2 900g 7r 2 riN 2 5000 20000 30000 SPEED P .P. M 1800g where N is rev/min. Separate investigation of the relation between droplet size (D) and wheel speed (N) at constant wheel diameter (d), and the relation between droplet size and wheel diameter at constant wheel speed have not supported equation (6.25). Droplet size is inversely proportional to diameter, but both Friedman (20) and Frazer (28) found D to vary as d - ", where Herring and Marshall (37) found variation to support d' 85 . Similar discrepancies were obtained from investigations into the droplet size-wheel speed relationship. Both Friedman and Frazer propose D cc N - ", whereas Meyer (41) proposes .D cc N - ' 69 and Herring and Marshall propose D oc The effect of speed on Sauter mean droplet size is shown from aqueous spray data to follow an average exponent of —0.6 in figure 6.9. A rule-of-thumb law of D oc N -2 is often applied in industry for assessing droplet size change in atomizers that impart large centrifugal forces to the feed liquid. Experimental data has not proven this otherwise as the low exponents (-0.6 to —0.83) have been established only with relatively small atomizers handling intermediate feed rates at low vane loadings. However, size data predicted by using D cc N " or D cc (N d) 4 °' 83 and compared with dried particle analysis of product atomized at industrially high feed rates have suggested the low power relations ( — 0.6 to —0.83) to apply, but in these cases vane loadings were low, as wheels contained numerous vanes. It is interesting to note the low loading conditions upon which experimental 10000 Figure 6.9. Effect of atomizer wheel speed of rotation on mean droplet size (aqueous sprayi). data have been obtained. Generally only low vane loading conditions and low viscous feeds were used, but even in this range a decrease in the power of 'N' accompanied a decrease in vane loading. This is shown in table 6.7 for low viscous feeds. Meyer (41) produced atomization conditions of velocity spraying at low D cc N -2 , but there is no feed rates by using high viscous feeds.and found -2 real evidence to point to the relation of D cc N being more applicable -c to high industrial capacities than D cc N ". Table 6.7. The Relation between Mean Droplet Size and Wheel Speed for Different Vane Loadings for Low Viscous Feeds Author Vane loading lb/hr ft wetted periphery* Power of wheel speed Scott et al. (39) Masters, Mothadi (38) Friedman, Gluckert, Marshall (20) Herring, Marshall (37) 9-80 380-950 800-5500 500-14 500 D cc N -° * 54 D cc N-°. 6 D N -a -° 8 3 D cc N * ' 6 *1000 lb/hr ft = 23.5 kg/hr cm. Wheel peripheral speed range: 100-500 ft/sec (30-150 m/sec). 112 ATOMIZATION 113 THE PROCESS STAGES OF SPRAY DRYING However, the trend in table 6.7 does indicate that if velocity spraying conditions are produced by industrial capacities creating high vane loadings with low viscous feeds or by use of higher viscous feeds at intermediate feed rates, an exponent of N between - 1 and -2 can well be considered acceptable. A working relation of D cc N -1.5 would be justified where vane loadings with low viscous feeds exceed 3 x 10 $ 1b/hr wetted ft (7050 kg/hr cm) for wheels rotating with peripheral speeds in the range 100-500 ft/sec (30-150 m/sec). Such vane loadings can occur in (a) wheels where flow area is minimized to prevent air pumping effects of the wheel, and (b) wheels with bushings for corrosive and abrasive feeds, where flow area is minimized to reduce areas of wear (see under atomizer wheel designs). Further work in this area of high vane loadings is required to substantiate exponent values of N applicable to industrial conditions. However, many industrial atomizers operate at low vane loading conditions due to the atomizer wheel design, which contain numerous high sided vanes. The lower power values established experimentally are more often than not adequate to represent industrial atomization conditions. For maintenance of a specified droplet size at proposed higher feed rates or increased feed solids, wheel peripheral speeds must be increased. From a practical viewpoint, decrease in droplet size is more readily achieved by increase in wheel speed than by increase in wheel diameter. It is advisable to first consider if the atomizer drive has spare power capacity for handling the feed rate at higher speeds, before considering fitting a wheel of larger diameter and operating at the same wheel speed. Often the fitting of an oversize wheel will cause the wheel perimeter to extend outside the atomizer drive lower casing. This creates the possibility of product build-up on the casing and wheel due to inevitable eddies caused by air movement around the wheel edge protrusion. (iii) Effect of Liquid 14scosity on Droplet Size. The variation of Sauter mean diameter with liquid viscosity at constant feed and wheel speed is shown in figure 6.10. Droplet size varies directly to the 0.2 power of viscosity (20). Figure 6.10 is based upon results (20) conducted on a 5 in (125 mm) diameter vaned wheel rotating at 14 000 rev/min. Viscosity of the feed liquid ranged over 1. 0-15 000 cP. Slight variation to the values of liquid density and surface tension accompanied the viscosity changes. Due to the inability to correct for changes in density and surface tension, the slight variations were assumed to have a negligible effect on the droplet size results. At higher peripheral speeds the exponent 0.2 also appears valid. This has been shown (42) by results with aqueous sprays formed from a 5 in diameter wheel rotating at speeds between 15 750 and 24 000 rev/min. For feed rate of 4-10 lb/min, sprays were sampled and the Sauter mean diameter calculated. Such data, when substituted in the group (D vs N'/M") gave SLOPE 02 0.2 0'l c'? Lo • DOB 006 - 9 004 a 002 10.01 V 14 88 0 } c P" n 10 (14681 0-1 ( 1488 ) 0.01 194.88 ) ABSOLUTE VISCOSITY Figure 6.10. Effect of feed viscosity on wheel atomization. values for the group in close agreement with values predicted from figure 6.10. Figure 6.10 thus provides a method to estimate Sauter mean diameter if viscosity data is known. Comparison of experimentally determined Sauter mean diameters with diameters predicted from figure 6.10 are shown in table 6.8. For aqueous sprays, agreement is of a high order. (d) Prediction of Mean Droplet Diameter and Spray Size Distribution In spite of intensive investigation into the mechanism of atomization from rotating atomizer wheels, the prediction of spray characteristics still remains uncertain. The effect of individual variables has been established over a li mited range and are presented in (c) above. There are few general correlations to express atomization features of commercial atomizer wheels. Table 6.8. Sauter Mean Diameter Predicted from Viscosity Data (13,42) (figure 6.10) (A Comparison with Experimentally Determined Values) Wheel diameter 5 in (125 mm) By experiment Group D„ 1\1'6 M 0.2 Sauter mean size (micron) 0.0484 0.0470 0.0485 0.0460 50.2 62.9 52.6 76.6 0.05 0.05 0.05 0.05 Aqueous feed rate (lb/min) Wheel speed (rev/min) Sauter mean size (micron) Group D. .1\1' 6 4.0 7.0 7.0 10.0 24 000 20 600 24 000 15 750 47.3 57.2 49.5 68.5 Where M is lbinnin, D„ is ft, N is R.P. M. By prediction M0'2 H4 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 115 Table 6.9. Relations to Predict Spray Characteristics from Atomizer Wheels Reference 1 (28) Equation D vs = 4.2 x 10 4(N) - ' 6 (p i ) Number 1 °-2 6 °-1 ° 5 ( ) • 1 11 ( 71 -T rz (6.26) Dvs = micron, N = rev/min, h = ft, M L = lb/hr, d = ft, P i = lb/ft 3 , a = dynes/cm, 2 (20) ( Al)p 0.6( Dvs = p i Nr 2 = cP ) 0.2 ( cypin h) 0•1 Mp M i; (6.27) K' = constant, value according to atomization conditions (38) (20) for conditions shown in table 6.5 column (4) K' 0.37 for conditions shown in table 6.5 column (1) K' = 0.40 D vs ft, r = ft, Mi„ = lb/min.ft, N = rev/min, Table 6.10. Comparison between Experimental and Predicted Sauter Mean Droplet Sizes (droplet size in micron) u l = lb/ft.min, a = lb/min e , p i = lb/ft 3 , h = ft 3 (20) D ma „ = 3.0D vs (6.28) 4 (38) D95 = 1.4D vs (6.29) 5 (37) D v1,4 = K mt 24 83 (Nd) * (nl ❑ 12 ° (6.30) D vivi = micron, d = in, M = lb/min, h = in, (39) Dvs = 5240(M p ) °.171 (7tdN) - 0.537 011r °.°17 Wheel speed (rev/min) Equation number 24 000 20 600 15 750 Liquid feed rate (lb/min) Peripheral speed (ft/sec) 486 426 325 (a) (b) 10.0 7.0 4.0 (c) (a) (b) (c) (a) (b) (c) 70.6 48.5 47.3 78.0 54.5 49.5 83.8 57.0 52.0 76.3 53.4 53.7 85.4 60.3 57.5 91.7 63.4 60.0 894 63.5 58.2 100.0 96.6 64.9 107.3 76.0 68.5 (a) Equation (6.26). (b) Equation (6.27)• (c) Experimental results (38). K = see table 6.11 6 at al. (20) for determination of the Sauter mean diameter of a spray are applicable to pure liquids of low viscosity. These two equations are limited by not being deduced from peripheral speed levels over 300 ft/sec. These speeds are nowadays common in industrial applications. Furthermore, all experimentation has been carried out on simple liquid systems, thus drawing doubts on the applicability of the equations to likely atomization characteristics of complex solutions, slurries and pastes that form many spray dryer feeds. However, comparison of experimentally derived values with those predicted theoretically by these equations when applied to high peripheral speed conditions (38) shows close agreement between measured aqueous spray and the spray predictions by the Friedman equation (6.27) but not with the Frazer equation (6.26). Such a comparison is shown in table 6.10. (6.31) Dvs = micron, Mp = g/sec,cm, d = cm, N = rev/sec, ul = poise Available correlations are- given in table 6.9 and conditions under which they were determined are given in table 6.5. Wheel performance at low peripheral speeds (50 ft/sec, 15 m/sec) is reported and illustrated photographically by Golitzine (43), but although the account is comprehensive, it cannot be applied to peripheral speeds of commercial importance (200-500 ft/sec, 60-150 m/sec). Within this higher speed range, droplet formation cannot be studied visually, and spray characteristics are predicted from empirical equations, the validity of which has been established experimentally from analysis of sprays. (1) Mean Droplet Diameter. For peripheral speeds up to 300 ft/sec (90 m/sec), the equations (6.26) and (6.27) proposed by Frazer (28) and Freidman In fact the experimental results for mean droplet size follow the dimensionless groups of equation (6.27), but with a constant reduced from 0.4 to 0.37. The Friedman relation between mean and maximum size equation (6.28) cannot be considered totally reliable. Measured maximum droplet size, when defined as the size below which 95 % of the spray is included appeared only 1.4 times greater than the measured mean droplet size. Equation (6.30) represents the volume mean diameter taken from the relation proposed by Herring and Marshall for prediction of size distribution 4 data. The constant (92.5 x 10 ) represents an average value. Comparisons between actual and predicted spray sizes have indicated that predicted values more closely resemble actual values if different values of this constant are used for various atomization situations. These values are given in table 6.11 related to dryer sizes. The atomizer operating conditions that relate to dryer sizes are given in table 6.12. It follows from table 6.11 that in small diameter test dryers (case I) where very high speed small diameter wheels are used at low feed vane loadings, fine spray sizes are obtained. The value of the constant is low. In pilot plant 116 ATOMIZATION 1 17 THE PROCESS STAGES OF SPRAY DRYING dryers (case II), a semi-industrial atomizer size is often employed, and at the feed rates employed is really over-sized. Fine sprays are obtained when the atomizer is run within its designed range, usually at peripheral speeds 300-550 ft/sec (90-170 m/sec). The value of the constant is also low. In industrial dryers of medium capacity (case III), the atomizer operates at rated capacity and speed. Sprays of high homogeneity are formed having larger mean diameters. The value of the constant increases accordingly and approximates to the average value quoted in equation (6.30). If the atomizer is run specifically at low peripheral speeds large droplet sizes are obtained and this is represented by increase in the value of the constant (case IV). For industrial dryers of large capacity (case V), the atomizer wheel has an extensive wetted periphery, and is sized to rotate with a high peripheral speed. Low vane loadings are maintained and for low viscous feeds, fine sprays of high homogeneity are produced, as depicted by a reduced value of the constant. For all dryer sizes, values of the constant will vary according to the product atomized and the wheel design. This is especially so if the wheel design differs considerably from the more common vaned types. When operating the dryer on a set product, the value of the constant for the dryer size and product can be established by wet analysis of the atomized spray. The values of the constant given in table 6.11 are offered as a guide to atomization assessment and to obtain data for first design calculations. Equation (6.31) has been proposed by Scott et al. (39) and represents the Sauter mean diameter of sprays formed by a small diameter atomizer wheel rotating at very high speeds. It is applicable to predicting droplet size in laboratory sized dryers of small diameter. The influence of each variable on the mean size is correlated by a simple exponential equation. Predicted values of mean diameter show close agreement to measured values when droplet sizes do not exceed 60 micron. Ce CN -e I II III IV V Drying situation and dryer size Dryers in general Small diameter test dryers Pilot-plant and, small scale production dryers Industrial dryer, medium capacity, peripheral speed greater than 200 ft/sec (60 m/sec) Industrial dryer, medium capacity, atomizer peripheral speed less than 200 ft/sec Industrial dryer, large capacity r - * This is an average value as used in equation (6.30). Modified value of constant for use in equation (6.30) 99.0 x 10 4 86.0 x 10 4 ett Ce 1 ems 5 0) 92.5 x 10 4 * 85.0 x 10 4 83.0 x 10 4 94.0 x 10 4 ix 71 • Table 6.11. Values of Constant in Equation (6.30) for Given Dryer Size Case 00 Ce 0 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 119 (it) Size Distribution. Size distribution data of sprays are best represented by the relation of Herring and Marshall (37). The relation is represented on square root probability paper by a plot of the group 0 0 0•8301/00•12 -4 C). 6 6 z FOR DATA ON CURVES SEE TABLE CO WHERE X 1 1 1 1 I I I I Np 0, 0 0 o I d ill o o C7 0I 1 1 , C ❑ NVHI SS31 39tl1N3Dd3d 3wrrion 3Alivinmn3 0 - co ••■ 1 1 LO O ca p oa C••• ❑ 0, Q p 0 C. 0 C , 1 0 In 0 NVH.I. SS31 30VIN33d3c1 31•JMOA 3A 11V 1111.4'13 - FOR DATA ON CURVES SEE TABLE 6.12 1 E a, WHERE X - against the cum ulative volume percentage less than D, the selected droplet h size. Plots are s o wn in figure 6.11(a) for size distribution data obtainable from laboratory and pilot plant dryer sizes, and in figure 6.11(b) for size distribution data obtainable from production sized dryers. The range of operational variables applicable to curves A-E are listed in table 6.12. Data are largely lacking for atomization of liquids other than water at high peripheral s peeds. Predictions of spray characteristics at high speed or sizing of wheels t o meet given spray characteristics are best carried out by applying the correlation on which figures 6.11 are based. Use of equation (6,27) with a m odified constant, particular to the product atomized is often adopted. The m odified constant can only be obtained from product drying experience. The Friedman-Gluckert-Marshall correlation does offer a quick method to scale-up wheels to handle a higher feed rate yet maintain a constant size distribution. Inspection of equation (6.27) shows that if vane height or number of vanes is increased to maintain the same conditions of feed rate per wetted periphery at increased feed rates, the predicted mean and maximum droplet size remains virtually the same. Thus if feed rate per wetted periphery i s ma intained the same on wheel scale-up based upon a constant wheel diameter, mean droplet size will be reproducible. For example, if a 50% increase in feed rate is required, without changing droplet size, the vane height can be increased 1.5 times to maintain the same feed rate per wetted periphery. All groups on the right-hand side of the equation (6.27) remain the same for the new feed rate conditions, except for that last, where there is an increase in value by the factor (1-5) 0 ' 1 or 1.04, Predicted mean droplet size from the scaled-up wheel is only 4 % higher than size obtained l by the quick sca e -up method based upon equal feed rate/wetted periphery conditions. This is subject to the authenticity of the Friedman-GluckertMarshall correlation for the atomized conditions considered. EXAMPLE 6.2 An industrial atomizer, fitted with a 9 in wheel operates at 18 000 rev/min, A fine atomization is required and the wheel contains 240 vanes (g in height). The feed rate is 2200 lb/hr. Predict the mean and maximum droplet size in the spray. The feed properties are p i = 70 lb/ft 3 , v= 74 dynes/cm, pt i = 1 cP. _C L -"- ) (6.30a) X x 10 4 0 (D(Nd) mi..24. 21.63 B 118 6 120 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION Method I : Friedman equation (6.27), Data surface tension (o- ) --- 5 x 10 2 lb/min 2 viscosity (A) = 4 x 10 -2 lb/ft min Function becomes D x 21 100 x 1.71) = 1.52D 4 2.37 x 10 Referring to figure 6.11(b), curve C Total wetted periphery = 240 x 0.375 7.5 ft 12 50% cumulative = 94 95 % cumulative = 176 2200 Mass flow per total wetted periphery - ( = 4.9 lb/min ft 99.95 % cumulative = 289 60 x 7.5 Wheel radius = 0.375 ft Substituting in values: Mn 0'6 Lp 1 Nr2 r 1 0.2 r 1.84x 10' 4 x 10 - 210.2 = 0.382 4-9 [Ni p] G. ' FL apinhl M _1 therefore 94 = 1.52D v m D vm = 62 micron 1•52D 95% D 95 = 116 micron D„, a „:D 99 . 95 % cum = 289 = 1.52D max Dmax = 190 micron Dvm:Dsoxciim = 10,6 4.9 2 L70 x 18 000(0.375) ] D 95 : D 95 x cum = 176 Size Prediction (micron) [5 x 10 2 x 70 x 7.5i" = 2.54 4.9' D Method I Method H Average Dvm 89* 62 75.5 (a) Sauter mean droplet size Use equation (6.27) with K' = 0.37 as vane liquid loading is low. Dmean DVS 75.5 53* 64.25 Dvs = 0.37 x0.375 x 1.84x 10 -3 x 0.382 x 2.54 = 2.40 x 10' ft D95 106 116 111 Dmax 226.5 190 208.25 = 75.5 micron (b) Size below which includes 95 % of spray (equation (6.29)) D 95 •=• 1.4D v5 = 106 micron (c) Largest droplet size (equation (6.28)) D max = 3.0D v5 = 226.5 micron Method II: Herring-Marshall correlation (Equation (6.30), required units shown in table 6.9) Data as in Method I (Nd) °. " = (18 000 x 9) 0 ' = 21 100 (nh)0•12 t24. (240 x 0.375) 0 ' 2 = 1.71 /2200\ 0.24 = 137 121 * Denotes an estimated value as volume mean diameter usually exceeds the Sauter mean diameter by 15-20%. Values of D mean and D95 establish the spray homogeneity, and define the particle size range expected in the dried product. It can be seen from the results that a fair degree of agreement exists between the two methods for predicting droplet size. Reviewing the results that established the two methods (20, 37), values predicted by Method II showed differences from values predicted by Method I by varying degrees. These differences were explained by such factors as different sampling and droplet sizing procedures. Practical experience has shown Method II to be more representative of low vane loading atomization. EXAMPLE 6.3 In developing the spray drying of an inorganic salt on a large-scale, pilot plant drying tests were conducted to obtain data on dried product characteristics and suitable drying conditions. A 24 vaned (4.75 in diameter) 122 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION atomizer wheel (vane height 1 in) was used . Operating at a feed rate of 220 lb/hr, and wheel speed 12 000 rev/min, dried product was obtained having a sieve analysis of > 120 micron 0.5 >100 micron 2.5 > 75 micron 19.0 % > 60 micron 56.0 > 44 micron 86.0 Estimate the change in size the spray droplet undergoes during drying. The feed liquid is of low viscosity and the dried product contains a fair percentage of spherical particles. Solution. Assume feed density and viscosity approximates to that of water, which justifies use of the Herring-Marshall relations. Units given in table 6.9. Hence : , (N ❑ i" = 8860 ol h ❑ .12 = 1.46 (m0 24 = 1 . 37 ❑ Substituting in Herring-Marshall relation (equation (6.30)) Yx„ um = D x 0.942 For these operating conditions : Wetted periphery = 24 in Feed rate per unit wetted periphery = 0.153 lb/min in peripheral speed = 249 ft/sec Based upon data, the predicted wet spray size distribution is obtained from figure 6.11(a) (curve B), where Ys = 44 Y50%= 83 Y95% = 137 Hence : size analysis of wet droplets D 5% = 46.7 micron /3 50 .4 = 88.1 micron D„cx = 145.5 micron 123 From plot of sieve analysis data of dry product % =- 36 micron D 5 ❑ % = 62 micron D 93% = 96 micron Estimated reduction in droplet size during evaporation = 24-34 %. 6.4 The product used in example 6.3 was next test dried in a larger capacity dryer, an industrial spray dryer of medium size. The purpose of the tests was to obtain additional size distribution data to enable the prediction of atomization characteristics for spray drying the product at a feed rate of 21.5 ton/hr using a high capacity vaned atomizer wheel (7.5 in diameter, 24 vanes, 0.62 in wetted height) at 13 000 rev/min. The additional tests were conducted with an 8.25 in diameter vaned wheel, having 4 vanes of wetted height 0.62 in. Operating conditions and the sieve analysis of the dried product are given below. The same feed solids concentration was used throughout : EXAMPLE Feed rate (lb/hr) Wheel speed (rev/min) Sieve analysis > 120 micron > 100 micron > 75 micron > 60 micron > 40 micron Test I 1140 11 250 Test II 1230 8650 3% 10 % 28 % 44 % 73 % 12.5 27.5 53.0 64.0 84.0 Using the above data, estimate the droplet shape change that occurs during evaporation, and predict the particle size distribution of the product obtained from the high tonnage operation. TEST Applying the Herring-Marshall relation (6.30a) (units given in table 6.9) Y`xcum = D x 0.7302 Now feed rate (M,) = 19 lb/min Peripheral speed (VT ) = 408 ft/sec Feed rate/unit wetted periphery (M r ) --- 7.66 lb/min in Conditions suggest use of figure 6.11(b) (curve E) Size analysis of wet spray 124 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 125 200 yx c u m X Wet spray prediction (micron) 5% 50% 95% 40 86 151 55 118 207 200 1 60 H 120 TEST II Applying Herring—Marshall relation (6.30a) Y%cum = D x 0•576 40 Now M = 20.6 lb/min VT = 311 ft/sec 00 80 120 1 60 200 240 260 Mp = 8.3 lb/min in 320 350 404 rwcRoNs PREMTED WET DROPLET 512E Figure 6.12. Size relationship between droplet and particle in example 6.4. Conditions suggest use of figure 6.11(b) (curve E). Yzcum X Wet spray prediction (micron) 5% 50% 95% 40 86 151 69 150 264 Applying the dried particle size data to the large tonnage operation, and employing the Herring—Marshall relation. Yx,cum = D x 0.384 Now M = 805 lb/min The relationship between wet droplet size and dry particle size is obtained by comparing the above wet prediction with the corresponding dry product sieve analysis. This is given below : Test T Wet Dry Wet Dry D5 55 118 207 20 56 113 69 150 264 28 74 145 D95 Mp = 54 lb/min in Conditions suggest use of figure 6.11(b) curve E for wet spray size. Corresponding dried particle sizes are obtained from figure 6.12. Test II Micron D 50 VT = 425 ft/sec Wet °4.. D5% The relationship between wet droplet size and dry particle size is given in graphical form in figure 6.12. D 59% D 95% X 40 86 151 Dry (micron) 108 224 394 51 121 205 126 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 127 Predicted dry product analysis becomes : 200 micron X150 X120 > 100 > 75 > 60 > 40 7 27% 50% 66 85 93% 98% (iii) Weight Distribution of Sprays. The weight distribution of sprays from rotary atomizers has been reported by Adler and Marshall (26). Herring and Marshall (37), Frazer, Eisenklam and Dombrowski (28) and Friedman, Gluckert and Marshall (20). Attempts were made to predict the weight distribution of a spray that falls within a given radial distance, The spray from a rotary atomizer is ejected horizontally. Each droplet size in the spray will decelerate by air friction at different rates. For still air medium conditions, droplets of different size will fall under gravity at different radial distances from the atomizer. The distribution in the vicinity of the atomizer is complicated by the air movement created by the atomizer rotation, but at distances of 3 ft (1 m) or more below the wheel, air movement due to the rotation is less significant, and a weight distribution can be obtained by collecting droplets that fall into radial zones around the atomizer. A typical weight distribution plot is shown in figure 6.13 for various atomizer designs operating at equal peripheral speeds and feed rates. The sampling plan was 1 metre below the atomizer. 00 ATOMIZER DIAMIETER: 125mm ATOMIZER 5PEE3 : 15,750 RPM F- A z cc 75 C LU 0 0 1— = 50 > 25 0 3 1 2 Radial distance from rotary atomizer 4 Figure 6.13. Spray weight distribution from rotary atomizers (sampling plane 1 metre below atomizer): A, wheel: 24 high vanes; B, wheel: 24 low vanes; C, wheel; 8 low vanes; D, disc: vaneless. Four different designs are shown. Each has a diameter of 125 mm, and speed of 15 750 rev/min. The feed rate is 1000 kg/hr. Figure 6,13 illustrates the atomizer producing the coarser spray to traject the spray over longer radial distances. The radial distance within which a given weight percentage of spray falls can be taken as inversely proportional to speed to the power 0.2, i.e. (N - 0 ' 2 ), and directly proportional to feed rate and diameter to the power 0 , 2, i.e. (ma, 2 d ° ' 2 ). This is an imprecise relationship, as the effect of the chamber walls, air flow, and wheel air pumping will influence the actual spray trajectory. During spray dryer operation, the drying air flow completely disrupts the theoretical spray trajectory and droplet fall. Data predicted from collection of droplets following trajectory in still air must be used with great caution if applied to actual dryer conditions. Droplet and spray trajectories are discussed in more detail in chapter 7. (a) Atomizer Wheel Performance During Spray Drying The majority of experimental conditions under which spray analysis studies have been conducted neglect influence of the drying air entry around the atomizer and air flow caused by wheel rotation. Theoretical spray and particle characteristics will differ from those in reality, as the liquid released from the wheel periphery is subjected to (i) air flow of the wheel pumping effects, (ii) drying air entry and (iii) any particle shape change that occurs during drying. (i) Air Pumping Effects. Little specific information is available on the effect of air pumping on spray characteristics. The mechanism of spray formation would suggest air flow by air pumping to assist atomization, but in a fashion not conducive to homogeneous spray formation. Air pumping is seen more as a primary source of energy loss than as a variable governing particle size of the dried product. Energy losses in small wheels can be quite substantial when compared to atomization energy requirements. Air pumping can effect product quality. It tends to aerate the liquid within the wheel, resulting in low bulk density products. Wheel design must minimize this effect if high bulk density products are required from low viscosity feed liquids. Air pumping effects contribute to spray-air mixing in the wheel proximity. In pilot plant spray dryers, air pumping has a considerable influence on the resulting air/droplet flow within the drying chamber. In industrial dryers air pumping has a negligible effect on overall air/spray flow within the chamber. Flow is governed solely by the air disperser design. Air pumping can, however, contribute to the formation of deposits on the surfaces on the wheel and atomizer drive casing. These deposits become scorched eventually, as they lie in hot air regions. The passage of air through a rotating vaned wheel is shown in figure 6.14. The vanes move the air outwards creating regions of low pressure over the 128 THE PROCESS STAGES OF SPRAY DRYING ATOMIZER DRIVE ATOMIZATION 129 CASING AIR DISPERSER LIQUID DISTRIBUTOR AIR FLOW PATTERNS AI R FLOW VANED WHEEL A Figure 6.14. Air flow through vaned atomizer wheel due to air pumping effects. PRESSURE DISTRIBUTION wheel top surface. Air ejected from the vanes draws in air from beneath creating a recirculatory air flow below the wheel. The likely pressure configuration around the atomizer in conjunction with a ceiling air disperser is illustrated in figure 6.15. The pressure distribution is plotted over the wheel centre line. Drying air entering the dryer through the air disperser passes along the outer surface of the atomizer casing and travels towards regions of lower pressure. The hot air will flow into the clearance between the wheel top surface and the base of the atomizer casing. Hot air enters the wheel causing partial drying of product in the interior. Spray droplets leaving from the upper surface of each vane will be entrained by the air flow into the clearance, especially when the air flow is excessive. Semi-wet product will be deposited on the metallic surfaces, dry out, and eventually be scorched by the hot air environment, Spray droplets and air leaving the lower surfaces of each vane possess sufficient momentum to further entrain air from beneath the wheel. Local eddies are set up with the likelihood of product being deposited on the lower surfaces of the wheel. Air flow through the wheel must be restricted as much as possible for the cleanest atomizer operation. This can be achieved by : (a) A minimum clearance between the wheel and atomizer casing. (b) Vanes are sized to provide a sufficient atomization surface, and yet to possess a cross-section area that reduces the air pumping capacity of the wheel to a minimum. (c) Restrictions to air flow are designed into the wheel top surface and liquid distributor. (d) Replacement of vanes by annular orifices (bushings or jets) CHAMBER PRESSURE REGION OF LOW PRESSURE AT WHEEL CENTRE, Figure 6.15. Pressure distribution at vaned atomizer wheel due to air pumping effects, so sized that the feed liquid substantially fills the orifices when air passages become virtually negligible. In case (d), atomization characteristics often deteriorate by use of jets instead of vanes for feed rates rated on vaned wheel loadings. Orifices restrict air flow, but atomization surfaces become insufficient to handle the feed rate effectively. The usual arrangement for vaned wheels to prevent excessive air pumping effects in industrial sized dryers is shown in figure 6.16. There is a minimum clearance between the wheel and the atomizer drive casing. The air pumping capacity of the wheel is met by the wheel drawing cool air from outside the atomizer. The cool air flows into the low pressure regions above the wheel. Hot air and entrained spray are no longer drawn into the top clearance. The cool air drawn into the wheel interior also prevents partial drying of product within the wheel. (ii) Drying Air Entry. The manner of drying air entry into the drying chamber is determined by the air disperser design, and controls the evaporation rate of the atomized spray. The actual position of the atomizer with respect 130 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING AIR FEED FA N FEED AIR FILTER 131 6 . W , 1 usur AIR LIQUID PEED PIPE B. FEED FEED AIR C COOL AIR FLOWS TO WHEEL FEED VANED WHEEL Figure 6.16. Arrangement for supplying cool air to atomizer wheel. Cool air supply to meet air pumping capacity is obtained by: A. Use of a small fan. B. Suction of air through a filter using wheel's own suction ability. A minimum clearance between wheel and atomizer casing,is maintained (see C) to limit air flow over wheel top surface. to the air • disperser is an important factor in the efficiency of the dryer. Dried product properties of a given material will vary according to the positioning of the atomizer. Figure 6.17 illustrates various rotary atomizer positions adopted in drying chambers and shown in relation to the air disperser. Further details on drying air entry and air flow within the drying chamber are given in chapter 7. (iii) Particle Shape Change. In all cases, it is the final size of the dried product that is of interest to the spray dryer operator. Apart from the importance of atomizer performance, it is essential to know the relationship between the size of droplets before and after drying. Unfortunately, there is no sound basis to draw conclusions as feeds vary so much in their physical properties and sprays dry in different manners. The relationship between the size of wet spray droplet and its size when in dried form can be expressed by a shape change factor (13). The shape change factor covers any droplet shrinkage or puffing during evaporation. AIR --b- — AIR AIR Figure 6.17. Positioning of rotary atomizer in relation to air disperser. The relationship between wet and dry forms is represented by D w = /3DD (6.32) where D w is the droplet size on atomization, and D, is the particle size in dried form. The shape change factor (/3) will vary for each product and each droplet size making up the spray distribution. Drying temperatures also effect the magnitude of /3. Values of fi are determined experimentally for a given product by observing the evaporation of a specific wet droplet size in constant air temperature conditions. When atomizers produce wet spray distributions 132 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION that can be equated to a distribution function, values of /3 can be obtained from sieve or other analysis of the dried product. Comparison between the dry particle distribution and the predicted wet droplet distribution gives an immediate value of )3 for a given wet droplet size or for a given wet droplet size increment. The shape change factor (/3) proves useful data in cases of required dryer scale-up. It is not uncommon to ascertain what alterations are required to atomizer control for maintenance of a given product quality (i.e. particle size), when dryer capacity is enlarged, feed concentration varied, or atomizer wheel design changed. The wet droplet size on atomization follows the relation -t D w oc (6.33) . (d) . (N)Fr (h)' (n) Equation (6.36) can further be modified to include the dryer evaporation capacity, as the feed rate can be expressed in terms of the evaporation capacity and feed moisture content. Thus 100 100 — 100/(1 + 0.01H)1 M = E[ or (6.37) M=E ofy and dried particle size is related to the operating variables through equations (6.32) and (6.33). Values of the exponent for each variable can be taken from table 6.6. Exponent values generally used for low vane loading conditions are : ,. = 13 - m()•2 1V1 L4 2 “2 r...2 'f 2 1 (6.35) A relation covering atomization variables and feed properties, and their interaction for maintenance of a given particle size can be derived from equation (6.35), as A,f0.2 '" 1 1 -ill 2 -10 . 2 L0.1 0.1 ro - 0.01 [,40.210.1„0.1m-0.6] [R n 1 iv '4 2 it2 "2 2 P2 [ "1 "1 (6.36) (6.39) Change in feed solids of the feed concentrate while maintaining a constant dryer evaporative capacity and atomizer wheel design. The required wheel speed to produce the same dried particle size is obtained from equation (6.39) where E 1 = E2, d 1 = d 2 , n 1 = n 2 , and h 1 = h2 . (6.34) . N o.6 m0.2 „.1. 2 [Ni' 6 {E 2 (1 + 0.01H 2 )/0.01H 2 } 0.2 {.E 1 (1 + 0.011/0/0.01H i l' 2 $ 2 4 2 4' 1 4 1 N2 ( 2 4 '4 i n?' N CASE 1 or 2D0 2. 1 dVh?' i ni' 1 NV Equation (6.38) provides a useful correlation to select wheel speed for maintaining particle sizes on alteration of feed properties and interchange of wheel design. This is evident by rearranging equation (6.38) m0•2 r 1- {E 1 (1 + 0.01H )/0-01H } ° ' 21 rE 2 (1 + 0.01.1/ )/0.01H I 'l /3/2(6.38) 1_ The above values cannot be considered applicable to all products. For certain products (for example, those exhibiting thixotropic flow properties) different values have been shown through experience to more closely represent the effects of any variable change on droplet size. The most suitable power values must be applied. In the vast majority of applications the above values will suffice. By combining equations (6.32) and (6.33) and applying the above power values fiD D oc d ru, • 0.01H where E = evaporation capacity of dryer, H = percentage moisture in feed (dry solids basis). By substituting equation (6.37) in equation (6.36) 1 Exponent (p) of feed rate (M): + 0.2 Exponent (q) wheel diameter (d): — 0.2 Exponent (r) wheel speed (N): —0.6 Exponent (s) vane height (h): — 0.1 Exponent (t) number of vanes (n): —0.1 133 .6 [Nr{(1 + + 0.01.11- 1 )/0.01H 1 r'fl 2 (6.40) CASE 2 Change in dryer evaporative capacity while maintaining the same atomizer wheel and feed properties. The required wheel speed to produce the same dried particle size can be predicted from equation (6.39) where d 1 = d2 , h i = h2 , n i = n2, Pi = 13 2 N2'6 2 — [m- 0.6 ( 1 2) °.21 El (6.41) 134 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING 135 Therefore CASE 3 Change in evaporative capacity accompanied by change in feed solids, but maintenance of the same wheel design. d 1 = d2 , h, = h2 , n 1 = n2 . Thus from equation (6.39) 6 N2' = 15 000'6 [0_600(1 + 0.01($2)) 0. 01(82)} ° ' 2 100/3 1 {800(1 + 0.01(122))/0.01(122)} 0 ' 2 95fi 2 = 3204 x 1.191 x 1.05 NO.6 NINE2(1 0-01H2)/0•01H2r.2/3I {E 1 (1 + 0.011/0/0.01H11 .2 132 (6.42) CASE 4 Change in evaporative capacity accompanied by change in feed properties and use of different wheel design. The prediction follows equation (6.39). EXAMPLE 6.5 A rotary atomizer is operating successfully at 15 000 rev/min in a dryer of 800 kg/hr evaporative capacity. If the same wheel and atomizer drive is transferred to a dryer of 1600 kg/hr evaporative capacity and operated on the same feed concentrate, what wheel speed must be applied to reproduce the same spray characteristics? In equation (639) d 1 = d2 , n, = n2, h 1 = h2, 16 1 = P2' Hence equation (6.41) is applicable N' 6 = 115 000 0.6 (1600/800) 02 1 N ° ' 6 = 368.1 N = 18 900 rev/min EXAMPLE 6.6 Calculate the required wheel speed of the atomizer as in example (6.5) to maintain product particle size if, for operation in the larger dryer, the feed concentration is raised from 45-55 % solids by weight. It is estimated that the factor governing the relation between wet droplet size and its corresponding dry particle form will decrease 5 % as solids concentration is raised to the new level. Equation (6.39) reduces to equation (6,42) as d i = d2 , n, = n 2 , h, = h2 . Data : N, = 15 000 rev/min E, = 800 kg/hr E2 = 1600 kg/hr 0.95/3, H2 = 55/45 = 1.22 lb/lb (122 % moisture dry solids basis) H 1 = 45/55 = 0.82 (82 %) N2 = 22 630 rev/min (f ) Atomizer Design Requirements Atomizer design is focussed upon the need to produce homogeneous sprays over a wide range of feed rates from a machine that is thoroughly reliable, and requires a minimum of preventative maintenance. The rotary atomizer must be dynamically balanced. Feed liquid distribution on to the wheel must be uniform, with no splashing on any wheel surface. Atomizer rotation must be vibration-free. Vibration causes likelihood of frequent mechanical failure. Smooth running of atomizers is of particular importance in large industrial dryers. Out-of-balance wheel rotation becomes more pronounced in atomizers designed for high peripheral speeds and large wheel liquid loadings. Flexibility is of great importance in atomizer design. The atomizer must handle a wide range of feed materials and yet have an operation controllable to produce any desired product specification. In meeting these requirements, many designs are offered by manufacturers. Atomizer design can be divided into. three parts : (i) The atomizer drive. (ii) The liquid distributor. (iii) The atomizer wheel. An industrial atomizer features a spindle rotating in heavy duty, high speed bearings that are fully lubricated. The wheel is mounted on the spindle and securely fastened. As the spindle and wheel rotate, feed material is fed to the wheel centre via the feed pipe and liquid distributor. The basic features of the atomizer design has been illustrated in an earlier chapter (figure 5.4). The wheel speed, feed pipe diameter and size of liquid distributor are selected according to the feed material atomized. The atomizer can handle feeds in solution, suspension, paste or powder form. The atomizer drive can be at fixed or variable speed. The feed pipe can be heated for handling liquids that tend to solidify at normal temperature levels. (i) Atomizer Drive. The atomizer drive rotates the wheel within a specified speed range and loading conditions. The drive can feature (a) the turbine principle, (b) gearing to gear up an electric motor, (c) a direct driven electric motor (fixed speed) or electric motor with frequency converter for speed control, (d) a belt drive. All have their advantages and disadvantages, whether they be reliability or cost. All drives must ensure that the operating speed of the atomizer does not correspond with the shaft speed, where natural vibration occurs. The various drives are shown in figure 6.18. 136 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION ELECTRIC MDTCR The power requirement for driving a vaned atomizer wheel is directly proportional to the square of speed at fixed feed rate, and not the cube of speed, the usual relationship for fan and pump performance. The wheel acts as an air pump or fan, but the common law does not apply. Increase in speed does not increase the liquid feed rate, as this is controlled externally of the atomizer. The theoretical net power consumption for vaned wheels is given by equation (6.43) (35) C04.1PRESSED AIR PIPE (a) 137 PK -=` 6.65 x 10 -12 M LN 2 (2d 2 (b) d,2,) (6.43) where PK is kw, N is rev/min, d, d d is in, M L is lb/inin. In practice, power consumptions of atomizer wheels will exceed values predicted in equation (6.43) as further power is required to overcome friction within the atomizer drive, and to power air through the wheel as a result of the air pumping effect. There is no general correlation available applicable to all atomizers as the power requirements of an atomizer wheel and atomizer drive system depends upon the designs employed. It is usual procedure for atomizer manufacturers to express the power requirement in the form of power per unit increase in feed rate (water basis) quoted at a reference wheel diameter and speed. The power variation with changes in feed rate and wheel diameter at a constant reference speed is expressed by (c) 1 2 PR = K n u1. .1[1 s III i DELT DRIVE a HEAR PDX ) FEED PIPE 1i —%115 mff 1111 u IM- I , ,. (d) VANED WHEEL IN (6.44) R uR where MAR DOE Muil. — 1 " ELECTRIC HOVER FEED PIPE IMItail ir RIFE71 - Fi ,1 SPIIJILE I 'MED WHEEL (e) PR = required power at reference wheel speed K = constant for given atomizer wheel and drive system (power requirement/unit increase in feed rate) • M, = operating feed rate MR = reference feed rate on which K is based d = operating wheel diameter d R -= reference wheel diameter The total power requirement of the atomizer (P K ) is given by K P Figure 6.18. Atomizer drives. (a) Turbine drive. (b) Direct belt drive. (c) Direct drive (electric motor with frequency converter). (d) Gear and belt drive. (e) Gear drive. P R + P1 where P, --- idling losses of the atomizer. (6.45) 138 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 139 Power requirements at speeds other than the reference speeds are obtained from equation (6.46) using P i, from equation (6.44) Ni 2 P2 = PR [- (6.46) NR where N = operating wheel speed NR = reference wheel speed P2 = power for required operation Atomizer Drives for Fractional Feed Rates. In spray dryers for laboratory use, chamber diameters are small. Very fine sprays are required to enable completion of evaporation in the limited residence times available. To obtain fine sprays small wheels are rotated at very high speeds. Where air turbine drives are used, speeds of the order 50 000 rev/min are reached. Electric motor drives with gearing enable 40 000 rev/min to be obtained with reliability. A vaned atomizer wheel with turbine drive is shown in figure 6.19(a). Atomizer Drives for Pilot Plant, Semi Industrial Industrial Feed Rates. For plants up to and including industrial applications involving moderate feed rates, belt drives often power the atomizer. If wheel liquid loadings are not high (e.g. drying low solid concentration feeds) a belt can drive the spindle directly. A V-belt drive to the atomizer via a gearing system is a more robust unit, however, and can handle higher wheel liquid loadings. Figure 6.19(b) shows an atomizer with a worm gearing system belt driven from a 35 HP motor. The 82 in (210 mm) diameter wheel rotates up to 15 000 rev/min (peripheral velocity = 335 ft/sec (110 m/sec)), where feed rates up to 2.0 ton/hr can be atomized. With reduction in wheel speed, atomizer capacity can be increased to 4.5 ton/hr at 10 000 rev/min. V-belts can handle up to 60 HP drive requirements. At higher capacities, direct drives to the atomizer are required. High frequency motors can be connected directly to the atomizer spindle and with suitable control gear, wheel speeds can be easily varied (376). High frequency motors can handle up to 125 HP drive requirements. Where synchronous electric motors are used, the spindle is powered via a gear box incorporating helical gears and vertical shafts. The gear box power transmission is a robust and reliable form of atomizer drive and is most suited to handle large feed rates. Atomizer speeds can be altered by change of the gear train in the gear box, but it is more common and convenient to control speed by a fluid coupling mounted between the atomizer gear box and the electric motor. An atomizer with a fluid drive is shown in figure 6.20. The positioning of the fluid coupling beneath the electric motor is illustrated. - — (b) (a) WA (c) ' (d) Figure 6.19. Rotary atomizer drives for atomizer wheels. (a) Turbine drive (wheel diameter shown = 50 mm). (b) Belt and gear drive (wheel diameter shown = 210 mm). (c) Helical gear drive (wheel diameter shown = 160 mm). (d) Epicyclic gear drive (wheel diameter shown = 210 mm). (By courtesy of Niro Atomizer.) 140 THE PROCESS STAGES OF SPRAY DRYING The fluid drive system is best incorporated with electric motor horse powers of 60 HP and upwards. Figure 6.19(c) shows an atomizer powered through a gear box by a motor mounted over the spindle. Wheel diameters reach 10 in (250 mm) for 100 HP drives. Feed rates of 6 ton/hr can be atomized at 18 000 rev/min. With reduction in atomizer speed capacity can be increased to 16 ton/hr at 10 000 rev/min. In high production dryers, for example, atomizer feed rates up to 50 tons/hr, the drive design shown in figure 6.19(c) is more than adequate. However, a smaller diameter wheel is used (61 in, 160 mm) plus strengthened bearings and gearing for transmitting a power drive of 200 HP. Feed pipes are also enlarged. At such high liquid loadings a maximum speed of 13 000 rev/min is imposed. During operation lower speeds are usually adopted (e.g. 11 000 rev/min). Atomization characteristics at these lower speeds are maintained ATOMIZATION 141 by increasing the vane area of the atomizer wheel. Many industries demand even higher feed capacities, and atomizers with 600 HP drives are now appearing. Such drives incorporate epicyclic gearing systems (figure 6.19(d)). High rotation speeds place great demands on the lubrication of the atomizer. Safety alarm circuits must protect the lubrication system. Special precautions are taken in the atomizer design to prevent oil penetration down the spindle into the atomizer wheel. Many designs incorporate air pressure protection via the spindle (figure 6.21). Miscellaneous auxiliary equipment is available to assist control of the atomizer performance. Tachometers can record spindle speed and detectors can meter spindle vibration. Atomizer wheel drives feature in patents (381)(387). Other patents cover a sterilizable (383) and pressurized drive (384). VENTING OF DRIVE CASING VENTING OF SPINDLE COMPRESSED AIR OR NITROGEN FILTERED AIR UNDER PRESSURE ELECTRIC MOTOR VARIABLE SPEED DRIVE ( FLUID COUPLING1 LABYRINTH ATOMIZER DEAR BOX AIR FLOW DOWN SPINDLE ATOMIZER DRIVE VANED WHEEL Figure 6,20. Rotary atomizer with variable speed control through a fluid coupling. Figure 6.21. Spindle pressurizing. Prevention of drying gases penetrating atomizer drive. (ii) Liquid Distributor. The liquid distributor is placed around the base of the spindle in close proximity to the wheel. This is shown in figure 6.22. Liquid flows on to the wheel as near to the centre as possible. The liquid distributor is often supplied from one or more feed pipes, and designs smooth out the flow around the periphery of the distributor and ensure equal flow 142 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING 143 FEED IN ATOMIZER DRIVE CASING LIQUID DISTRIBUTOR O VANES HOLES A-A B-B WHEEL SPINDLE Figure 6,22. Positioning of liquid distributor with atomizer wheel. into each vane of the wheel. Methods used widely involve (a) imparting rotary motion within the distributor and (b) the formation of a reservoir within the distributor. The reservoir feeds several constant head outlets in the form of holes drilled in the distributor plate. Liquid distributor designs are shown in figure 6.23. Patented designs include (402) (403). The distributor must be leak-proof. Liquid leakage on to the top surface of the wheel results in problems of semi-wet or scorched deposits forming on the atomizer wheel and drive surfaces. The liquid distribution velocity to the wheel must not be so high that splashing occurs. Splashing causes liquid to find its way onto the top of the wheel resulting in problems associated with a leaking distributor. For a selected wheel speed, the distributor must never permit any vane to approach flooding conditions. Imperfect atomization and heavy deposit formation on the atomizer result. Liquid velocities commonly used in distributors range between 9-15 ft/s (3-5 m/s). The liquid distributor is designed together with the atomizer wheel it accompanies. Use of an incorrect design can cause flooding. Flooding prevails when liquid is distributed onto the wheel surface in such a way that the bulk flow arriving on the wheel surface cannot be accelerated away from the central area fast enough. Accumulation occurs with flooding. (iii) Atomizer Wheels. Numerous atomizer wheel designs are available. This is illustrated from the available patents. Designs are claimed to give a spray that dries to a product of desirable characteristics, General wheel Figure 6,23. Liquid distributor designs. (a) Liquid distributor with tangential entry. (b) Liquid distributor with angled slots forming a swirl chamber. (c) Liquid distributor with constant head outlets. design appear in patents (385) (386) (387) (388), a high bulk density milk wheel (389), wear resistant wheels (44) (391) (393), multi-stage wheels (394) (395) (396) and powder—liquid wheels (397) (398) (399). Atomizer wheels produce sprays of high homogeneity over a wide range of mean droplet sizes. Control of size distribution is carried out by change in wheel speed. With excess power available for wheel speed increase, size distribution can be maintained for higher feed rate conditions. Such flexibility of operation ensures dried product qualities to be as desired. Atomizer wheels have many important operational features. The chance of clogging is virtually non-existent given correct wheel selection. The projection of spray into the drying air gives effective spray—air contact for achieving fast drying rates. Maintenance is minimal. These features often tip the scales in favour of rotary atomization in circumstances where alternative atomization techniques could just as well be applied to a product. The atomizer wheel and the drive need precision manufacture, but the operation features offset the high cost of the atomizer. Atomizer wheels are designed to withstand the centrifugal forces they are subjected to during rotation, and designs in fact carry suitable safety 144 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING factors. Due to the elasticity of the wheel material, distortion can take place during rotation. Allowance for distortion enables wheel dismantling for cleaning or parts replacement. The wheel is placed on the end of the spindle. The spindle end is conical so as to facilitate correct wheel centring, easy mounting and removal. The wheel must then be securely fastened to the spindle with suitable locking devices. The wheel is positioned with a suitable clearance between distributor and wheel. Under no circumstances must the wheel rub the distributor during rotation. This can cause (a) sparks and initiate explosion within the drying chamber, (b) atomizer drive spindle fracture, (c) hot spots on the wheel surface, leading to formation of burnt particles in the product. (a) (b) (c) (d) Figure 6.24. Designs of vaned atomizer wheels. (a) Straight vanes. (b) Curved vanes (wheel top cover removed). (c) Wear resistant vanes (inserts), (d) High capacity vanes. (By courtesy of Niro Atomizer.) 145 Selected Atomizer Wheel Designs: Standard Atomizer Wheel (Vaned). This is the multi-purpose wheel having straight vanes (figure 6.24(a)). There are usually 18-36 vanes. The design is cheap to fabricate and requires no special liquid distribution techniques. The wheel is commonly supplied with pilot plant and experimental dryers, being capable of operating over a wide range of feed rates and periphery speeds. The straight channels are virtually clog-free, but the wheel does pump large quantities of air. The vanes can be shaped to form rectangular or oval flow channels. Nozzle Atomizer Wheel. A nozzle wheel features small diameter orifices (jets) instead of channels (476). The air pumping effects are substantially reduced. The wheel finds application where product aeration must be minimized. The limited orifice cross-sectional area for liquid discharge allows only relatively small feed rates to be effectively atomized. Atomizer Wheel for High Bulk Density Products. Present day operations involving high tonnage production often require high bulk density dried products, e.g. dairy products. Designs with curved vanes produce high bulk density powders at high feed rates, figure (6.24(b)). In the case of skim milk powder, 7-10 % increase in bulk density can be achieved over a straight radial vaned design. Apart from increase in bulk density, curved vanes reduce the amount of occluded air in the product, a feature of special importance to products containing fat, e.g. whole milk powder. Atomizer Wheel for Corrosive Feeds. In cases of liquids that are corrosive but not abrasive, it is usually worthwhile to fabricate the whole wheel in a metal resistant to corrosion. Hastelloy, tantalum and titanium are commonly used. Atomizer Wheel for Abrasive Feeds. Problems of excessive wear on wheel surfaces when abrasive feeds are atomized are overcome by incorporating resistance surface (inserts) within the inner wheel body. Figure 6.24(c) shows a wheel with resistant surfaces on each straight vane. The inserts are replaceable. The layout permits particle size distributions, characteristic of straight vaned wheels, to be obtained with abrasive feeds. The importance of these surfaces is illustrated in figure 6.25 where the condition of a standard straight vaned stainless steel wheel is shown after abrasive foreign matter entered the feed accidentally and was passed to the atomizer for a few hours. Use of inserts would have prevented such wear. Atomizer Wheel for Abrasive and Corrosive Feeds. Abrasive and corrosive feeds pose the gravest operating conditions for an atomizer wheel. The high feed velocity over the wheel surfaces causes rapid wear unless the surfaces are protected. All surfaces likely to come into contact with the feed must be adequately protected from abrasion and corrosion. A wheel as shown in figure 6.24(c) can be used, but if the feed is highly abrasive and corrosive, regular maintenance and insert replacement is required. A novel and 146 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 147 wear over the entire surface. This is accomplished by rotating the bushings 90 degrees at a time. For further details on the maintenance of the wheel, the reader is referred elsewhere (45). The wheel design creates several thotand hours of operation per bushing before replacement becomes essential. Such extended operation periods apply to the most abrasive of mineral ore concentrates that are currently spray dried in large tonnages (45)(46)(47). Examples include flotation concentrates from the mineral ore industry. Molybdenum disulphide, clays, fertilizers, cement and cryolite can also be handled. For the wheel design in figure 6.26, any wear is restricted to the bushing. To reduce the cost of bushing replacement, the wheel is fitted with the minimum number of radial bushings for obtaining the specified dried product particle size. Reduction in the number of bushings used in a wheel will increase the coarseness of the resulting spray. Where coarse sprays are acceptable, the minimum bushing requirement offers attractive savings in operational costs. If fine dried particles are desired, the number of bushings are simply increased. Wheels with up to 24 bushings are not uncommon. Wear resistant bushings or surfaces used in wheel operation are usually carbides, when feeds are abrasive and corrosive. In less demanding Figure 6.25. Abrasive wear on vaned atomizer wheel. recently patented antiwear arrangement (44) completely overcomes these problems. A wheel with such an arrangement is shown in figure 6.26. The atomizer wheel features wear-resistant sintered bushings, so placed to protrude within the inner chamber of the wheel. Such arrangement produces a protective layer of solids to be formed right from the start of the spray drying process. Solids separate out from the feed as a layer along the outer wall of the inner chamber. The thickness of the layer corresponds to the projection distance of the bushings. The protecting layer of solids, together with the use of wear-resistant bushings and a wear-resistant base plate enables the wheel body to be fabricated in stainless steel and yet possess a long operating life. The atomizer wheel possesses the most effective and cheapest built-in abrasion control, since the abrasive solids in fact provide their own protective layer. Use of this wear-resistant bushing and base-plate arrangement in a conventional wheel body prolongs the life of the body by several hundred ti mes when operating with abrasive and corrosive feeds. Wear occurs slowly at the surface of the bushings in direct contact with feed concentrate, but bushing life is quadrupled by repositioning the bushings to equalise 00.00000 0 Affair MEN Wheel hub 1. Wheel 2. Inner chamber 3. Wheel periphery 4. Wheel base 5. Wheel top plate 6. Annulus for feed distributor 7. Wear resistant bushing 8. Steel bushing 9. Bushing recess 10. 0-ring seal 11. Wear resistant base plate 12. Protective layer of concentrate 13. Outer wall of inner chamber Figure 6.26. Atomizer wheel with bushings for abrasive and corrosive feeds (45). 148 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING conditions alumina is suitable. Ceramic bushings can withstand higher centrifugal forces than carbides. For the severest of conditions silicon carbide is adopted as a first-rate all-round performer. Tungsten carbide has good wear resistance with neutral solutions, but it is not resistant to strong acids or alkalies (i.e. PH values, 0-5 and 9-14). Acids attack the cobalt binder. Tungsten carbide is susceptible to oxidizing acids. Chromium carbide has less wear resistance but good corrosion resistance. Use of a nickel binder renders the carbide inert to nitric acid. Large Capacity Atomizer Wheel. A double wheel design is used for feeds that provide no atomization difficulties, but where high feed rates must be handled. The wheel consists of two levels (tiers) of vanes, see figure 6.24(d). A double liquid distributor distributes the feed equally into each tier of vanes. By using two or more tiers, liquid loadings on each vane can be maintained low, achieving complete atomization while total feed rates are high. (g) Application of Atomizer Wheels. Applications of atomizer wheels are found in many major industries, including, for example, ceramics, dairy products, dyestuffs, foodstuffs, inorganic chemicals, mining and pharmaceuticals. Such varied application is due to atomizer wheels being able to handle all feeds that have good flow characteristics and a molecular structure that permits break-up of liquid into individual droplets. Through the correct choice of wheel design, feed liquids, slurries and pastes having either heat sensitive, thermoplastic, abrasive, corrosive or high viscous properties can be successfully atomized. Although one atomizer unit is used per drying chamber, there is no reason why multi-atomizer units cannot be applied in very large drying chambers. Where multi-atomizer units are used, drying air is supplied around each atomizer wheel. Atomizer wheels are incorporated with nozzle atomizers (83) in a drying chamber to produce products of special size distributions. 6.5.4. Disc Atomization (Vaneless Bowls, Cups, Plates) (a) Introduction Inverted bowls, cups and plates are classified as vaneless disc atomizers. Unlike atomizer wheels, friction between the liquid and the disc surface is increased to prevent liquid slippage over the surface. Liquid is fed on the underside of the plate or the internal surface of the cup or bowl and is pressed against the surface as liquid flows outwards to the edge. The disc , can consist of single or multi-tiered plates. A multi-tier plate disc is shown in figure 6.27. A cup atomizer is shown in figure 6.28. The difference between bowl, cup and plate-type atomizers lies in their cone-angle. (The cone-angle is defined as the angle the release surface of the atomizer makes with the axis of rotation.) The plate disc cone angle approaches 180° giving the atomizer a flat design of large diameter. The 149 Figure 6.27. Disc atomizer (plate type, multi-tier). (By courtesy of Niro Atomizer.) cup atomizer has a much smaller cone angle giving a longer design of smaller diameter. The bowl atomizer lies in between. At the operating speeds of rotation, feed liquid is distributed on to the disc and attains rotation due to the friction between the liquid and disc FEE D LIQUID DISTRIBUTOR Figure 6.28. Disc atomizer (cup type). 150 THE PROCESS STAGES OF SPRAY DRYING surface. The liquid flows outwards, forming a thin liquid film over the entire contact area. With no vanes present to restrain liquid flow, liquid issues from the entire disc periphery. The mechanism of atomization for plate, bowl and cup type atomizers is similar to that already described in section 6.5.2. Disc design, rotation rate, feed rate and liquid properties (density, surface tension and viscosity) intercombine to influence the final disintegration of liquid into a spray. At low feed rates and low rotation rates atomization is by direct droplet formation. This mechanism changes with increasing feed rate to one of disintegration of liquid ligaments. When the ligaments can no longer accommodate the liquid supply arriving at the disc edge, a film is formed around the complete disc periphery. Sprays are formed by the break-up of this fil m. This is known as the velocity spraying mechanism. At low disc peripheral speeds, sprays of wide size distribution are formed. Increase in peripheral speed improves spray homogeneity. The atomization mechanism stages are illustrated in figure 6.3. Feed rate is expected to have a greater influence if droplets are formed from the velocity spraying mechanism rather than from disintegration of liquid ligaments. This influence is through control of sheet thickness by the feed rate. For optimum performance of vaneless disc atomizers, the liquid layer should be uniform over the entire disc surface. These conditions are obtained through uniformity of liquid supply, vibrationless rotation and smooth disc surfaces. A further prime requirement concerns the manner of liquid distribution on to the disc. The moment liquid reaches the disc surface, it must undergo immediate centrifugal acceleration that renders gravitational effects negligible. Centrifugal forces must exceed ten times gravity for effective atomization. Atomization mechanism of cup atomizers is described by Dombrowski and Munday (30). (b) Fluid Flow over Vaneless Discs Liquid flow over plate, bowl and cup type atomizers is similar. Liquid extends over the atomizer surface as a thin film. Final release of liquid in spray form is prominently in the horizontal direction. The lips of both types can be shaped to provide a small liquid axial velocity component on discharge. For discs operating under spray drying conditions, a liquid film is present at the disc edge, but the film thickness decreases rapidly as the liquid moves away from the edge. The film thickness, once extended outwards becomes dependent upon flow rate, disc rotation and disc diameter rather than liquid viscosity and density. The liquid properties govern film thickness on the disc surface. Droplets formed by the disintegration of this film move away from the disc with a velocity resultant of the radial and tangential components acquired on point of release. ATOMIZATION 151 Radial Velocity (V r). The radial velocity varies according to the Hinze and Milborn (48) equation [Pico 2 Q 2 sin 0 ' 13 (6.47) Vr = 127r2rth ] which rewritten in terms of disc speed, becomes Vr [2/3 1 Q 2 N 2 sin 01 1 / 341 = 3 3 (6.48) 3 where Tir is ft/min, p i is lbs/ft , Q is ft /rnin, d is ft, 1.4 1 is lb/ft min. For a plate-type disc, the semi-cone angle approaches 90°, thus sin 0 = 1. Frazer (28) regrouped equation (6.48) in terms of liquid viscosity expressed in centipoise, and lir in ft/sec. The conversion factor becomes 11/3 =0.043 60 L3 4 x 10-2 The equation according to Frazer (28) for a plate-type disc thus reads N2n211/3 (6.49) yid Tangential Velocity (V 1 ). The tangential velocity component depends upon the velocity acquired by the liquid through frictional effects with the rotating disc surface. The velocity can vary from that of the disc peripheral velocity (nNd) at low feed rates to fractions of the peripheral velocity at high feed rates. Conditions of severe slippage have been given in equation (6.7). These are conditions where the tangential component becomes less than one half of the disc peripheral velocity. As a guide for intermediate slippage conditions, for values of (M/ tord) in equation (6.7) of 500, 1000, the corresponding liquid tangential velocity can be taken as 0.8, 0.6 of disc peripheral velocity (14). The release velocity (V resultant) and angle of release follow equations (6.22) and (6.23). EXAMPLE 6.7 A five inch plate type disc is atomizing 10 lb/min of liquid at 15 000 rev/min. What are the liquid release characteristics at the disc edge? Radial Velocity (K) Use of Frazer equation (6.49) (sin 0 = 1) where p i = 62.4 lb/ft' N = 15 000 rev/min Q = 10/62.4 ft 3 /rnin d = 5/12 ft /./ 1 = 1.0 cP V= 0.043 152 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING Substituting in values 41 ft/sec Tangential Velocity (V T ) Degree of slippage of liquid over disc. Referring to equation (6.7) [10 x 60 x 121 ---- 460 1 x x5 ( 153 to break-up. The ligament diameter can be deduced theoretically by applying continuity conditions to flow in each ligament. Flow per ligament per unit time multiplied by the number of ligaments issuing from the disc edge equals the total feed rate. Hinze and Milborn (38) propose a semi-empirical relation for the number of ligaments (Z) present at the disc edge. Based on experimental data from cups, Z can be equated to : [p1 N2d31 5/ 12 [1 1/6 (6.54) Z = 0.678 ti? Partial slippage conditions as 460 < 1440. Hence use where N is rev/min, d is ft, kt, is lb/ft min, a is dynes/cm. VT = 0.8 Vildi se ) Disc peripheral velocity Table 6.13. Relations to Predict Droplet Size from Vaneless Discs VT(disc) = it dN = 326 ft/sec Therefore VT = 326 x 0.8 = 260 ft/sec Release velocity ( V.iesuitant) (equation (6.22)) 2 + 412)1/2 Vi-esuitant = (260 Atomization mechanism Reference [ Direct drop formation (49) Ligament formation (48) Sheet formation (49) 263 ft/sec Number Equation 3011 DAy = “3 2 27Ep i @rdN) sin 0 D is ft, Q is ft 3 /min, p i is lb/ft 3 , N is rev/min, d is ft, p i is lb/ft min 512 mad) — 111 11/2 ( ( Q (piN2d3) 0.77 DAy = 2 Nd a Units as in equation (6.50) - Release angle (a) (equation (6.23)) tan -1 (41/260) = 9° Note: The resultant discharge velocity can be in practice equated to the tangential component, as 1/T » (c) Droplet Size Prediction Droplet size produced by vaneless disc atomizers varies according to the atomization mechanism applicable to the conditions of disc operation. Relations to predict droplet size are given in table 6.13. For other relations the reader is referred to Dombrowski and Munday (30). For the case of atomization by direct droplet formation (at low feed rates and low disc rotation) droplet size can be equated approximately to the thickness of the liquid film at the disc peripheral surface. Equation (6.50), table 6.13 represents the order of droplet size formed. At the point of droplet detachment, however, the retaining thread of liquid also disintegrates into smaller satellite droplets, but these form only a small percentage of the total liquid flow. At higher feed rates, where droplet formation is by ligament disintegration, the resulting droplet sizes are the resultant of mechanisms described in section 6.5.2. Photographic evidence (48)(49) has shown ligament disintegration from vaneless discs to conform to the Rayleigh instability theory, where droplet size can be obtained from the ligament diameter prior 1.06M 5 2 -6 1.91 x 10 (Nd) 1• (CIA4)°'66 PI [(il/P1) 3 D is microns, M is lb/hr, p i is gicm , a is dynes/cm, d is in, µ l is cP D Ay = 6 6.657 DAy = [ Tr (6.51) (6.52) °- 2 5 r (31) (6.50) 1-5 0.33 (6.53) 22 r(o D is cm, r is cm, co is sec', p i is g/cm 3 The use of equations relating break-up of ligaments automatically involves the limitations of the ideal system it described. Therefore for a vaneless disc, droplets produced can be approximated to the diameter of the ligament. A relation for obtaining droplet size in this manner is given in equation (6.51). The elongation of the ligament as it moves away from the disc edge will produce smaller droplet sizes than obtained from direct droplet formation. On continued increase of feed rate, a point is reached when the ligament cannot handle the volume flow and a sheet of lig aid forms around the disc edge. Atomization is governed by the mechanism of sheet disintegration ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING (velocity spraying). The transition between ligament and sheet conditions, as expressed by Hinze and Milborn (48) follows the relation [ pig ] [ p1co 2d31 0.6 [ 1,1 2 0.167 --- constant (6.55) crd 3 p l ed a For values of the constant exceeding 1.77 (fpm units) sheet formation around the disc edge prevails. The droplet size resulting from the disintegration of the sheet can again be related to the sheet thickness at the point of break-up although the nature of the liquid break-up by air forces results in greater range of sizes produced. Sprays produced from sheet disintegration are generally less homogeneous than from ligament or direct break-up mechanisms. For sheet disintegration the average droplet size can be calculated from equations (6.52) and (6.53). EXAMPLE 6.8 Calculate the average droplet size obtained from the atomizer operating as in example 6.7. At 15 000 rev/min the atomization mechanism will be by disintegration of liquid sheets at the disc edge. Method I: Use of equation (6.52), Data d = 5 in M = 600 lb/hr = 1 g/cm 3 a = 74 dynes/cm = 1 cP N = 15 000 rev/min substituting values in equation (6.52) DAv 1.0[(1.0) 0.25 1.06 x 600 (74 x 600) 0.66 + 1.91 x 10 -6 (75 000)9" 1.06 x 600 (13 350) ° ' = 55 micron (d) Performance of Vaneless Discs The performance of vaneless discs follows similar trends described previously for atomizer wheels. Effect of Feed Rate on Droplet Size. Mean droplet size is proportional to feed rate. The exponent has been shown to vary according to the atomization mechanism involved, but no clear conclusions have been drawn. Results by Waltman and Blyth (40), Friedman and co-workers (20), and Herring and 155 Marshall (37) have reported exponent values to vary between 0.1 and 0.4 for low viscous feeds (1-15 cP) feed rates 5-60 lb/min and disc peripheral speeds between 150-210 ft/sec (46-64 m/sec). Meyer (41) operated inverted bowls at higher peripheral speeds (460 ft/sec) and reported that increase in viscosity from 330-6800 cP increased the exponent from 0.2 to 0.4 at feed rates under 16 lb/min of a thixiotropic slurry. Mean droplet size is generally accepted as being proportional to the 0.2 power of feed rate at constant disc speed, for commercial conditions where low viscous Newtonian feeds are involved. This is shown in figure 6.29 as the variation of Sauter mean droplet size with feed rate of an aqueous solution. E tij 10000 RPM 200 N 12000 RPM U) 15000 RPM 23000 RPM SAUTER MEAN 154 10 1.0 0.1 5.0 FEED RATE (got /min ) 12 cm DISC. SINGLE TIER. Figure 6.29. Effect of feed rate on mean droplet size from disc atomizer (plate type). Effect of Disc Speed on Droplet Size. Mean droplet size is generally accepted as being inversely proportional to the 0.6 power of disc speed under commercial operating conditions. This is illustrated in figure 6.30 by the Sauter mean droplet size variation with disc speed of spray produced by a 10 cm two-tier plate disc. Effect of Peripheral Speed on Droplet Size. Mean droplet size is inversely proportional to disc peripheral speed. The exponent has been shown to vary according to the atomization mechanism. At low feed rates of low • 156 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 2 TIER . 10 cm die DISC S. 0 of FEED = 164 157 5.0 = 1.5 15,000 RPM FEED RATE . 2 litres/ rni n DISC DIAMETER .120 mrn. 500 959 5 99 r A i Y SAL1TER MEAN 1.0 Kg /m in SLOPE — 066 z 90 ;T- 80 10 Kg/min 4 , 5 Kg/min 'I TIER 6 95 • rt 70 I- 50 50 (..D 40 1— 30 1g 20 CL 10 20 2,000 S,000 10,000 w 5 • L.) 1 20.000 DISC SPEED .(RPM) Figure 6.30. Effect of atomizer disc speed on mean droplet size. viscous feeds, direct droplet or ligament disintegration mechanisms apply and exponent values between — 0.6 and — 0.8 have been reported by Waltman and Blyth (40), Friedman and co-workers (20), and Herring and Marshall (37). With creation of a sheet disintegration mechanism (velocity spraying) by operating with high viscosity feeds (6800 cP) Meyer (41) reported an increase in exponent to — 2.1, for a feed rate 10 lb/min (4.5 kg/min) and peripheral speed 420 ft/sec (130 m/sec). Reduction of peripheral speed below 330 ft/sec saw a substantial reduction in exponent down to — 0.7. An exponent of — 0.8 is generally accepted as the working value in commercial operating conditions. Droplet Size Distributions. Droplet size distributions of plate and inverted bowl-type discs have been reported by Herring and Marshall (37) to follow equation (6.30). The wetted periphery for plate discs equals nd per tier, and replaces the vane wetted periphery in equation (6.30). The increase in the number of tiers per disc will decrease the mean droplet size of the spray provided liquid distribution to each tier is equal. Data from the spray drying of sodium orthophosphate solution show the effect of the number of tiers, as represented in figure 6.31. For a given operating condition sprays formed from a plate-type disc are coarser than sprays formed from vaned wheels. This difference in coarseness is not so striking at plate speeds over 12 000 rev/min and feed I 20 I 50 DROPLET SIZE ID) 100 200 micron ) Figure 6.31. Effect of number of plate tiers of a disc atomizer on particle size distribution. rates giving low disc loadings. Under these circumstances, spray homogeneity compares favourably with that of sprays from vaned wheels. It is at low speeds of rotation that atomization by plate-type discs produce coarse sprays having greater homogeneity than that obtained from low speed vaned wheels. Atomization appears more controllable at low speeds when using vaneless discs. It is this characteristic that gives plate discs their main area of application, the production of coarse powders without presence of fines. This is illustrated in figure 6.32, where droplet size distributions for the atomization of sodium orthophosphate solution at low speeds are plotted for a plate disc and vaned wheel respectively. (e) Application of Vaneless Discs. Vaneless discs of the bowl- and plate-type are often applied when coarse particle size powders are required at high production rates. The multiple tiers of plates enable their use in high capacity dryers. Atomizers of the cup type are at present used under conditions of much lower liquid feed rates. Applications include detergents, ceramics and clays, although the platetype design does not lend itself too well to abrasive materials. 158 ATOMIZATION 159 THE PROCESS STAGES OF SPRAY DRYING ATOMIZER SPEED 6000 RPM ATOMIZER SPEED10,000 RPM DIAMETERS 120MM -- DIAMETERS 120 MM A _ \ . 6 SU - 3 TIER PLATE DISC _ 3 TER PLATE DISC 6 6 8 . . 24VANED WHEEL - a 24 VANED WHEEL 3 . i . DROPLET . , I f t 50 100 200 SIZE ID) {MICRON . 1 400 I I 50 100 200 300 DROPLET SIZE I D1 I MICRON I Figure 6.32. Size distributions from atomizer wheels and discs. Vaneless discs fill the role of an atomizer for specialized applications. Although overshadowed by vaned wheels and nozzle atomizers they are used to advantage when coarse but fairly homogeneous sprays are required at low feed rates, and/or when a low speed rotary atomizer drive is available. Patents covering vaneless discs include (392), a heated disc (400) and a rotary cup (401). 6.6. Nozzle Atomization 6.6.1. Introduction The function of the nozzle atomizer is the acceleration and disintegration of bulk liquid flow, terminating with the dispersion of the resulting droplets to form a spray. A single orifice or ejector cannot be considered an atomizer. The liquid is disintegrated if the liquid jets are turbulent enough, but the droplets are not dispersed by the action of the nozzle. Energy transfer during nozzle atomization is very inefficient (18) (30). Arising out of attempts to improve (a) the degree of atomization, (b) nozzle flexibility and (c) spray trajectory, various nozzle types have been developed. Three types will be covered, namely, those utilizing either pressure, kinetic or sonic energy for liquid bulk break-up. The centrifugal pressure nozzle, which is based upon pressure energy utilization is the most common of the three types. Spray size distribution characteristics, energy transfer, the spray ' pattern and design simplicity have established such nozzles in many and varied spray dryer applications. The centrifugal nozzle is discussed in section 6.6.2. Nozzles based on kinetic and sonic energy are discussed in sections 6.6.3 and 6.7.3. Atomizers that incorporate both the principles of kinetic nozzles and rotating cups are mentioned in section 6.6.4. 6.6.2. Centrifugal Pressure Nozzle (a) Theoretical Principles The principle of the pressure nozzle is the conversion of pressure energy within the liquid bulk into kinetic energy of thin moving liquid sheets. The sheets break-up under the influence of the physical liquid properties and by the frictional effects with the medium into which the liquid sheet is discharged. Invariably the medium is air. Liquid sheets range in thickness from 0.5 to 4 micron. Sheet instability is rapid as any influence that causes fluctuations in the order of this thickness promotes sheet disintegration. Pressure energy conversion to kinetic energy* in a centrifugal pressure nozzle is carried out in such a way that the resulting liquid motion is rotary. This arrangement enables greater energy transfer leading to improved atomization. The principle parts of a centrifugal pressure nozzle are shown in figure 6.33(a). External views of typical nozzles are shown in figure 6.33(b). The mechanism of sheet formation follows the principles described earlier in section 6.2. Pressure applied to the liquid within the nozzle forces the liquid out of the orifice. Rotation imparted to the liquid upstream of the orifice develops a conical spray as liquid passes out from the orifice. The sheet velocity is constant, and the thickness of the sheet diminishes as the cone develops. There is a maximum sheet length for a given pressure. Increase in pressure reduces the sheet length. Increase in viscosity acts to lengthen the sheet, whereas the increase in surface tension has the opposite effect. Increase in sheet velocity and increased turbulence caused by frictional effects with the discharge medium act to reduce sheet length. Reduced frictional effects from spraying into a medium at sub-atmospheric pressure result in elongation of sheet length. Sheet lengths can hardly be seen visually in commercially sized nozzles operating in spray dryers. High nozzle velocities and the resulting turbulence on atomizing liquids of low viscosity provide very short lengths. High viscous liquids, subjected to high pressures which maintain high nozzle velocities again prevent development of the sheet length to any degree. * Less than 0.5% of applied energy is utilized in liquid break-up (18). Virtually the whole amount is imparted to the liquid at kinetic energy. The horsepower requirement for pressure nozzles can be expressed (30). f ti = 7QAP x 10' HP where AP is p.s.i. Q is imp gal/min, 160 THE PROCESS STAGES OF SPRAY DRYING NOZZLE BODY ATOMIZATION NOZZLE HEAD 161 LIQUID FLOW LIQUID FLOW LIQUID FLOW ORIFICE SLOTTED SWIRL INSERT (a) CI NCLI NED SLOTTED INSERT A. B. r SPIRAL GROOVE INSERT swIRLt61 INSERT Figure 6.34. Inserts for generating liquid rotation within centrifugal pressure nozzles. Three types of inserts are shown in figure 6.34. Centrifugal pressure nozzles that incorporate tangential feed entry or use inserts are shown in figure 6.35. The theory of centrifugal pressure nozzles is discussed in detail by Marshall (35) and Green (482). A complete mathematical treatment is presented. ORIFICE (b) (i) (b)(ii) Figure 6.33. Centrifugal pressure nozzles. (a) Principle parts. (b) Typical nozzles ; (i) Delavan type (sdl) spray drying nozzle, (ii) Delavan type (sdx) spray drying nozzle. The internal design of the centrifugal pressure nozzle is critical in forming the liquid into thin conical sheets, capable of breaking up with a minimum of external disturbance. Methods of imparting rotary motion within the nozzle include use of spiral grooved inserts, inclined slotted inserts, swirl inserts, or simple use of tangential flow entry. The slotted inserts feature multiple feed inlets into the orifice, but each slot is of small cross-sectional area, and prone to clogging. An effective feed strainer must be incorporated in the feed line or nozzle body, and be regularly cleaned. The swirl insert has a single feed inlet. Like the nozzle with tangential feed entry, a natural free vortex flow is produced with a minimum of friction. The swirl channels have comparatively large flow passages, and enable such nozzles to handle high solids feed without undue wear or clogging. Highly abrasive or corrosive feed, however, wear the nozzle whatever swirl mechanism is adopted, although wear rates are minimized by use of special materials (e.g. carbides). (Patented nozzle designs are given in references (442) to (450).) SWIRL CHAMBER FLOW CHANNEL TANGENTIAL TO SWIRL CHAMBER C. b. E © 1 2 111E1 c. 1 © 3 4 EU ( 1 2 3 0 L, a 6 5 1 7 8 0 6 7 a Figure 6.35. Centrifugal pressure nozzle construction. (a) Centrifugal pressure nozzle with tangential liquid entry (62). (b) Centrifugal pressure nozzle with swirl inserts (61). (c) Centrifugal pressure nozzle with inclined slotted inserts ; 1. nozzle, 2. washer, 3. orifice, 4. swirl insert, 4a. inclined slotted insert, 5. end plate of distributor, 6. liquid distributor, 7. washer, 8. nozzle body (61). 162 ATOMIZATION 163 THE PROCESS STAGES OF SPRAY DRYING (b) Spray Patterns Sprays formed by the designs shown in figure 6.35 have hollow cone patterns symmetrical with respect to the nozzle axis. The pattern has a clearly defined spray angle on discharge from the orifice but the angle decreases and becomes less well defined away from the orifice due to effects of the ambient air conditions in relation to the momentum of each droplet. The spray angle is shown diagrammatically in figure 6.36. The hollow cone spray has an air core at the centre of the orifice. The air core is formed as a result of liquid rotation within the nozzle. Greater liquid rotation creates a wider spray angle, and larger air core. Increase in spray angle signifies decrease in nozzle capacity as shown in figure 6.36(d), by a plot of spray angle versus nozzle discharge coefficient. II A SPRAY ANGLE I DROPLET POPULATION PROFILES TH EORETICAL SPRAY COVERAGE AT RATED SPRAY ANGLE. 160 SOLID CONE SPRAY 160 HOLLOW CONE SPRAY a. P2 it 120 2 100 SO 2 A2 < P I SO Al 20 02 0.6 0.4 00 DISCHARGE COEFFICIENT C D } c. d Figure 6.36. Spray angle characteristics. (a) Droplet population in solid cone and hollow cone sprays. (b) Nozzle spray angle. (c) Effect of pressure on spray angle. (d) The relation between discharge coefficient and spray angle for a typical hollow-cone centrifugal pressure nozzle used in spray drying. Hollow cone spray patterns can be transformed into solid cone spray patterns by balancing the rotational motion with an axial liquid velocity component. In solid cone sprays, droplets are distributed fairly uniformly throughout the conical pattern although spray droplet population is highest in the centre. Hollow and solid cone patterns are shown in figure 6.36(a) with their spray droplet population. For equal feed rates and feed pressure, droplet size distribution is more homogeneous in the hollow cone than solid cone. The solid cone contains a higher proportion of larger droplets, and these droplets are concentrated at the centre of the pattern. Successive wear in the nozzle orifice can produce undesirable spray characteristics by creating non-symmetrical sprays. Spray pattern symmetry, its importance in spray drying and its measurement is discussed by Tate (50). Flat patterns from fan spray nozzles have not as yet been seriously applied in spray drying, although much data have been acquired on fan nozzle performance (30) (480). Flat patterns could be used to advantage in small drying towers. The nature of the pattern with droplet travel in one plane prevents interference between sprays in closely bunched nozzle assemblies and prevents product deposits at the dryer walls due to a minimum of radial droplet travel. Nozzles having either hollow or solid cone spray patterns are used in co-current, counter-current and mixed flow drying chambers. The hollow cone nozzle; however, is especially suited for co-current systems as the majority of droplets making up the spray lie on the extremity of the cone and are readily contacted with drying air to initiate rapid evaporation. Where solid cone sprays are used in co-current systems the spray droplets present in the centre of the cone are surrounded by high humidity atmosphere for longer time periods. This is due to the extended time for the spray dispersion to expose the central droplets to the hot drying air. Solid cone sprays are readily applicable to counter-current flow systems. The drying air meets the full face of the cone pattern. Contact between spray droplets at the centre of the pattern is as good as at the extremity. Furthermore the larger droplets of the spray distribution present in the centre of the cone pattern are moving in a prominently axial direction and thus show less tendency to disperse outwards for early impact in a semi-wet state on the dryer walls. The droplets making up the extremity of the spray cone are of smaller size, and although they possess a radial velocity component on leaving the nozzle orifice, their size and contact with drying air enables completion of droplet surface drying before arrival at the dryer wall. Where hollow cone sprays are used in counter-current flow dryers, greater degree of wall deposits may occur, especially in small chamber volumes. Control of wall deposits makes adjustment to the air disperser critical. The spray from a hollow cone spray nozzle may possess a more uniform size distribution, 164 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING but with the droplets directed from the nozzle with a radial velocity component, and the high droplet population at the extremity of the pattern, longer drying times can result for complete drying of the spray and this leads to wall deposit conditions. In mixed flow dryers, hollow cone sprays are best applied when the first phase of the droplet-air flow is co-current, i.e. as in a layout shown in figure 5.9(a). Where droplet-air flow is first counter-current (see figure 5.9(b)) use of a solid cone spray can lead to chamber operation with reduced deposit formation. Solid cones enable droplets to remain in the centre of the drying chamber until their highest trajectory is reached, and thus cause the droplets to remain airborne for longer time periods during the second phase of co-current flow. Increasing the airborne time of droplets just fractions of a second can have significant effect on the degree of completion of moisture removal from the droplets and the minimizing of deposit formation at the dryer walls. The desirability of either hollow or solid cone sprays in particular types of dryer exemplifies the role of spray aerodynamic properties in the formation of the spray pattern as observed during dryer operation. Aerodynamic spray properties, namely velocity of entrained air, droplet velocity and spray force provide information for optimising spray dryers featuring nozzle atomization. These spray properties govern (a) droplet population within the drying chamber, (b) the extent of hot air-droplet mixing near the nozzle, and (e) the rate of droplet penetration through the drying air towards the chamber walls or base. Knowledge is far from complete as to how momentum is distributed within a spray pattern, between spray droplets and entrained air, or as to whether the variation in droplet population within the spray pattern is predictable at various distances from the orifice. The established aerodynamic laws of droplet motion cannot be directly applied to the spray system as there is considerable flow interference between droplets, and the shape of droplets can be distorted during flight. Air entrainment at a given distance from the orifice tends to be independent of the spray pattern, being governed principally by the laws of turbulent transfer in air jets. For sprays of fine droplets, the majority of movement in the spray at the nozzle orifice is converted into the momentum of the entrained air stream within relatively short distances from the nozzle (i.e. within approximately 3 ft (1 m)). The total flow of air associated with the spray increases as the spray broadens on moving away from the orifice in the pattern defined by the spray angle. This increasing entrainment of air into the spray assists rapid spray evaporation by creating intimate spray-air contact. The degree of entrainment, however, does not depend upon the spray angle entirely, as the droplet population throughout the spray pattern appears a factor of 165 great influence. Hence the air entrainment occurrence differs for solid and hollow cone spray patterns of the same spray angle. For a solid cone spray, air might not penetrate the centre of the spray pattern until droplets have travelled quite some distance from the nozzle. For hollow cone sprays air penetration is much more rapid and spray-air mixing more effective. It is desirable to know the influence of entrained air on droplet motion from nozzles as relative velocity between droplets and the air is a prime factor in moisture evaporation rates from the spray. There appears some relation between feed rate, operating feed pressure, cone angle and spray pattern, but no generalized form is available at present. The spray ejection velocity from the nozzle followed by air entrainment maintains droplet velocities considerably higher than droplet terminal velocities over time periods where the majority of moisture evaporation takes place. There are inevitable errors caused by basing heat and mass transfer rates in nozzle dryers on mean drying air velocity or droplet terminal velocities. However, any error acts to give conservative evaporation times, but air entrainment effects promote faster droplet trajectories to the wall, and trajectory time may prove too rapid for completion of evaporation, with resulting wall deposits. Air entrainment into sprays (480) has been recently reported (1969) by Benatt and Eisenklam (51). A model for entrainment was developed and confirmed using centrifugal pressure nozzles on aqueous feed. A dimensionless entrainment parameter was introduced. The model enabled entrainment rates (mass flows of entrained air) to be predicted. (c) Fluid Flow from Centrifugal Pressure Nozzles The flow of liquid from the orifice of a centrifugal pressure nozzle can be illustrated by velocity vectors as shown in figure 6.37. At the outlet (c), liquid at a given point on the orifice wall will have a component of forward velocity (u„) and one of tangential velocity (u h ) imparted by the liquid rotation produced by the tangential liquid entry. From basic geometry, the liquid leaving this point will travel in a straight line at an angle (tan -1 u h /u„,) to the nozzle axis. The orifice does not run full, the air core within the orifice ranging from 0.4 to 0.8 of the orifice diameter. Applying the continuity equation to liquid flow through the nozzle configuration shown in figure 6.37 results in equation (6.56). For two inlets : 2(gri nie1 } = 2gr 2 bu y (6.56) where : b = liquid film thickness at orifice, r = inlet feed channel radius, r 2 = orifice radius 166 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING 167 where n = 0.5 for turbulent flow, C v = velocity coefficient, h = pressure head, P = total pressure drop. Feed flow through the nozzle, stated in terms of a discharge coefficient (C D ) can be deduced from equation (6.60). The discharge coefficient represents the ratio of the actual liquid discharge rate to that theoretically possible under ideal conditions of energy transfer. The discharge coefficient is related to the velocity coefficient by an area coefficient CA where CD = Cl/CA . For centrifugal pressure nozzles, the presence of the air core reduces the area of liquid flow through the orifice and CA tends to CD . The velocity coefficient approaches unity values accordingly. Thus : LIQUID FILM THICKNESS I N ORIFICE Volumetric flow rate (Q) = feed velocity x flow cross-sectional area. (6.61) Q = Vres C A A where A = orifice area. Combining equations (6.60) and (6.61) for turbulent flow: 1/2 Q = cv (2gh) 112 C A A = C v (2g— Figure 6.37. Velocity diagram for liquid flow from a centrifugal pressure nozzle; r 1 = inlet channel radius, r 2 = orifice radius, R2 = swirl radius, b = liquid film thickness at orifice. The feed channel length is assumed long enough to create tangential and not diffuse flow into the nozzle. The velocity of the liquid entering the nozzle (V irile ,) is given by MI - (6.57) KM et 27tr2ipi = where M, = mass liquid flow rate. Thus follows from equation (6.56) 14,, 7' (6.58) rzu From the geometry of the spray, the resultant velocity of the liquid sheet leaving the nozzle (Vres ) is given by : Vinlet Vres = [4 + Ufl 112 n (6.62) P) 1 / 2 Q = CD A(2gh) 112 = CD A(2g— (6.63) Alternatively, the mass flow rate (M L } = Qp and equation (6.63) can be rewritten (6.64) ML = CDA-( 2gPa12 The discharge coefficient depends upon the size of the orifice, and varies with the dimensions of each nozzle design. It follows from equation (6.64) that a plot of flow rate against the square root of the total pressure drop results in a straight line, the gradient being a measure of C D A(2gp) 112 (6.59) For cases of very low friction losses in the nozzle, the tangential velocity component for liquid leaving the nozzle can be calculated by applying the law of conservation of angular momentum to the nozzle flow, Referring to figure 6.37 uh r 2 (6.65) VinIetR = (6.60) where R = mean swirl radius of feed inlet to swirl chamber. Expressed in terms of pressure drop across the nozzle : P Vres ies = Cv (2ghr = C,(2g— ) now CD = CVCA CAA 168 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION Example 6.9 illustrates the basic calculations for determining flow characteristics from centrifugal pressure nozzles. EXAMPLE 6.9 The variation of liquid feed rate with pressure for a centrifugal pressure nozzle of design shown in figure 6.37 is given in the table below. Calculate the flow properties of the nozzle when operating at 60 psig with a liquid of density 70 lb/ft 3 . tan 24° = C 0 A(2gp) 112 Feed pressure P (psig) P 112 115 140 160 185 20.25 30.25 42.25 56.25 4.5 5.5 6.5 7.5 Feed rate Feed pressure P (psig) M (lb/hr) p112 8.5 9.5 . 10.5 72.25 90.25 110.25 205 230 250 Data : 25 0.5 x 12 x 3600 tan 24 f.p.s. wilts 1. Calculation of Discharge Coefficient (C D ) Substituting data in equation (A) C D --- 25 tan 24 1 0.5 x 12 x 3600 X A(2gp) 1 / 2 - 25 x 0.4452 4 0.5 x 12 x 3600 x n(0.070) 2 144 (64.4 x 70) 1 / 2 = 0.34 Measured cone angle at 60 psig = 80° 2. Calculation of Inlet Velocity to Nozzle At operating pressure of 60 psig : P' 12 --- 7.746. Mass feed rate (from graph) M = 188 lb/hr. Inlet velocity to nozzle (equation (6.57)) Nozzle dimensions : feed channel diameter to swirl chamber = 2 off: 0.052 in orifice diameter = 0.070 in internal diameter of swirl chamber = 0.302 in The feed rate vs pressure data is plotted in figure 6.38. The gradient approxi- 1 188 44 1 = 25.3 ft /sec = 3600 H 2(n/4)(0.052)2 x 70 = 3. Calculation of Resultant Velocity of Liquid Sheet Leaving Nozzle Using equation (6.59) where C v is taken as 1. 300 (17. es ) [64.4 x 60 x 1441 1 / 2 = 89.2 ft/sec 70 250 4. Calculation of Forward Velocity (U,) from Nozzle For a cone angle of 80° = 20 where from figure 6.37 _c° 200 k 150 LI, Li w U- (A) The conversion factor to express the gradient in f.p.s units (for the abscissa and ordinate scales of figure 6.38) ( Feed rate M (113/hr) 169 mates to tan 0 = - U, 100 U] (B) tan 40 = 0.8391 50 0-8391U, Uh = 0 2 3 4 5 6 7 . ps ig 2 1 2 (FEED PRESSURE) I 9 10 1 . ' Figure 6.38. Variation of feed rate with square root of nozzle pressure (example 6.9), Now resultant velocity (Fres ) = ( Uv2 + UD I / 2 and by combining equations (6.59) and (B) Vr „ therefore U, = 65.8 ft/sec 89.2 = (LT, + 0-83911/,2)" 2 170 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING L 5. Calculation of Film Thickness From equation (6.58) where 1 h = .2 171 v 'Tile, r, U, r 1 = 0.026 in r 2 = 0.035 in b= (0.026 2 ) 25.3 x = 0.0074 in 0.035 65.8 5 20 30 P2 PRESSURE RATIO (7 , ) 6. Calculation of the Percentage Conservation of Angular Momentum From equation (6.65), where R = (0.302 — 0.052) 0.125 Uhr2 //inlet)? 0.8391 x 65.8 25.3 0.035 12 a. 12 X 100 = 61 % 0.125 (d) Nozzle Operating Characteristics (i) Relation between Flow Rate, Pressure and Density. Performance of the nozzle is effected by pressure, liquid density and viscosity. The flow rate is directly proportional to the square root of pressure, and varies inversely with the square root of liquid density. This relation is only approximate. Q 1/2 Q2 (P2 (Pi) 112 Q1 \PI I 1P 2i (6.66) The relation between the ratio of two operating flow rates and the two corresponding operating pressures is shown in figure 6.39(a). The relation between the ratio of two operating flow rates and the two corresponding liquid densities is shown in figure 6.39(b). Any change in liquid density is usually associated with changes in other liquid properties, and thus the above relation does not apply in all cases. The effect of viscosity on flow rate cannot be clearly defined being dependent upon the specific nozzle design and operating conditions involved. Increase in viscosity can increase flow rates especially in conical spray nozzles, although the reverse trend can be observed in other designs. The exact effect must be determined by experiment for a given nozzle design and operating conditions. (ii) Spray Angle. A minimum pressure is required to develop any form of spray angle. The minimum is approximately 20 psig (1.4 atm). Increase of pressure decreases the spray angle, but influence is slight, especially if measured near the nozzle orifice. At higher working pressures above 200 psig (14 atm) the spray angle becomes reduced due to air entrainment 04 1.0 100 FEED DENSITY RATIO b. Figure 6.39, Feed rate, feed pressure, feed density ratios for centrifugal pressure nozzles, effects. Viscosity has a significant effect where an increase produces a narrower spray angle. At very high viscosities the spray angle is so reduced that a plug stream of liquid results, and atomization ceases. The effect of pressure on spray angle is illustrated in figure 6.36(c). (iii) Effect of Operating Variables on Droplet Size Effect of capacity on droplet size. Larger droplets accompany increase in feed rate for increases occurring within the rated feed rate range of the nozzle. This is illustrated in figure 6.40(a). If initial feed rate is well below the rated flow, atomization is incomplete, as the liquid velocities within the nozzle are inadequate. In this case increase in feed rate will decrease droplet size until the rated capacity of the nozzle is reached. 172 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 173 Spray angle and droplet size. Smaller droplets are formed from sprays of larger spray angle. This is shown in figure 6.36(d). Increase in spray angle decreases nozzle discharge coefficient. Decrease of discharge coefficient decreases feed rate and this for a constant pressure reduces droplet size. Effect of pressure on droplet size. By virtue of greater energy at higher pressures, droplet size will decrease with increase of pressure, although there are varying opinions as to the exact relation involved. For trend NOZZLE INSERT : GROOVED CORE SAUTER MEAN DIAMETER 1M ICRONS) 400 1.5 ato 3 ato 6.5ato 10 do 17.5 ato 200 900 50 10 estimation droplet size can be assumed to vary as the — 0.3 power of pressure within the medium pressure range. At very high pressures, further increase of pressure has virtually no effect on atomization. Inspection of figure 6.40(a) illustrates increase of pressure to reduce mean droplet size at fixed feed rate. Pressure is plotted as a parameter. Effect of feed viscosity on droplet size. Coarse atomization results from increase in feed viscosity. Droplet size can be taken to vary with viscosity to the power 0.17-0.2. The exact relation between spray mean droplet diameter, droplet size distribution and feed viscosity is particular to each nozzle design and dimension. General trends are illustrated in figure 6.40(b) and 6.41 for a 0.79 mm orifice grooved core nozzle. Some increase in capacity can also accompany viscosity increase, further assisting coarser atomization. With viscosity increase the air core of the nozzle becomes increasingly filled with liquid. At a given pressure, capacity will increase until the nozzle operates with no air core. Capacity increases are small, however. Very high viscous materials cannot be atomized by pressure nozzles. 100 AQUEOUS FEED RATE NOZZLE INSERT:GROOVED CORE NOZZLE PRESSURE: 29.5 ato Kg/HOUR NOZZLE INSERT - GROOVED CORE FEED RATE - 0.715 Htros/mi n NOZZLE PRESSURE • 29.5 ato ORIFICE DIAMETER: 0.79mm 99.9 90 99.5 99 CUMULAT)VE VOLUME PERCENTAGE z FEED RATE , 0.715 iitersImin ORIFICE DIAMETER: 0.79 mm 80 w w 70 x 8 95 90 80 70 60 50 40 30 20 10 5 60 0.5 01 s:1 0 (b) 2 3 6 5 6 7 FEED VISCOSITY c.5 Figure 6.40. Effect of variables ((a) feed rate, (b) feed viscosity) on Sauter mean diameter. W5 0 2 4 12 10 6 811 1, '2 (DROPLET SIZE) 2 (MICRONS )1 14 Figure 6.41. Effect of feed viscosity on spray droplet size distribution. 16 174 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 175 Effect of surface tension on droplet size. Energy supplied to the nozzle has to overcome both viscous and surface tension forces. Hence liquids of high surface tension become more difficult to atomize. Surface tension values of feed liquids that are nozzle atomized vary over a relatively small range, and thus effects of surface tension changes on droplet size are much less significant than for changes in viscosity. Effect of orifice size on droplet size. Droplet size increases with the square of orifice diameter, other nozzle parameters being held constant. (iv) Droplet Size Distribution. The available range of droplet sizes obtained with centrifugal pressure nozzles is extensive. Whether wide or narrow distributions are produced depends upon nozzle dimensions, operating pressure and feed conditions. A typical size distribution is given in figure 6.42 to illustrate the range of sizes obtained from a nozzle operating in conditions well representative of a general spray drying application. Droplet size distributions of pressure nozzles are fully described by Marshall (35). Many sprays are represented in linear form when presented as a square root normal distribution (380). (e) Prediction of Nozzle Performance Correlations to predict nozzle performance are available for given nozzle designs. An overall working formula has as yet eluded investigators. Correlations utilize either known operational data or nozzle dimensions. Doumas and Laster (52) and Dombrowski and Hasson (53) have proposed methods to predict performance where only the nozzle dimensions are known. The methods involve use of nozzle parameters established experimentally on nozzles having tangential swirl channel inlets as shown in figure 6.43. Nozzles used by Doumas and Laster featured circular inlet FEED PRESSURE . 300 p.s. 1.g FEED RATE. 350 Lb /hr (VISCOSITY < 5 c.p. ) TANGENTIAL INLET SWIRL CHAMBER. IN CUMULATIVE PERCENT BY VOLUME LESS THAN 999 5 99.9 99.5 99 LIQUID IN 95 90 LIQUID OUT 80 a. 70 60 50 40 30 LIQUID IN 20 10 5 0.5 0-05 0 100 200 LIQUID OUT 300 DROPLET DIAMETER D. (MICRONS ) Figure 6.42. Typical droplet size distribution of a centrifugal pressure nozzle used in spray drying. b. Figure 6.43. Nozzles with tangential feed entry. (a) Nozzle used by Doumas and Laster (52). (b) Nozzle used by Dombrowski and Hasson (53). 176 ATOMIZATION 177 THE PROCESS STAGES OF SPRAY DRYING channels. Nozzles used by Dombrowski and Hasson featured inlet channels of rectangular cross section, so chosen due to the practical difficulties of drilling circular holes that are truly tangential to the swirl chamber. The inlet channel length to diameter—width ratio in both types of nozzle designs permitted full tangential and not diffuse flow into the swirl chamber. 1.00 co • 0-80 c 2 060 0.40L L.Lr • 020- n. 0 C. 2 4 {r 10 8 6 or 12 14 16 16 A' Figure 6.44. Nozzle dimensioning relations after Doumas and Laster (52). (a) Relation between discharge coefficient and nozzle dimensions. (6) Relation between mean spray angle and nozzle dimensions. (c) Relation between the parameter (cc) (equation (6.68)) and nozzle dimensions. Method of Doumas and Laster (52) 0 4 2 6 8 10 12 The feed rate through a swirl nozzle of design shown in figure 6.43(a) is derived from conservation of momentum, Bernoulli and continuity equations. From the feed rate relation (equation (6.63)), the discharge coefficient and spray angle can be expressed in terms of the nozzle dimensions expressed 1 112 as a parameter (Rr 2 lri)(r2 /R ) , where R = swirl chamber radius, r, = radius of inlet feed channel, r 2 = orifice radius, R' = (R 1. 1 ). The discharge coefficient expressed in terms of the nozzle dimensions equals a(1 — C0 112 (6.67) C D = (1 a + a2(x)2)1/2 for values of 2 14 R r r2 ' 1 f t i t 0, rr re r, (6.68) = 1 — —2 A' = r2 R (6.69) rt From equation (6.67), CD and r c are independent of h, the head of liquid at the nozzle. A direct relation between CD and the nozzle dimensions is shown in figure 6.44(a). This enables the direct determination of the discharge 1 11 l coefficient, where CD is plotted against the parameter [A (r 2 /R ) 1. The mean spray angle (0) is calculated from the parameter (figure 6.44(b)). The mean spray angle correlates to 2 4 6 - b. (2 2' 1R 8 10 ( 1 /2 12 14 15 11 r R (r2 \ 1 16 9 = 43.5 log [14( 2 rl R1 (6.70) 178 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 179 The air core diameter (r e ) is calculated from equation (6.68), which rearranges to 12 re = (1 — a)' r2 (6.71) The calculation of re is simplified by obtaining values of a from figure 6.44(c), where A' in equation (6.69) is readily determined from the nozzle dimensions. EXAMPLE 6.10 Nozzle atomization with a centrifugal pressure nozzle (Swirl type) is used to produce 500 lb of powder (moisture content 3.5 %). The feed concentrate is 32 % TS, and specific gravity 1.14. The nozzle orifice is 0.112 in diameter. Spray angle is 60° at 500 psig operating pressure. After 500 hours of operation, atomization deteriorates, and the product becomes off-specification. At the time when the control laboratory can no longer grade the product as acceptable, the nozzle spray angle had increased to 75° under normal feed conditions. Estimate from the above data the possible wear that had taken place within the nozzle orifice. The final diameter of the orifice can be calculated using figure 6.44. Production rate = 500 lbihr = 1505 lb/hr The nozzle discharge coefficient (C D ) can be calculated from the spray angle (0), using figure 6.44(a), (b). For 0 = 75°, figure 6.44(b) 1/2 = 3.8 rl which from figure 6.44(a) Cr, = 0.18, now Q = CD A(2gh) 112 Q A= ( 1505 — 5.88 x 10' cu ft/sec 3600 x 1.14 x 62.3 r 2 ft2 144 h= (500 + 14.7)33.9 = 1040 ft 14.7 x 1.14 r 2 144Q = C (2gh) 112 D r= ( 144 x 5 , 88 x 10' n0.18(64.4 x 1040) 112 ] r = 0.076 in Original diameter of orifice = 0.112 in, area = 0.00985 in 2 Final diameter of orifice = 0.152 in, area =- 0.01814 in' 2 Therefore area increase of orifice due to wear = 0.0083 in . Method of Dombrowski and Hasson (53) The method was developed from investigations into the flow characteristics of swirl nozzles of the design illustrated in figure 6.43(b). The inlet swirl channels are rectangular. The nozzle pressures studied ranged over 50-150 psig (3.5-10 atm) on aqueous feeds. Operating feed conditions cover a flow number range of 1-10 imperial gallons/hr (psig) l " 2 . The flow number relationship is given by Flow number (FN) = ( ( 2 )0.5) x 9. 65 100 Feed rate of concentrate to the nozzle = 500 x 1 0 32 r22R\ I where 1 atm = 33.9 ft of H 2 O (6.63) (6.72) The nozzle parameter is given as (A/(d 2 x d M )) where A = area of inlet swirl channel(s), d M = mean diameter of inlet vortex in swirl chamber, d 2 = orifice diameter. The mean diameter (d M ) is obtained from the swirl chamber diameter (d 3 ) and the swirl channel width (1), where d M = (d 3 /). The nozzle parameter was developed from the Taylor (54) solution of the mechanics of low viscous liquid flow through swirl nozzles. Spray angle and discharge coefficient are directly related to the nozzle parameter, as shown in figure 6.45(a), (b). The deviation from ideal flow conditions can be corrected for in terms of the ratio of orifice length to diameter (L/d 2 ). This correction is shown in figure 6.45(c). The prediction of spray angle and discharge coefficient is straightforward using figure 6.45. The ratio of orifice length to orifice diameter (L/d 2 ) is obtained from the nozzle dimensions, and the correction factor (F 1 ) for the effect of (L/d 2 ) on spray angle is obtained directly from figure 6.45(c). The correction factor F, is combined with the nozzle parameter and the ratio (L/61 2 ) to form a modified parameter Fl A _ W m \ 11212/3 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION The modified nozzle parameter forms the abscissa in figure 6.45(a), (b). The spray angle can be read directly from figure 6.45(a) using a known value of the modified nozzle parameter. For prediction of the discharge coefficient, a correction factor F2 is used to modify the apparent discharge coefficient, applicable to the case of theoretical frictional flow. Firstly the modified nozzle parameter, as stated above, is used to read off the apparent discharge coefficient from figure 50 - 150 pAr.g 0.5 18 p 04 15 z 1•4 uf- 181 NO1133k:1800 180 r.) rr cr 02 1.2 0.1 0-1 AQUEOUS FEED 10 10 0.5 100 7-) ORIFICE LENGTH ORIFICE DIAMETER 80 G, Lu ELI Figure 6.45. Nozzle dimensioning relations after Dombrowski and Hasson (53). (a) Variation of spray angle with modified nozzle parameter. (b) Variation of apparent discharge coefficient with nozzle parameter. (c) Correction factors F 1 F2 for the effect of orifice length and diameter on spray angle and discharge coefficient. 60 w 40 2 ?<- 20 a. Lt) 0 0.4 0•8 12 16 2-0 2.4 26 32 6.45(b). The actual discharge coefficient is finally calculated using the correction factor (F2 ) where 2 (-zia2 j MODIFIED NOZZLE PARAMETER , )' F2(CD(apparent) — 0-05 CD(actual) I (6.73) The value of (F2 ) is obtained from figure 6.45(c). EXAMPLE 6,11 A swirl nozzle with two tangential, rectangular inlet channels is operating at 7 atm at rated flow. The dimensions of the nozzle are as follows : as 0q APPARENT DISCHARGE COEFNCIENT Orifice diameter (d 2 ) = 3 mm Orifice length (1) = 1.5 mm Mean swirl diameter (d m ) = 18 mrn Swirl chamber diameter = 22 mm Inlet channels — 4 x 4 mm Predict the spray angle and discharge coefficient. The nozzle type and dimensions suggest the Dombrowski and Hasson method applicable : 1. Nozzle Parameter 1 A\ d 2 c/ 1„/ ) 0 0.4 06 1.2 1.6 A 2.0 2.4 1 2.8 ! 12 d MODIFIED NOZZLE PARAMETER 7 F _bl_) '2 '3 i i d2 .d m k d 2 i r i 3.2 = 32 56 4 7 0-57 2. Ratio i dm 112 b. 2x4x4 3 x 18 ke12) = ( 18y/2 -3- = 6 112 = 2.4495 182 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 183 2 3, Ratio : orifice length to diameter The flow number is the ratio of (Q/P" ) but can be obtained directly from the relation 1 (—1 ) = P = 0.5 d2 FN = 293C D A 3 4. Modified nozzle parameter : \ 'd m \ 1/212/3 Ft = 0.39(0.57 x 2.4495) 213 = 0.487 A [(d d m ) From figure 6.45(a) spray angle = 75' 5, Now for a modified nozzle parameter of 0.487, the apparent discharge coefficient (from figure 6.45(b)) CD(a = 0.35. From figure 6.45(c): pparent) Correction factor (F 2 ) = 1.6 as — = 0.5 d2 Hence : Actual discharge coefficient C D(ac ,„„, ) is calculated from equation (6.73) C D(actual) = (1.6 x 0.35 — 0.05) = 0.51 (f) Prediction of Mean Droplet Size of Sprays from Centrifugal Pressure Nozzles The factors governing the mean droplet size of sprays for a given set of operating variables are very complex. An empirical approach is the only way to establish relationships. Relationships between mean droplet size and operating variables have been established through spray analysis at various values of the nozzle design variables; orifice- diameter, ratio of orifice length—diameter, liquid pressure, and discharge medium pressure. Many of the correlations proposed apply specifically to one design of nozzle and atomizing liquid, but empirical correlations are available for use in first design and performance calculations. These are given in table 6.14 in four sections. The first three sections quote correlations found applicable to nozzles having specific swirl chamber designs. The fourth section includes empirical correlations of centrifugal pressure nozzles in general. Nozzles with grooved inserts where liquid rotation is created by flow through angled grooves or slots are covered by relations quoted by three different investigators. Equation (6.74) proposed by Frazer, Eisenklam and Dombrowski (55) expressed the Sauter mean diameter in terms of a flow number (FN) governing volume flow rate (Q) and nozzle pressure (P). (6.83) when the orifice area (A) is in cm 2 . Equation (6.75) by Moulton and Turner (56) resulted from fitting extensive data into the correlation between Sauter mean droplet size and orifice diameter, flow rate, surface tension and viscosity. Droplet mean size is shown to be proportional to the 1.5 power of orifice diameter and inversely proportional to the 0 , 44 power of flow rate. This correlation is unique in attaching such importance to surface tension with a power relation up to 0-6. It is interesting to note that viscosity shows little prominence. This is rather misleading, although over the viscosity range investigated (less than 3 cP) influence would be slight. Equation (6.76) by Nelson and Stevens (8) expressed the volume mean diameter in terms of the fluid flow characteristics from the nozzle as defined by the Reynolds and Weber numbers. The volume mean diameter exceeds the Sauter mean diameter by approximately 15-20 %. The factor (Y) in equation (6.76) is dimensionless and consistency of units must be adhered to when calculating the Z-value. Nozzles with swirl plates to create liquid rotation were also studied by Frazer, Eisenklam and Dombrowski (55). Two equations (6.77) and (6.78) are quoted. A wide range of liquid variables are covered. Nozzles with simple tangential entry were studied by Moulton and Turner (56). Equation (6.79) results from treatment similar to that given by equation (6.75). The power values in both equations were found to be of the same order. The average geometric standard deviation (S G ) for the Moulton and Turner nozzles was correlated in terms of orifice diameter (mm) where SG = 0.173 + 0.126 log ic+ do (6.84) The similarity between the equations (6.75) and (6.79) gives greater confidence when discussing the suitability of general correlations. Such correlations (equations (6.80-6.83)) show the Sauter mean diameter in terms of operating variables. Equation (6.81) by Tate and Marshall (57) interpreted nozzle performance in terms of the axial velocity (U,) and the tangential velocity ( U T ) components on liquid discharge. The average axial velocity is given by the ratio of the volumetric flow rate to area of liquid flow through the nozzle orifice, i.e. u= v n(rgr2) rc (6.85) where Q = volumetric feed rate, ro = orifice radius, rc = air core radius. (i) Grooved Equation log io D vs = 1.808 + 6-94 Range + 0.138(FN) AP D vs = 16.56(4 -52 )(6 °-713 )(yr 55 )(Q logio D vm = Y do and (ii) Swirl plate 0-444) where Y = -0-144Z 2 + 0.702Z - 1.26 we ) 0.2( v) 12] Z = log io (Re) --G Re Dvs = 335(FN)• °9 v ° " 25 A p0.348 RFTSD 1 L AP 3- D vs = 119.2 1-589)(61)-594)(4-22o)(2-0.537) (iii) Tangential entry Dvs 41-4(c1Q = (iv) General D vs - 0-5 157 --o ( r;) 0-45 597(0) D vs = 286(d o + 0.17) exp 76704 .33 D MMD (u, -11(u .00-4.0 (d o is in, U v , UT is ft/sec) 13 Q 100 > AP > 25 psi 2.0 > FN > 0-05 0 = 60° (6.74) (55) o- = 26-37 dynes/cm p = 1.024 - 1.073 g/cm 3 - 0.9-2-03 cP Q 1-30 US gal/sec do = 0-7-1.5 nun (6.75) (56) P 1000 psi Q = 4.0-70 gal/hr 0 = 52-91° (6.76) (8) p = 0.746 Wan' AP = 12-300 psi FN 0.5-2-0 v = 2.0-18-5 cs = 22 dynes/cm (6.77) (55) AP < 100 psi FN = 10-500 B- 85° (6.78) (55) (6.79) (56) (6.80) (7 ) (6.81) (57) (6.82) (58) (59) do = 1-4-2.03 mm o- = 26-37 dynes/cm Q = 1-30 US gal/sec = 0.9-2-03 cP p i = 1.024-1.073 g/cm 3 1-5 (ici do [P 1 pr . 0.0094U-1-1 Equation number Reference UT = 7-50 ft/sec U v = 40-150 ft/sec NOI1VZIWOIN Nozzle swirl chamber design DNIANCE AVIldS .40 SIDVIS SSff3O2id UHI 00 Table 6.14. Correlations to Predict Mean Droplet Size from Centrifugal Pressure Nozzles 186 THE PROCESS STAGES OF SPRAY DRYING For swirl chambers U T = 42 .4 —5w where A s , = area of flow into swirl chamber. For grooves UT = 187 ATOMIZATION For values of U, in ft/sec, equation (6.85) can be rewritten as (0.407Q/4) where orifice diameter (d o ) is in and feed rate (Q) is US gal/min. The air core can be calculated from equations (6.68) and (6.69) and figure 6.44(a). As a guide, for orifice sizes above 0.05 in diameter, air core diameters are 0.7-0.8 orifice diameter. Below 0.05 in the air core decreases to 0.4 orifice diameter. Exact values depend upon nozzle designs and operating conditions. The average tangential velocity (U T ) is calculated from the flow rate, flow area, and the swirl angle imparted to the flow. Q cos a (A g )n Assume the dried product particle size distribution is similar to wet spray distribution. Method I (Lewis—Nukiyama—Tanasawa equation) Substituting pilot plant operating values in equation (6.80) D vs = 86 micron 86 = 157( 0.5 70 440 (6.86) 86 = 63 + 87 0.45 1 + 597( 70 x 1.02 r 15 0.35 ° 5 L.K N O.05(440/1.02) ' ] F0.3361 " KN K N = 0.8. (6.87) For scaled-up dryer : 120 Feed rate per nozzle = 60 where (A g ) = groove cross-sectional area, n = number of grooves, a = angle of grooves to plane 90° to the nozzle axis. For values of UT in ft/sec equation (6.87) can be rewritten as 0.32Q cos a UT = = 0.5 gal/min. x 4 Increase in capacity obtained solely by pressure change (A g )n where (A g ) is in' and (Q) is US gal/min. The much quoted Lewis—Nukiyama—Tanasawa relation (7) is given in equation (6.80). It differs greatly in form from the Tate—Marshall equation . as droplet size appears independent of the tangential velocity for constant feed rates, orifice sizes and liquid pressure. Use of equation (6.80) requires a value of the constant K N , which invariably necessitates experimental determination or (as a last resort) estimation. Predictions of mean droplet size using the two general equations are not consistent, but are usable in first design calculations to establish the order of magnitude of the spray droplet size. The Tate—Marshall correlation is the easier to apply. Example 6.12 illustrates predictiOn of mean droplet size using the two equations. The Kim—Saunders equation (6.82) is proposed for large scale nozzles. EXAMPLE 6.12 A centrifugal pressure nozzle operating successfully in a pilot spray dryer is to be used in a larger unit. Operating with a feed rate of 21 gal/hr at 440 psi, analysis of the dried product gives a Sauter mean diameter of 86 micron. If the feed rate in the scaled-up dryer incorporates four similar nozzles, and the total feed rate is 120 gal/hr, what mean droplet size is likely to be obtained? Feed data: p = 1.02 g/cm 3 , o- = 70 dynes/cm, p = 10 cP. Nozzle data : d e = 0.05 in, U, = 57 ft/sec at 21 gal/hr, UT = 13.4 ft/sec. Q = fl = 0.35 gal/min = 440 psi P2 N al 2 (6.66) LQii .5 2 — ) = 900 psi Pressure required for new condition = 440 x( 0 0.35 Substituting in equation (6.80) P = 900 psi KN = 0.8 Q = 0.5 gal/min D os = 71.5 micron G. Method II (Tate—Marshall equation) Substituting values into equation (6.81) for nozzle operation in pilot plant unit 10, s = 286(0.05 + 0.17) exp [57 — 0.0094(13.4)] = 286(0.22) exp 0.102 -= 70 micron. For scaled-up dryer : Tangential velocity component at nozzle = UT = 13.4 x Axial velocity component at nozzle = U v = 57 x 0.50 = 19.1 ft/sec 0.35 0.50 = 81.5 ft/sec 0.35 188 ATOMIZATION 189 THE PROCESS STAGES OF SPRAY DRYING Substituting values in equation (6.81) the mean size predicted at higher pressure 13 0 0094 19.1 ] D„ = 286(0.05 + 0-17) exp [81•5 = 286(0.22) exp — 0.02 = 62 micron Size predicted by equation (6.80) D vs = 71.5 micron. Size predicted by equation (6.81) D„ = 62.0 micron. (g) Nozzle Operating Features and Nozzle Applications Centrifugal pressure nozzles are employed in a variety of applications where feeds are of low viscosity and contain no large solid particles in suspension. With correct nozzle selection both fine and coarse sprays can be obtained. A comprehensive range of nozzles are offered by all nozzle manufacturers to meet any requirement of capacity and spray angle. • The advantages of centrifugal pressure nozzles lie in their low cost, ease of replacement and simple maintenance. Low costs result from nozzles being machined from small metal bulk, usually of readily available metals, i.e. standard stainless steels. All parts of nozzles are readily dismantled. Manufacturers have achieved the fine art of being able to duplicate performance of replacement metering parts of a nozzle, i.e. orifices and swirl inserts. This enables replacement parts in reconditioned nozzles to perform consistently without constant adjustment to the feed system. It must be pointed out, however, that for reasons of economic manufacture, slight deviations in nozzle performance are inevitable from part to part, but variations from rated flow or spray angle are only of the order 3-6 %, which for industrial spray drying applications can be tolerated. Maintenance of nozzles is straightforward as their construction is basically simple. All parts fit with small tolerances and there is little chance for assembling nozzles incorrectly. Attention must be given to any packing seals as these must always be in perfect condition. A leaking nozzle creates wet deposits in the drying chamber. The main disadvantages concern the need for high pressure pumps, effective feed filtering (straining) to prevent orifice clogging, and severe restrictions on the type of feed material the nozzle can handle without undue wear. Nozzle durability has increased considerably over the last decade by the use of modern materials, that are extremely abrasion and corrosion resistant. Nozzle erosion must be prevented, as spray dissymetry results from worn metering parts. Wide fluctuations in feed rate can then occur. A poor quality product is produced, and there is extensive dryer down time for nozzle maintenance. Centrifugal pressure nozzles are prone to wear as high liquid velocities are generated in the swirl chamber and orifice. The higher the feed pressure and feed solids content, the greater the chance of nozzle wear. Wherever high velocity flow occurs, the flow surface is fabricated in a hard material. Tungsten and silicon carbides are highly anti-abrasive. Chromium carbide resists oxidation or chemical attack, and is used to counter corrosive feeds. Alumina is also used for anti-abrasive or anti-corrosive surfaces. Centrifugal pressure nozzles are not too flexible and optimum operation is within a narrow range of working conditions for a given orifice size and swirl chamber. The flexibility of nozzle assemblies is improved by the design of nozzle bodies to handle a wide range of feed rates through interchangeable orifices and swirl inserts. This is illustrated in figure 6.46 where aqueous feed rates are plotted at fixed pressure against orifice diameter at constant swirl chamber size. Three swirl chamber sizes are given denoted by A, B, C. FEED PRESSURE: 14 ata /2060 p.5.1 1000 0 0.1 I l i 50 0.5 NOZZLE ORIFICE DIAMETER (mm) Figure 6.46. Range of orifice sizes per given nozzle body for optimum atomization conditions. 190 THE PROCESS STAGES OF SPRAY DRYING It can be seen that nozzle body flexibility increases with increased nozzle size, as a greater range of orifice sizes can be fitted on the nozzle body and the feed rate range duly extended. For the smallest nozzle (swirl body A) the range of orifice size that can be fitted covers 0.7-10 mm, and only variation of feed rate between 25-65 litres/hr (5.5-14 g/hr) can be handled for complete atomization. For the larger swirl body B, orifice sizes of 0.9-4.0 mm can be incorporated and a feed rate range of 450 litres/hr (100 g/hr) is achieved with the lower limit around 70 litres/hr (15 g/hr). The swirl body C gives the largest nozzle the greatest flexibility, since any feed rate between 100-1000 litres/hr (22-220 g/hr) can be atomized if interchangeable orifice sizes between 1 , 0-4.5 mm are available. When operating nozzles, care must be taken in their handling. The metering parts are machined with great precision, and thus the slightest damage must be avoided if nozzle performance is to be maintained. A streaky or off-line spray results from damaged orifices or swirl inserts, and the situation may well be aggravated by creating abnormal feed rates. To maintain nozzle performance, periodic cleaning is essential. Reduction in feed rate or streaky sprays may be due to a dirty nozzle, although with correctly filtered feeds, the best of modern nozzle designs are not prone to clogging during operation. Clogging is likely if product is allowed to dry out in the nozzle during shut down. It is standard practice to dismantle the nozzles during shut down, remove any hard deposits on the outer surface with a stiff brush and wash all metering parts thoroughly. If the nozzle is not reassembled immediately, the parts should be left in clean water or weak caustic soda solution. Sizing nozzles for a required dryer performance is often complicated by nozzle selection being made from brochures listing nozzles rated on aqueous feeds. Product flow will invariably differ from that of water. It is advisable to consult nozzle or spray dryer manufacturers for advice or for approval of nozzle selections. Nozzle manufacturers offer comprehensive service as regards performance of their nozzles on particular feeds. For enquiry into a nozzle recommendation, a form similar to that shown in table 6.15 is filled in and supplied to the manufacturer. For products like milk or coffee, Table 6,15. Nozzle Recommendation : Enquiry form A. Customer Date of enquiry B. Product details Product to be atomized % solid content Feed temperature Feed density Feed viscosity at feed temperature ATOMIZATION 19 I Mass flow rate Volumetric flow rate Ph value C. Other feed properties (delete where applicable) Newtonian/non Newtonian flow characteristics Corrosive/abrasive Any special chemical structure? yes/no Chemically active with stainless steels? yes/no D. Spray dryer details Dryer type and size and nozzle location Feed pipe size to nozzle(s) Inlet air temperature Outlet air temperature Number of nozzles in dryer Available operating feed pressure Dryer chamber dimensions Co-current/counter-current/mixed flow E. Dry product details Production rate Moisture content Bulk density Solubility Mean particle size F. Nozzle performance (a) Any limitations on bulk density, if so, state : (b) Desired particle size distribution (c) Any limitation on number of nozzles mounted in dryer. If so, state maximum and minimum number : (d) Any safety hazards in handling product (e) Any particular spray angle G. Previous Nozzle experience in dryer (if any) Manufacturer Nozzle type Number of nozzles mounted Rated flow rate per nozzle on water Wear history of nozzle Any particular operational problems associated with above no zzle(s) For manufacturer use only Recommended nozzle Nozzle type Number mounted in dryer Pipe size Metering parts—type Operating pressure Remarks signed 192 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION that are spray dried in large tonnages using nozzle atomization, charts are available to convert the nozzle water rating, stated in a brochure to the desired product rating. The product solids content must be known. A typical conversion chart is shown in figure 6.47 for the case of a 42 % skim-milk concentrate, atomized with a swirl insert nozzle. At the nozzle rated pressure the aqueous feed rate is seen to exceed the milk feed rate as feed rates increase (dotted line abc). Pressure is represented as a parameter, and thus performance of the nozzle at pressures greater or less than rated pressure can be read off immediately. For selection of nozzles, when the feed rate, feed solids and available operating pressure is known, the equivalent water rating can be read off the chart (dotted line egf). This rating enables correct nozzle selection from the brochures. 42% T S. SK1r'4 WU< CONCENTRATE, 25 . 200 CENTPOISE, 24 16 12 8 4 0 4 8 12 16 20 24 28 32 36 40 CONCENTRATE FEED RATE ( litres / mi Figure 6.47. Performance of centrifugal pressure nozzles (rated on aqueous feed) on 42 % TS skim milk concentrate. (Nozzles with swirl insert.) Nozzle atomization is fully established as a mode of atomization in spray dryers. Centrifugal pressure nozzles are used extensively in many industries, where spray dried products are manufactured in large tonnages. Examples of such products include milk, coffee, detergents, soaps, ceramics, catalysts and many inorganic salts. The use of nozzle atomization for given products is given under each product section. These are found in the chapters on applications, chapters 13-18 (section V). 193 (h) Nozzle Assemblies for Commercial Use A single nozzle assembly is used wherever capacity and particle size requirements of the dryer can be fulfilled without nozzle duplication. A single nozzle layout simplifies the operation by its ease of control and ease of nozzle observation. In industrial sized dryers utilizing nozzle atomization, multi-nozzle assemblies are invariably installed to handle high feed rates. Assemblies are designed to provide equal operational conditions at each nozzle for uniformity of feed atomization. Each nozzle is located so that constant evaporation conditions are obtained around each nozzle. There are two locations of nozzle assemblies commonly used in co-current flow spray dryers. Nozzles are mounted around the periphery of the chamber, or nozzles form a cluster and are positioned at the top of the dryer surrounded by a ceiling (roof) air disperser. Both types have their advantages and disadvantages. The wall assembly permits ease of access to the nozzles from the dryer side enabling nozzle replacement and maintenance to be carried out quickly and simply. Observation of the performance of each nozzle is straightforward. Greater care has to be given in providing uniformity of flow to each nozzle. This is especially so if slurries are being atomized as there is a tendency for the feed solids to settle out in the horizontal feed distributor ring. However, this nozzle assembly is widely used and with much success. The cluster assembly claims improved evaporation conditions by locating the nozzles in the centre of the air disperser for optimum spray—air contact. Access to the nozzle cluster, and observation of nozzles is more complicated but such complications are offset by the advantages of uniform feed distribution to each nozzle. The arrangement of nozzles with access to each nozzle through the dryer wall is applied to dryers of counter-current and mixed flow type. Nozzles arranged in clusters from a single feed pipe system are not so common. For counter-current flow dryers, non-rotary air flow conditions often prevail and the individual positioning of nozzles via the dryer wall enables convenient nozzle adjustment for creating effective spray coverage over the chamber cross-sectional area. For mixed flow dryers, a nozzle cluster on a single feed pipe gives poor nozzle accessibility. Nozzles are normally mounted singly via the dryer cone wall. With this mounting only short feed pipe lengths are required to position each nozzle in the central area of the chamber. The advantage of easy accessibility to each nozzle is obtained without the constructional difficulties of maintaining rigid nozzle positioning over extended pipe projection lengths into the chamber. The number of access points around the chamber wall or the number of feed pipes making up a nozzle cluster can be minimized by the use of multihead nozzles. Each multi-head nozzle can operate 2-3 orifices effectively FEED IN AIR IN AIR IN FEED IN ET?' PRIXECT OUT D. AIR OUT ONIANCE AVIIdS AO SRO NUS SSRDOIld al-II AIR IN FEED IN FEED IN AIR IN AIR IN -.' G. PRODUCT OUT H. PRODUCT OUT Figure 6.48. Positioning of nozzles in relation to air disperser. Table 6.16. Key to Figure 6.48 Air flow pattern in chamber Chamber design Air disperser type Conical base Conical base Conical base Flat base Conical or flat base Roof Tangential entry (top) Roof End Base F Vertical co-current Rotary Vertical co-current Rotary Vertical co-current Parallel Horizontal co-current Rotary Vertical counterRotary or parallel current Mixed Rotary G H Mixed Mixed Conical base Conical or flat base A B C D E Rotary Rotary Conical base Nozzle assembly Single or multi heads, in cluster Single or multi heads, in cluster Single or multi heads, side mounted Single, end mounted Single or multi heads, in cluster or side mounted Roof Single or multi heads, central location Tangential entry (top) Single or multi head, in cluster Tangential entry (side) 'Single or multi head, in cluster NOLLVZINIOIV Dryer type 196 THE PROCESS STAGES OF SPRAY DRYING in spray dryers. Should one of the orifices function incorrectly, however, the whole nozzle head has to be shut off, removed from the dryer and dismantled. This deprives the chamber of the throughput of 2 or 3 orifices and can contribute to a marked reduction in dryer capacity if, for instance, only four nozzle heads are mounted in the chamber. Reduction in capacity need only be short lived, as with good access to the chamber, nozzle exchange can be quickly accomplished. Where any reduction of capacity is undesirable (even over short time periods) a stand-by nozzle arrangement is incorporated in the feed system layout. The use of multi-head nozzles is most effective when nozzles are mounted in close proximity of the air disperser. If multi-head nozzles are mounted at the chamber wall, spray is distributed with less uniformity over the chamber cross section. The high droplet population created by each nozzle is less well contacted by drying air. Air can channel past the droplet population limiting full utilization of the dryer capacity. Whatever the type of nozzle assembly selected for commercial use, all contrive to meet the following features. 1. Ease of access to nozzles. 2. Ease of nozzle removal. 3. Uniformity of feed distribution. 4. Possibility to isolate each nozzle. 5. Possibility to visually observe nozzles in operation. The positioning of nozzle assemblies in relation to the dryer air disperser is illustrated in figure 6.48. The key is given in table 6.16. 6.6.3. Pneumatic (Two-Fluid) Nozzle Atomization (a) Theory Pneumatic nozzle atomization involves impacting liquid bulk with high velocity gas. The mechanism of atomization is one of high velocity gas creating high frictional forces over liquid surfaces causing liquid disintegration into spray droplets. The theory of liquid break-up follows the principles given in section 6.2 as proposed by Castleman (16) amongst others. Liquid disintegration in the presence of gaseous flow involves complex situations of liquid instability, but the overall process can be considered to occur in two phases. The first phase involves the tearing of the liquid into filaments and large droplets. The second phase completes the atomization by further breaking these liquid forms into smaller and smaller droplets. The entire process is influenced by the magnitude of the liquid properties ; surface tension, density and viscosity, and the gaseous flow properties of velocity and density. Gaseous media used primarily in pneumatic nozzle atomization include air and steam. Inert gas, e.g. nitrogen, is chosen for specialized closed cycle spray drying systems. (Hereafter, in section 6.6.3 the gaseous atomizing medium will be ATOMIZATION 197 referred to as air, unless stated otherwise.) A high relative velocity between liquid and air must be generated so that liquid is subjected to optimum frictional conditions. These conditions are generated by (a) expanding the air to sonic or super-sonic velocities prior to contacting the liquid or (b) directing the air flow on unstable thin liquid sheets formed by rotating liquid within the nozzle. Liquid break up is so rapid and effective that sprays of low mean droplet size are formed. Both low and high viscous liquids can be handled. For small liquid feed rates, rotation of liquid within the nozzle is not essential for complete atomization. High velocity air can readily penetrate a low velocity solid liquid jet, causing the necessary turbulence and energy transfer to form a spray of narrow spray angle. Sprays are characterized by high homogeneity. At larger liquid feed rates, however, even high velocity air cannot penetrate the thick solid liquid jets involved. Atomization is incomplete, and there is a wide droplet size distribution throughout the resulting spray. A high percentage of liquid remains in the centre of the spray as a solid jet, and on leaving the nozzle is ejected over large distances. At higher commercial feed rates the liquid bulk must be formed first into thin sheets to assist liquid instability, for effective air—liquid contact and break down of liquid into ligament form or individual droplets. Unless the sheet formation or 'feed prefilming' takes place ineffective atomization results, even at high air velocities. A solid jet of liquid is simply accelerated by the air so rapidly that the liquid acquires the air velocity, minimizing the shear forces between liquid and air. The whole atomization mechanism cm.pends upon these shear forces. Hence pneumatic nozzles often feature centrifugal pressure nozzle designs in the liquid nozzle head to enable the formation of conical liquid sheets through liquid rotation within the nozzle. (b) Design Features Various design techniques are available to produce optimum conditions of liquid—air contact for atomization. All feature prefilming of the liquid in the feed nozzle orifice, and air annulus sizing for acquiring optimum relative velocity between air and liquid at the air nozzle orifice. Four designs are featured : 1. Contacting of air and liquid within the nozzle head (internal mixing). 2. Contacting of air and liquid outside the nozzle head (external mixing). 3. Combined internal and external mixing by using two air flows within the nozzle head (three-fluid nozzle). 4. Contacting air and liquid at the rim of a rotating nozzle head (pneumatic cup atomizer). Internal, external and combined mixing designs of convergent nozzles are illustrated in figure 6.49(a), (b) and (c). Convergent nozzle heads are the 198 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING AIR SLOTTED SWIRL IN SERT ORIFICE FEED-A1R MIXING CHAMBER OINTERNAL MIXING (TWO-FLUID) FEED SLOTTED SWIRL INSERT AIR ORIFICE FEED ORIFICE b) EXTERNAL MIXING (TWO-FLUID) AIR PRIMARY AIR !Ar.4.12LIN FEED SECONDARY AIR •Nit am=4 • Psil■..-2z&iz 7Aka 1P 'iwk i .2, 417.10,..w...womakires illi 1111!"- --15 -..... w.,...h...1,, Im -_ ..,11 11i 1. ., , r:. 7 111111MIIIINk. ■ Nil IIIMIIIIIIIIMMIIII .•....em..i.lik 4AImi v. m 199 most widely applied in spray drying. The pneumatic cup atomizer is illustrated and described in section 6.6.4 (page 229). Internal mixing designs offer the advantage of achieving higher energy transfer* than with external mixing. However, external mixing enables greater control of atomization by independent control of both liquid and air streams. The combined mixing nozzle is a combination of basic internal and external mixing designs. It incorporates the high energy transfer advantages associated with the former type, with the greater control of the spray characteristics obtainable with the latter type. Combined mixing designs provide greater amounts of available kinetic energy for atomization. It is therefore used with liquids of high viscosity, where the advantages of being able to atomize such difficult liquids offset the very low efficiency of the nozzle and the large amount of air required for nozzle operation. Patented nozzle designs are given in references (451) to (463). Counter-contact between air and feed enables the highest nozzle efficiency to be attained. Referring to figure 6.49(c) the feed and primary air flows are subjected to rotation in different direction. Relative velocity on contact is at its highest, optimum energy transfer is created, and feed break-up is completed to form a spray of small droplets. The central air jet of secondary air has little rotation but acts to initiate feed—air mixing and feed break-up. The pneumatic cup atomizer is used for high viscous liquids or to obtain very fine sprays from low viscous liquids. The prefilming of liquid at the rotating nozzle edge provides an excellent uniform liquid sheet for contact with the air flow. (c) Droplet Release and Spray Angle Pneumatic nozzles have great flexibility in producing small droplet sizes over a wide range of feed rates, but the small droplet size does not prevent the occurrence of extensive spray penetration from the nozzle head. On release from the nozzle orifice droplets are carried forward by the momentum of the spray and expanding atomizing air. The droplet size characteristics can be varied over a wide range by adjustment of the feed—air flow ratio at the nozzle head. Spray angles are narrow and cannot be varied appreciably by adjustment of the feed—air flow ratios to the nozzle. The maximum spray angle is of the 4 * Even so, less than 0.5 % of applied energy is utilized in liquid break-up (18). Virtually the whole amount is imparted to the liquid and air as kinetic energy. The horsepower requirement assuming isentropic expansion can be expressed (30): c) COMBINED INTERNAL— EXTERNAL MIXING (THREE-FLUID) Figure 6.49. Designs of pneumatic nozzle heads. Px = 0 • 136M A T {0.5Ma 2 + 2.5[1 --- ( P 0.286 HP P2 where MA is lb/sec, T is °R. Ma is Mach No., P1 /1)2 is initial to final pressure ratio, 200 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING order 70-80°, and is obtainable at the rated maximum feed rate and air pressure for the larger throughput nozzles. The spray angle is decreased by decreasing the feed rate at constant air pressure. Decrease in air pressure will increase the angle as long as the maximum angle has not been obtained. Spray angles can be held constant by modulating air pressure with the feed rate. With internal mixing nozzles, the spray angle changes with the feed—air ratio. The higher the ratio, the larger the spray angle. A mass ratio of feed—air 25 :1, for example, may feature a spray angle of 70-75°, a reduction in this ratio to 8 :1 might well produce an angle of, say 50-55°. A typical relationship between feed rate, air rate, and spray angle for an internal mixing nozzle is shown in table 6.17. The effect on nozzle performance of holding either air pressure, feed rate and spray angle constant is shown. Table 6.17. Typical Performance of Internal Mixing Type Nozzles Aqueous Air feed rate Air rate pressure (lb/hr) (cfm) (atm) Spray angle Constant variable 50 100 150 1150 1300 1400 2.0 0.85 0.25 12.5 11.5 10.0 1.35 1.35 1.35 3.4 3.4 3.4 45° 75° 80° 40° 50° 55° air 200 200 200 1.45 2.5 3.8 1.35 2.05 2.7 70° 60° 50° feed rate constant 1150 1250 1350 10.0 12.0 14.4 2.6 3.4 4.1 45° 45° 45° spray angle constant pressure constant With more viscous feeds, larger mean droplet sizes are produced, but homogeneity is not so high. Pneumatic nozzles have operational flexibility, producing either small or large droplets over a wide range of feed rates according to the air rates (pressures) applied. This is quite unlike the centrifugal pressure nozzle, where capacity has a limited range for complete atomization. Nozzle designs producing small mean aqueous droplet sizes (10-20 micron) are reported by Gretzinger and Marshall (63). Nozzles producing coarse aqueous sprays of mean droplets of the order 300 micron are reported by Chen and Kevorkian (64) for internal mixing nozzles. Gretzinger and Marshall used feed rates of the order 1 lb/min (0.45 kg/min) and small orifice nozzles, whereas Chen and Kevorkian used feed rates of 90-250 lb/min (40-115 kg/min) and larger diameter orifices (7/16-1 in, 11-25 mm). Large mass flow ratios of feed to air (10:1) were used. The production of fine sprays is dependent, however, upon the liquid orifice being circular, and the air annulus (or annuli) being concentric. Eccentric positioning of the liquid orifice in relation to the air nozzle produces sprays of deflected spray angle. The spray contains streaks of partially atomized feed. When orifices are completely true, droplets are distributed uniformly throughout the spray cone. Solid cone sprays are produced. (e) Effect of Variables on Droplet Size Pneumatic atomization has received attention from many workers, but available data do not appear to correlate to any close degree. Available correlations apply to particular nozzle designs operating over restricted working ranges. It does appear, however, that compared with alternative atomization techniques, pneumatic nozzles have been found truly functionable only at flow rates considered moderate by other techniques. Although this may be so, pneumatic nozzles can provide the all important spray distribution when handling feeds of more exacting liquid properties. Studies (65) have shown that the mean spray size produced by pneumatic atomization follows the relation D= In many low throughput nozzles, where extremely fine sprays are produced (mean diameter 15-20 micron), the spray angle may be as low as 10-20°. However, this angle exists at the nozzle head, and within a short distance, the spray disperses. (d) Spray Characteristics Sprays of low viscous feeds are characterized by low mean droplet sizes and high degrees of homogeneity. Formation of sprays having a mass median diameter of 15-20 micron is well established for pneumatic nozzles. 201 A ( V i?ei par B rirr M iq (6.88) where Vrei = relative velocity between air and liquid at nozzle head, Mair/Mlig = mass ratio of air to liquid. The exponents c4 and fi are functions of nozzle design, and A, B are constants involving both nozzle design and liquid properties. (i) Effect of Air/Liquid ratio Of ah./M iiq) on Droplet Size. The mass ratio is one of the most important variables to effect mean droplet size. Increase in the ratio decreases droplet size. Where the nozzle is used to produce THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 203 a FEED - WATER 0 40 160 120 80 200 240 280 SPRAY MEAN DROPLET DIAMETER ( MICRONS ) 0. AIR VELOCITY- SONIC 100 AIR--LIQUID MASS RATIO coarse sprays, the mass ratio becomes the most significant variable as depicted in equation (6.88). Values of M ai ,./Miiq range from 0.1 to 10.0. Below 0.1 atomization deteriorates rapidly even with liquids that are readily atomized. The upper value of 10.0 is the limit for effective ratio increase to create smaller sizes. Above ratio values of 10 atomization proceeds with excess energy expenditure without marked decrease in mean droplet size. Investigators have indicated that droplets of 5 micron do not disintegrate into smaller sizes in the presence of high velocity air but experimental sampling of sprays from nozzles show that sizes down to 1 micron are apparent. The mean droplet size approaches a limiting value asymptotically for increased values of the mass ratio. This is shown in figure 6.50(a), where the effect of air—liquid mass ratio on spray mean droplet diameter at various values of atomizing air velocity is depicted. The effect of air—liquid mass ratio on spray mean droplet diameter at various values of feed viscosity is shown in figure 6.50(b). The limiting value decreases with the (approximately) 0.36 power of the total nozzle air rate. (ii) Effect of Relative Velocity on Droplet Size. Mean droplet size decreases with increase in relative velocity. This can be seen from a cross plot of figure 6.50(a). Increase of the relative velocity between air and liquid at the point of contact increases the air dynamic force (V 2 p a ) in equation (6.88) and more energy is available for atomization. The effect of relative velocity becomes most pronounced when fine sprays are being formed at low feed rates. Hence the limiting mean droplet size is directly related to the air velocity. In fact, mean droplet size varies inversely with the air velocity to the power of 1.14, and inversely to the power 0.57 of the air dynamic force. (iii) Effect of Viscosity on Droplet Size. Increase in viscosity increases mean droplet size. This follows basic atomization theory. The complexity of the atomization mechanism prevents a precise variation to be established. The exponent of viscosity lies in the range 0.30-0.37. Kim and Marshall (66) propose an exponent of 0.322. (iv) Effect of Air Density on Droplet Size. Increase in air density at constant air velocity increases the air dynamic force, resulting in a decrease in mean droplet size. This follows from equation (6.88). (f) Prediction of Mean Droplet Size The ability to predict spray size characteristics is a necessary requirement whenever pneumatic nozzles are to be applied in spray dryers. Correlations expressing nozzle performance are given in table 6.18. The three correlations for two-fluid nozzles represent the most quoted generalized equations available. Figure 6.51 shows nozzle designs on which data for the correlations were obtained. The mean droplet size of sprays is related to the operating nozzle conditions. One correlation is given for three-fluid nozzles. AIR-LIQUID MASS 202 80 - 6-0 - 4.0 2.0- 250cp 5 cp 40 80 120 160 200 240 SPRAY MEAN DROPLET DIAMETER (MICRONS) Figure 6.50. Effect of nozzle operating variables on spray mean droplet size. (a) Effect of air- liquid mass ratio and air velocity on spray mean droplet diameter (typical performance curves for two-fluid nozzles at intermediate feed rates). (b) effect of air-liquid mass ratio, liquid viscosity on spray mean droplet diameter (typical performance curves for two-fluid nozzles at intermediate feed rates). • • ,:". 17z frq . • > 0 . 72 CIL ,9 • P_. c. P • CD 0 THE PROCESS STAGES OF SPRAY DRYING FL " rn ro „ • Iv P 0 P P C) CD a t !-1 - 5 g” r, g a !..-1 . < 1,3 t'- co r 0 Cy en p 6 F.4- '11 ° O. != 7 n •• ch G. ') P Q. o C9 CD vi 0- N ET' S0 I-, N 8' ,: z 0 i t O 31ZZOtq 0rrT1J-a3aHi • 0 N 0 Fp' -,- w co 0. cp 4: •-•1 0 k4;:p . - Table 6.18. Correlations for Predicting Droplet Size (micron) from Converging Pneumatic Nozzles Nozzle type Two-fluid converging Equation number Reference Equation °.s = 1410[o- + 191 ill 91 "5 x 10 3 1•5 ( 0)9 1) °-5 Q. where IIa is ft/sec, p, is lb/ft 3 , o is dynes/cm, i.i, is cP, Q, is ft 3 /min. Dvs (6.89) (65) (6.90) (63) (6.91) (66) (6.92) (66) v. pi M i- H DM,, = 2600 H M GL 04 a where M, is lb/min, 11,, is P, L is cm, G. is lb/min ft 2 . r ( ) 0-17( 1 ) ( m a i ml 249o- ' 1 4 . 3 2 = OY -/ MtvID ( v r2eip JO- 5 7A0. 3 6 4-16 + 12601_ [ 1 ;C I" M1) where m= —1 at (-- 2-) <3 ML in = —0.5 at ( Three-fluid converging D 8140 1 0-"i4 -32 ) °.11 1 + 1240 54 0 P?'" Pia saw) mmD where m = —1 at ( M --1 < 3 M, . Ma M m = —0.5 at Via) > 3 , f)( VreOsecondary air where M, is lb/min, V is ft/sec, p is lb/ft 3 , o- is dynes/cm, is cP, f,„ is wt fraction. Va(av) = fw( Vrel)primary air + •( 1 NOIIVZIIAlaLY >3 ML M, is lb/min, A is in 2 , p i is cP, o- is dynes/cm, p is lb/ft 3 . 206 Nozzle dimensions Liquid nozzle (in) Air nozzle (in) Air anulus area (in') Equation (6.90) GretzingerMarshall (63) Equations (6.91), (6.92) K imMarshall (66) Internal mixing Sauter mean 7-97 < sonic 43-75 19-73 0.3-30 1-10 External mixing Mass mean 5-30 sonic 65 50 1-30 1-25 3.8-22 0.01-0.666 10-100 External mixing Mass mean 6-350 250-sonic 50-65 30-50 8-50 0.06-40 0.7-10 0.015-2.0 0.10-80 0054-0.217 0.145-0.279 0.0035-0.0124 0054-0-222 0.120-0.272 0.00354.054 0.02-1.0 - wiipii p ...." . _I . yo-2 QA ° SAUTER MEAN DIAMETER (MICRONS 1 Equation (6.89)NukiyamaTanasawa (65) III. 1000 Table 6.19. Experimental Conditions Covered by Pneumatic Nozzle Droplet Size Correlations Design Mean size Mean size range (micron) Air velocity (ft/sec) Liquid density (lb/ft') Surface tension (dynes/cm) Liquid viscosity (cP) Mass ratio iM - a iMI — liqu i d,1 Air rate (ft 3 /min) Liquid rate (lb/min) Atomizing pressure (prig) 207 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING ° L . 500 3 - A 100 - - - 10 0, --'- . 2 7.1 6 3 ., _ QA 0 E_ 3 — ° -10 A I 1 - 3.- =104 °A 1 . i 1 i . k 10 -4 1 L 1 I l f i t . i I I -2 -3 0 10 RELATIVE) SEC 0.008-0.08 0.040-0200 00012-0.030 Operating conditions applicable to the equations in table 6.18 are given in table 6.19. Other droplet size relations are given by Lapple (25) and Dombrowski (30). (i) Nukiyama Tanasawa Equation (65). Equation (6.89) expresses the Sauter mean diameter in terms of nozzle operational variables. The equation is not dimensionally consistent. It is plotted for aqueous sprays in figure 6.52. The equation is frequently cited for general application, but in fact was established for feed rates only up to one pound per minute with small diameter nozzles. Applicable nozzle designs are shown in figure 6.51(a). There is doubt on the validity of the equation, if air velocities within the nozzle approach sonic values. At low feed rates, values of the volumetric ratio (Q a/Q i ) exceed 5 x 10 3 in most designs at sonic velocities, and thus the second term in equation (6.89) has little effect on the mean droplet size. The correlation reduces to 1( — (6.93) D cc - Vair PI The exact relationship between relative velocity and the Sauter mean diameter is not clear over the complete range of operating conditions. Experience has shown that air velocities of the order of sonic with mass airliquid ratio of ten are required to produce mean sizes under 25 micron. Figure 6.52. Nukiyama—Tanasawa plot for converging two-fluid nozzles operating on aqueous feed. For equation (6.89) in metric units, values of VA are expressed in m/sec and viscosity in poise. The constant in the first term becomes 585 and the constant in the second term becomes 597. The droplet size distribution for two-fluid nozzles studied by NukiyamaTanasawa followed the function : dN = d(D) (6.94) exp ( - cDg) where N = number of droplets smaller than D, b.c. = constants, m = 2, q = dispersion coefficient. Equation (6.94) can be rewritten as dN d(D) = HO' exp ( - CD's) (6.95) Mugele and Evans (6) show that equation (6.95) can be rewritten as In ( D2 1 dN D(D)) In qc (31 q ) ( 3) r- 1 DN a log10 —( D2 . d(D) ) = (log10 CD 0 (6.96) (6.96a) 208 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING where a is the term containing the gamma function. A plot of log in (1/D 2 . diVid(D)) against D 4 will be a straight line if the spray follows the distribution. For Nukiyama—Tanasawa nozzle designs, q, the dispersion coefficient can be taken as unity. The corresponding plot is shown in figure 6.53. The Sauter mean diameter can be calculated from the value of slope (c = b/2.3). Mugele and Evans (6) show the Sauter mean diameter to be represented by 1/ r--6 ) (r-5 ) (6.97) q q The slope of the plot, figure 6.53, is the measure of c in equation (6.97). DSMD = 9 ( 1 10 ■ 0 10 \ \ upon nozzle dimensions and cannot be equated automatically to unity. Experimentation has shown, however, that 'q' does remain constant per given nozzle design. Values of 'q' can vary between 0.15 and 2.0. For a given spray sample, values of 'q' are selected by trial and error to determine the value that gives the actual spray distribution the closest agreement to the linear relationship of figure 6.53. The size distribution is best conducted by counting droplets that fall into equal size increments (AD), i.e. droplets within the range 7.5-12.5 :12.5-17.5 micron, etc, where AD -= 5. The number of droplets (AN) per given size increment (AD) is obtained. For every size increment, the value of log 10 [(1/D 2 )(AN/AD)] is calculated, and plotted against Dq, where q is the selected value. Values of q are adjusted to obtain the best linear relationship. The relationship between Sauter mean diameter and the slope of the Nukiyama—Tanasawa distribution plot for values of dispersion coefficient is given in table 6.20. 10 - Table 6.20. Relationship between Dispersion Coefficient, Sauter Mean Diameter and Slope of the Nukiyama-Tanasawa Plot (6) q 3 10 1, 5 50 100 150 200 DVS 2 1 0.5 0.33 0.25 10-4 10 209 1.5 b ° ' s 5 b' 110b -2 4080b -3 2.13 x 10 5 b -4 b 2.25D vi 5 Dv-si 10.514s5 a.33 16.0D s 21-5Dv-sO.25 250 SAUTER MEAN DROPLET SIZE (MICRONS ) Figure 6.53. Nukiyana-Tanasawa distribution (a typical plot). The gamma function (r) is described in many textbooks on advanced mathematics. For example, see (67). Function values are obtained directly from tables (68). When q = 1, the gamma function of any integer is the factorial of the integer minus one. Thus for any integer (n), I",, = (n — 1) ! For determination of the Sauter mean diameter, where half integer gamma functions are involved in equation (6.97), F() = m 112 . If other fractions are involved in the gamma function, tables are used. The higher the value of `q' that correlates spray data to the Nukiyama—Tanasawa distribution, the narrower the distribution. General application of the distribution to other two-fluid nozzle designs is doubtful, if the dispersion coefficient is kept al nity. `q' appears dependent EXAMPLE 6.13 A convergent two-fluid nozzle (internal mixing design) is atomizing a Newtonian fluid of 5 cP viscosity at a rate of 48 lb/hr. What mean droplet size is expected if the atomizing air is regulated to a mass air—liquid ratio of five? Liquid Data o- = 70 dynes/cm p i = 80 lb/11 3 Nozzle Data liquid orifice diameter = 0.18 in air annulus area = 0.03 in' Air Data Atomizing air pressure 50 psig at 80°F. 210 THE PROCESS STAGES OF SPRAY DRYING 211 ATOMIZATION Low feed rate and nozzle design suggests Nukiyama-Tanasawa equation applicable. 48 0-8 Liquid feed rate (Q L) = — = 0.8 lb/min — = 0-01 ft 3 /min 80 60 I 5 I I I I I )) =2500 LL ,i ) (Po L D PLOT OF , 104 4 I I 4 I I I 1 " - I I 5 1 I 4 l • • ... ••■ — ... Mass ratio = 5. •• — MEDIAN DROPLET DIAMETER Air rate (QA) = 4.0 lb/min Air density = 0.323 lb/ft 3 QA 4.0 12.4 ft 3 /min 0-323 '= Q r _ 0-01 12.4 = 8-1 x 10' n0.18 2 Area of liquid orifice = = 0.0254 in 2 4 Area of air annulus = 0.03 in 2 — .- — — ..• — •• — 10 15 - QA 1 . Liquid velocity negligible : Air velocity taken as the relative velocity. Substituting values in equation (6.89) . 5 r 5 19 + 1(70 x 80)• 5 ] = 1-42[0-875] °.5 + 191 5 [(5600)' 5 x 101 1.5 104 1 045 [8-1 x 10-1]1.5 = 1.02(0-935) + 191(0-067)" 5 (0-81) 1 ' s = 1.33 + 191(0-296)(0-729) = 1.33 + 41 = 42.33 micron Note: As the liquid properties are similar to water, figure 6.52 can be used to obtain an estimate of the mean droplet size. QL QA = 8-1 x 10' J. = 0-00111 (sec/ft) v From figure 6.52 D vs = approx. 40 micron. I I 7 1 1 1. 1 i e i l l i —_ I I 1 1 1 1. , . Figure 6.54. Gretzinger—Marshall plot for converging two-fluid nozzles, . po , i AIR-LIQUID MASS RATFO 12 4 144 Air velocity = — x 990 ft/sec 60 0 03 - 1410 I i Dvs = ( 990 80] cc 1.0 0 01 144 0 . 94 ft/sec 60 x 0-0254 - Liquid velocity 4,', L.104 , i cm,gmm - (ii) Gretzinger-Marshall equation (63). Equation (6.90) expresses the mass mean diameter in terms of the nozzle operating variables. The equation is shown plotted in figure 6.54. Metric units are applied to the parameter (p a L). The mass mean diameter correlation was drawn up from data using a convergent external nozzle design at low feed rates. An applicable nozzle design is shoWn in figure 6.51(b). Mean droplet sizes within the range 5-30 micron were obtained at feed rates up to 40 lb/hr. Presentation of the droplet size data in the form of figure 6.54 permits the determination of air and liquid rates for mean diameters within this size range. The correlation is of particular interest, as it offers a nozzle design procedure. The design method by Gretzinger-Marshall (63) is illustrated in example 6.15. The method is restricted to co-current contact between air and liquid, and is not applicable if air contacts the liquid at right angles. For rapid and approximate determination of droplet size, a nomograph shown in figure 6.55 can be used. The nomograph was drawn up by Chattergee (69) for air-water systems. Mean droplet size for a Gretzinger-Marshall type nozzle can be obtained directly from the diameter of the nozzle wetted periphery (inches) and the nozzle feed rate, stated in imperial gallons per minute. The nomograph proves a handy method to determine the range in which mean droplet sizes ( micron) of low viscous feeds, i.e. feeds having similar flow properties to water, are likely to be produced. The droplet size distribution data obtained 212 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION NOZZLE AQUEOUS FEED RATE From figure 6.54 DMMD = 7.6 micron {IMP GALLSPER NOZZLE WETTED PERIPHERY (INCHES) 30 ZD From equation (6.99) 1.0 Dvs = 5.3 micron D•6 20 (b) Using figure 6.55 (assume feed properties as those of water). Now wetted periphery = 0.18 in 0.3 1.0 D 30 0 Feed rate = 006 04 004 0.03 02 DMMD = 6.5 micron 0-01 D. MASS MEDIAN DIAMETER 1 MICRONS? Figure 6.55. The Gretzinger-Marshall droplet size relation expressed as a nomograph (69). for the external mixing nozzle are not found to fit standard distribution functions. Gretzinger and Marshall expressed the size distribution in terms of the mass median diameter and the geometric standard deviation (S e ). The geometric standard deviation could be expressed by = 1.77 D (6.98) The relation between the mass mean diameter (.13„,,,m ) and the Sauter mean diameter (D vs ) for use where comparison with other correlations expressing Dvs is required, is given by log D M ,, m = log D vs + 1.1513 log' (S G ) (6.99) General use of the equations (6.90) and (6.98) is not recommended unless nozzles conform to the test nozzle design of external mixing and low feed rates are used. EXAMPLE 6.14 Determine the mean droplet diameter if data in example 6.13 is applied to an external mixing nozzle. Use (a) Gretzinger-Marshall curves, (b) nomograph. Data as in example 6.13 ; mass ratio = 5. (a) Diameter of wetted perimeter (equated to liquid orifice diameter) 0.18 x 2.54 = 0.467 cm Parameter (p a L) = 0 323 48 62.3 = 0.0623 imp gal/min x 80 60 From figure 6.55 0.02 G 213 ' )0.467 = 23.6 x 10 -4 62.4 The accuracy of the predictions depends upon values of air density at the point of liquid contact, and the contact periphery. These values are often subject to speculation. Figure 6.54 is applicable in determining suitable nozzle designs and operational nozzle data for a desired mean droplet size. The GretzingerMarshall method for calculating nozzle performance is illustrated in example 6.15. The Gretzinger-Marshall method is as follows : 1. For the desired mean droplet size, use figure 6.54 to obtain corresponding values of the parameter (p a L) and mass ratio (M a/M,). 2. Assume likely values of air density (p a ), temperature (Ta ) and liquid nozzle wall thickness (t d) for the system under consideration. 3. Calculate values of L from parameter values in step 1. 4. Tabulate internal diameter values of the liquid nozzle. 5. Calculate the liquid flow Reynolds Number (Re) in each case. Tabulate values (Re = 4/x x QpIp) where Q = volumetric flow rate per unit tube width. Delete chosen conditions, where Re is greater than 1000. 6. Calculate liquid film thickness (t) using the volumetric flow rate Q, where Q = pgt3 1311. This is plotted in figure 6.56 for (Re) numbers less than 1000. Plotted on log-form it supplies a direct relationship between Q and t. 7. For correct nozzle operation, film thicknesses must be greater than 0.03 cm, but less than 0.06 cm. This range represents the most favourable atomization conditions. 8. Calculate atomizing air rate. 9. Calculate atomizing air annulus (A = M alV a p a ). 10. Calculate atomizing air annulus cross-sectional area. 214 THE PROCESS STAGES OF SPRAY DRYING 1 1 1 1 - 1 f 1 1 1 i 1 1 ATOMIZATION 1 , I I f I' 1 1 11 I I 1 I 1 I i 215 Table 6.21 0-1 : - - , 1 , 0 , .i 1- - '7. I II Iv V Parameter ( x 10 4 ) (cm) (cm) 30 25 20 15 10 5 1.000 0.833 0.677 0.500 0.333 0.167 0.880 0.713 0.557 0.480 0.213 0.047 III Estimated condition M c./M I 1 2 3 4 5 6 0.32 0.38 0.48 0.70 1.00 2.00 L VI Re td VII (cm) FFLM TRIMNESS t I CM - 0.01 ^ . - 1 I 0.046 0.050 0.054 0.056 0.074 0.120 - Re < 1000 0-301 364 448 575 668 1500 6800 1 1 1 1 1 1 I 1 j 1 10 -4 1 1 1 1 1 1. I 1D-2 [ GA N i i l l i f r I 1 1 3. Calculate values of L (metric units) 1 1 1 to° 10 t For condition 1 = cufEt Figure 6.56. Plot of film thickness against feed rate (for flow conditions in nozzle head). 30 x 10 -4 = 1.0 cm 0-003 Therefore liquid tube thickness - 0.06 cm diameter of tube t d = L - (2 x 0.06) = L - 0.12 cm 11. Calculate atomizing air pressure (P) using the equation according to Fliegner (70): p M a (T) 112 (0.533)C D A . (6.100) 12, Calculate geometric standard deviation (S G ) using equation (6.98). 6.15 Design a small converging external mixing pneumatic nozzle to atomize 20 lb/hr water and produce a mass mean diameter of 20 micron. What is the corresponding Sauter mean diameter? The nozzle is to be operated at sonic velocity. 1. For 20 micron, values of (p a L) and (M a/M,) are given in table 6.21 using figure 6.54. 2. Assume p a 0.003 g/cm 3 , Ta = 80°, liquid tube thickness (t d) = 0.0235 in = 0.06 cm. EXAMPLE Sonic velocity at 80°F = (540°R) = (gKRT/MW) 112 = Va (32.2 x 1.4 x 1.545 x 10 3 x 540) 1 / 2 29 Va = 1159 ft/sec 4 Re = x Qp, 12 it 3 3 where Q is volumetric flow rate per tube width (cm /sec cm) p i = 1 g/cm , = 0.01 g/cm sec (1 cP). Q is calculated from the given mass feed rate, 3 where 20 lb/hr -= 0.32 ft /hr 4 1 ft 3 = 2.83 x 10 cm Q 3 = 0.32 x 2.83 x 104 3 = 2.86 cm /sec 3600 x 0.88 1-0 4 Re = - x 2-86 x -= 364. 0.01 it (6.10) where K = specific heat ratio, R =. gas constant = 1.545 x 10 3 ft lb/°R, MW = molecular weight = 29. Va where L = 1.0 cm, t d = 0.880 cm. 4. Values of ❑ for conditions (2-6) given in table 6.21, column (V). 5. The Reynolds Number can be calculated Values of Re are calculated for all conditions. These are given in table 6.21, column VI. Conditions 5 and 6 are eliminated as Re is greater than 1000. 6. Calculate liquid film thickness (t). The figure 6.56 where t is plotted against (Qpip). Thus for condition 1 Qp 2.86 x 0.01 I) 1.0 = 2.86 x 10 - z cm 3 2 cm sec) 216 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING Corresponding value of t = 0.046 cm. Calculate values of t in conditions 2-4. Values given in table 6.21, column VII. 7. For favourable atomization conditions suitable values of t lie between 0.03-0.06 cm. Any of the conditions (1-4) are applicable for nozzle design to produce the required mass mean diameter. Condition 4 will be selected for its highest air-liquid flow . ratio. Experience shows that a high air-liquid ratio is the surest requirement for effective atomization to sprays requiring such a small mean droplet diameter. 8. Calculate atomizing air rate - 0 70 Now M 1 = 0.333 lb/min. Hence M a = 0.233 lb/min. 9. Calculate air annulus (a). Now A = M alV a p a and by substituting values in consistent units, A = 0.00406 in 2 . 10. Calculate diameter of outer air annulus (d o ). From nozzle geometry A = (7r14)(4 - di) where outer diameter of liquid tube = (0.480 + 0.12) = 0.60 cm = d 1 . Hence d i = 0.236 in A = 0.00406 in' 0.00406 + 0.236 2 = d1). 0.785 0.247 in = d o 11. Calculate atomizing air pressure (P). By applying the Fliegner equation (6.100) where M a = 3.88 x 10' lb/sec, T = 540°K, CD -= 0.95, A = 0.00406 in 2 . P = 43.7 psia. 12. Calculate the geometric standard deviation (S G ) of the resulting spray. Using equation (6.98) S, = 1.77(20' 14 ) = 2.72 The Sauter mean diameter for the spray is given by equation (6.99) log 20 = log D v , + 1.1513 log' 2.72 13010 = log, 0 D v , + 1.1513 log1 0 2.72 Dvs 12.1 micron. The nozzle design for the specifications of the problem is depicted in figure 6.57. AIR TEMPERATURE Ta = 80 217 0 AIR FLOW = 0.233 lb /rni n AIR LIQUID FLOW =0333 Ib AnLIQUID ' AIR AIR VELOCITY Va .1159 ft/sec AIR PRESSURE P 43.7 psia a Figure 6.57. Dimensions of nozzle design in example 6.15. (iii) Kim-Marshall equation (66) (Two-Fluid Nozzle Atomizer). Equation (6.91) expressed the mass median diameter in terms of the nozzle dimensions and operating conditions. The applicable nozzle design is shown in figure 6.51(c). It is applicable to convergent external mixing designs operating with Newtonian liquids. The equation is considered acceptable in representing various designs of pneumatic nozzles since difference in designs are allowed for in the value of the constants. The value of the powers appear fixed if convergent designs are considered. The equation has been developed from results obtained over a wide range of operating variables, and appears applicable to commercial nozzle conditions. The dynamic force of the atomizing medium and the mass air-liquid ratio are clearly shown to be the two most important variables of nozzle performance. There is a similarity with the Nukiyama-Tanasawa equation, but the Kim-Marshall equation predicts larger droplet sizes especially in the smaller size ranges under similar conditions. Closer agreement with the Gretzinger-Marshall equation has been suggested if the second constant in equation (6.91) is increased from 1260 to 3100 (66). Droplet size distributions from the Kim-Marshall test nozzles do not comply with the logarithmic, square root probability or Rosin Rammler distribution functions. Analysis of spray data having the same order of D i, /,„ D , but obtained from varying operating conditions, has shown percentage diameters of spray droplets from convergent type nozzles to be linearly proportional to the median diameters. Droplet diameters corresponding to 10, 25, 75 and 90 % of the cumulative volume distribution can be obtained from the mass mean diameter as : D10 = 0.33 DMMD (6.102a) . D25 = 0 57Dmmn (6.102b) D75 = 1•51DmmD (6.102c) D90 = 1 •98DMMD (6.102d) 218 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING For comparison of data with alternative correlations involving the Sauter mean diameter D vs , the relation Dvs = 0.83D m „ Data cr = 70 dynes/cm (6.103) = 5 cP can be applied. A distribution function for pneumatic nozzle designs in general has been shown by Kim-Marshall to correlate with remarkable accuracy to the modified logistic equation. Based on the logistic equation by Pearl-Reed (71), the cumulative distribution (0,) less than a diameter D (volume basis) is related to droplet size as (1), b(1 b) b - exp (arD) b (D v b= 1 - b 1 + c exp (rx*) (6.105) A plot of log [(1 - b)/(0,, - b)] against x* represents the volume distribution curve as a straight line, where values of r and c are obtained from the graph as the slope and intercept, where r = - 2.18, c = 6.67. Substitution of these values in equation (6.105), the relative cumulative distribution less than D becomes c1) „, = ( 1.15 ) Tiro = 990 ft/sec p a = 0.323 lb/ft' p i = 80 lb/ft 3 Ma = 5 (6.104) where r is a parameter, and a and b are constants. Kim-Marshall used a size parameter (x*) defined by the ratio (D/D MMD ). Equation (6.105) rewritten in terms of (x*), where a = (D MMD ) - ' becomes 0.150 (6.106) 1 + 6.67 exp ( 2.18x*) Equation (6.106) has an inflection point at = 0.42 and x* = 0.87. The constants (r and c) appear to hold for pneumatic nozzles of different dimensions and design features. Equation (6.106) can be used to predict size distributions of pneumatic nozzles. Differentiation of equation (6.106) with respect to x*, yields the volume frequency c/),, function. 16.7 exp ( 2.18x*) [1 + 6.67 exp (- 2.18x*)] 2 (6.107) Similar distributions on number and surface basis are derivable by use of appropriate multiplying factors. EXAMPLE 6.16 Compare the nozzle performance predicted in examples (6.13) and (6.14) with a prediction using the Kim-Marshall equation. 219 A = 0.03 in 2 A. Sauter Mean Diameter (Dva ) using Kim-Marshall equation. Substituting in equation (6.91) ) 249(70 0 ' 4 1 )(5 0.3 2 0.36 0-$7 2 DMMD (80) ° '" (0.03) [(990) x (0.323)] (5 )2 \ 0.17 1 c) - 0 5 + 1260 x ((990)o.54)k-i 80 x 70 ) D M MD = 8.4 micron From equation (6.103) Dvs = 0.83 x 8.4 = 7.0 micron B. Size Distribution of Spray For cumulative distribution and frequency data equations (6.106) and (6.107). Data for values of x* are given in table 6.22. The cumulative distribution and frequency curves are plotted in figure 6.58 from data in table 6,22. Table 6.22 X* Dmicron Cumulative distribution (relative) 0.25 0.5 0.87 1.0 1.5 2.0 2.5 2.1 4.2 7.3 84 12.5 16.8 21.0 0.086 0.208 0425 0.505 0.770 0.910 0.970 Frequency (relative) (volume basis) 0.410 0.525 0.650 0.400 0.160 0.068 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION 10 0 ,8 ) 06 - 0.4 inflection point (7.3 )(0.4 2 5) > 0.2 - 0.2 w CC 0 4 8 12 15 24 20 MASS MEAN DIAMETER Limp RELATIVE CUMULATIVE DISTRIBUTION LESS 1 .0 (VOLUME BASIS I 220 H z Figure 6.58. Size distribution for two-fluid nozzle (after Kim—Marshall (66)), (a) Cumulative plot. (b) Frequency plot. Droplet sizes corresponding to 10, 25, 75 and 90 % of the cumulative volume distribution can be calculated directly from equation (6.102). 221 The close agreement between the Gretzinger—Marshall and the Kim— Marshall predictions but substantial difference with the NukiyamaTanasawa prediction is due to the design of nozzles used in the investigation. The Japanese workers used internal mixing designs, while the American workers used external mixing designs. Use of the correlations must be restricted to the design of nozzle under investigation. The topic of nozzle dimensions and the effect on spray size remains highly controversial. Nukiyama—Tanasawa report no effect on mean droplet size for increase in liquid nozzle diameter in their designs. Gretzinger reports decrease in spray size, whereas diverging nozzle designs show increased spray size. D. Kim—Marshall equation (Three-Fluid Nozzle Atomizer) Equation (6.92) correlates the performance of a three-fluid nozzle atomizer. The nozzle design is shown in figure 6.51(e). The liquid flow is contacted on two sides by two separate air flows. Such nozzles perform similar to two-fluid converging designs. Spray uniformity is improved by virtue of greater energy being available for atomization. The overall efficiency of the nozzle is lower. The form of equation (6.92) resembles equation (6.91). The exponent of the air dynamic force increases to 0.72 from 0.57. This suggests the mechanism of atomization for the three-fluid designs may differ from conventional designs. Air rate remains the greatest influence on droplet size. Inspection of the equation shows the velocity of contact between air and liquid to be determined from the mass fractions (f,,,) of air flowing in the primary and secondary nozzle annuli. The velocity is given by D 14 = 2.8 micron V = (MT/re ,) primary nozzle) + (1 — f,,(K e ,) secondary nozzle) (6.108) 4.8 micron where f,, = fraction of total atomizing mass air rate passing to primary nozzle. (g) Comparison between the Spray Characteristics of Two- and Three-Fluid Nozzles The spray characteristics obtained by two- and three-fluid nozzles are similar when atomizing low viscous Newtonian feeds at low to intermediate feed rates. A single air stream is sufficient to complete liquid break-up and achieve a fine atomization. The second air stream of the three-fluid nozzle often raises the air—liquid flow ratio above the limit where further increase of this ratio produces a reduction in mean spray size. Use of the second air stream merely constitutes a waste of energy, except perhaps for high feed rates of low viscous liquids, when a marginal improvement in spray characteristics is obtained for this extra energy input. Two-fluid nozzles are available from manufacturers' stocks in all sizes. Small nozzles can produce sprays of mean size down to 30 micron on relatively low viscous feeds. Larger nozzles for commercial use produce coarser sprays as higher feed rates must be handled per nozzle. D25 = D75 = 12.7 micron D90 = 16.6 micron C. Comparison of Mean Droplet Size Data Results using the three proposed correlations, equations (6.89), (6.90), (6.91) on identical nozzle operational data are given in table 6.23. Table 6.23. Comparison of Predicted Mean Droplet Sizes Correlation Sauter mean diameter (micron) Nozzle design Nukiyama—Tanasawa Gretzinger—Marshall Kim—Marshall 43.3 5.3 7-0 internal mixing external mixing external mixing 222 THE PROCESS STAGES OF SPRAY DRYING For high viscous feeds, there is a great need for the second air stream of the three-fluid nozzle, if complete atomization is to be achieved, and a fine spray produced. For high feed rates, substantial air flows are required in each nozzle stream. For non-Newtonian high viscous feeds, a two-fluid nozzle will prove satisfactory only if feed rates are low. As feed viscosity is increased, a two-fluid nozzle will commence to produce coarse irregular atomization at a much lower viscosity level than with a three-fluid nozzle. Hereby lie the main advantages of three-fluid nozzles in spray drying (326) ; (a) the ability to atomize higher viscous feeds and yet form sprays of low mean droplet size, and (b) to produce a narrower droplet size distribution with low viscous feeds. Comparing a two- and three-fluid nozzle of similar size and operating under similar conditions, the three-fluid nozzle will generally produce mean spray sizes 10-15 lower than two-fluid nozzle for mean sizes under 100 micron. (h) Pneumatic Nozzle Assemblies and their Operation Pneumatic nozzles are mounted individually around the chamber wall or roof, or in cluster form located in close proximity to the air disperser. Mounting positions are similar to those described for centrifugal pressure nozzles. The desirable features of mounting as listed on page 193 also apply. Nozzle access and nozzle removal is complicated by having both air and feed lines to each nozzle. The piping arrangement becomes even more complex with three-fluid nozzles, where for each feed line, two independently controlled air supply lines are connected to each nozzle. Wherever nozzles are mounted in the drying chamber, the piping at the nozzle body is covered by a sheath. The sheath forms a compact arrangement. The sheath exposes a minimum of surface area to the drying air while providing a surface that is easy to clean. Nozzle piping connections for twofluid (both internal and external types) and three-fluid nozzles are shown in figure 6.59. All supply connections are made outside the drying chamber, so that the complete nozzle arrangement can be lifted out of the chamber for cleaning or maintenance. The feed system for pneumatic nozzles involves separate control of both feed and gaseous medium (air/steam) supply. The basic feed system for twofluid nozzles is shown in figure 6.60(a). It is established practice to have air flowing to the nozzle before feed is passed to the nozzle. This prevents the nozzle spitting on start-up. A uniform spray and clean nozzle head conditions must be obtained right from the start of operation. Feed deposits during start-up invariably increase during operation, causing deterioration in atomization. Control can be either manual or automatic. Compressed air from a general supply line or local compressor is filtered and the pressure is adjusted ATOMIZATION SHEATH SHEATH a. 223 b. C. Figure 6.59. Piping connections for pneumatic nozzles. (a) Piping connection for a two-fluid nozzle (external mixing). (b) Piping connection for a two-fluid nozzle (internal mixing). (c) Piping connection for a three-fluid nozzle. at a pressure reducing valve to correspond with the operating nozzle pressure. Air flow rate is adjusted by a control valve, and the actual flow rate is observed on a metering device, e.g. a rotameter. When steam is used as the atomizing medium, supplies to the nozzle must also pass through a strainer. This is to prevent any scale or rust particles lodging in the nozzle annuli creating mal-distribution of steam. Feed is pumped to the nozzle via a strainer. All oversize particles, whether foreign matter or product lumps must be removed as the slightest of blockages will give poor nozzle performance. For internal mixing two-fluid nozzle designs, pressures in the feed and air lines are virtually equal. For external mixing two-fluid nozzles, air and feed flow are independent of each other and the pressure depends upon the annuli areas and required flow rates. For three-fluid nozzles, the central air flow contacts feed within the nozzle, and the pressure of these flows is closely related. The velocity of feed entering the nozzle is much lower than the air flow, which then acts with an ejector effect on the feed flow. Feed pressure at the nozzle is slightly lower 1-i_an the air pressure. This ejector effect often enables low feed rates to be handled by the nozzle without the need for a feed pump. Figure 6.60(b), (c) shows two feed systems 224 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION PRESSURE REDUCING VALVE ROTAMETER CONTROL VALVE AIR FILTER FEED WELL__ FLOW METERING DEVICE COMPRESSED AIR FEED FOSITNE DISPLACEMENT PUMP a FEED ATOMIZING AIR NOZZLE CONSTANT HEAD FEED TANK FEED NOZZLE STRAINER OVERFLOW CONSTANT HEAD FEED TANK FEED DISTRIBUTOR RING 225 Air and feed pressures for pneumatic nozzles are observed on standard Bourdon-type pressure gauges. A diaphragm inlet to the feed pressure gauge is required to prevent feed entering the gauge mechanism. The feed rate is conveniently measured by a metering device of the magnetic flow type. An automatic feed—air flow system is shown in figure 6.60(d). The air flow is set manually at the control valve. The air pressure required at the nozzle is prefixed by manual adjustment of the pressure reducing valve. The air flow rate is metered continuously at an orifice plate or venturi. The pressure difference is monitored and transmitted to the ratio recording controller. The controller adjusts the feed rate so that the air—feed flow ratio is maintained. Any change in the air rate causes the air—feed ratio to move away from the set value. The correct ratio is restored by adjustment to the feed pump speed. Distribution of air and feed is from circular rings mounted around the exterior of the drying chamber or on the roof, figure 6.61. This arrangement enables feed and air flow to each nozzle to be shut off when removing nozzles for cleaning or maintenance. If air is used as the gaseous atomizing medium, prefiltering can take place at the point of take-off from the DRAIN DRYING AI R C. b, TWO -FLUID NOZZLE FEED DRYING AIR DRYING A IR ATOMIZING AIR FEED ATOMIZING AIR ORIFICE PLATE OR VENTURI CONTROL VALVE (MANUAL) AIR OR STEAM RATIO RECORDING CONTROLLER MAGNETIC FLOW METER PREFILTERED PEED MONO PUMP WITH VARIABLE SFEED DRIVE AND PNEUMATIC CONTROL a. DRYING AIR FEED Figure 6,60. Feed systems for pneumatic nozzles (two-fluid). (a) Basic system. (b) Siphon feed system. (c) Gravity feed system. (d) Automatic feed system (automatic air—feed ratio control). C. ATOMIZING AIR that do not require pumps. Liquid passes to the nozzle under either siphon or gravity feed. These systems are straightforward to operate, and provide uniform feed flow. Successful operation depends upon the maintenance of the required siphon and liquid head. b. Figure 6.61. Feed and air distribution rings for pneumatic nozzles. (a) Two-fluid nozzle, roof ring distributor. (b) Two-fluid nozzle, wall ring distributor. (c) Three-fluid nozzle, ring distributor in air disperser. 226 THE PROCESS STAGES OF SPRAY DRYING supply main. If steam is used, there is always scale formation throughout the pipework, and filters must be placed as close to the nozzle body as is conveniently possible. Modification to the standard feed system is required for paste-like materials. Many such materials have poor flow properties yet are able to be effectively atomized in pneumatic nozzles of the external mixing type. Pumping pastes into a distribution ring layout is often not possible, or if a degree of pumpability is attained, distribution to each nozzle is by no means satisfactory. In these cases, thick pastes or filter cakes are screw-fed to the nozzle. This involves a complex feed arrangement for each nozzle and therefore is most conveniently adopted in small to medium sized dryers, where a single nozzle mounting is sufficient to meet the drying chamber evaporative capacity. A screw feed pneumatic nozzle is shown in figure 6.62. The thick paste is fed continuously or dumped batchwise into the hopper. The paste is fed to the nozzle orifice by two screw feeders, one in the horizontal and the other in the vertical plane. Paste is pressed through an adjustable feed annulus and immediately contacted with high velocity atomizing air. In the nozzle head the air flows from an annulus within the feed annulus. Turba and Nemath (72) describe this type of nozzle design. AIR FEED HOPPER SCREW FEEDERS NOZZLE HEAD Figure 6.62. Two-fluid paste nozzle with screw feeder. Nozzle cleanliness, whatever the nozzle design, must be maintained at all times. Flushing the nozzle with water is often not sufficient to thoroughly clean the nozzle passages, and any remaining product will dry out during dryer shut down. Dismantling the nozzles during shut down is the recom- ATOMIZATION 227 mended procedure, and wherever labour conditions exist to permit such practice, this should be carried out. It is useful to recall that dried out product remaining in the nozzle head on dryer start-up can cause as many performance problems as a dirty gaseous medium supply. Dryer shut down or reduction in capacity due to mal-operating nozzles is more costly than the extra time spent to ensure complete nozzle cleanliness. (1) Advantages and Disadvantages of Pneumatic Nozzles. The advantages of pneumatic nozzles lie in their capability to produce sprays of high homogeneity and of small mean droplet size. These characteristics can be obtained over a wide range of operating conditions, while handling either high or low viscous feeds. The nozzle design has its operational advantages over other nozzle types. The presence of liquid orifices larger than those in centrifugal pressure nozzles reduces the likelihood of nozzle clogging under normal working conditions. However, the nozzle annulus or orifice for the gaseous medium flow is much smaller by comparison, and all foreign matter that can lodge in the nozzle must be prevented from reaching the nozzle head. Filtered compressed air or clean steam is essential. Pneumatic nozzles do not require high pressure pumping equipment, a notable advantage over centrifugal pressure nozzles, where high pressure working can give operational and maintenance problems. The disadvantages of pneumatic nozzles concern (i) the high cost of compressed air, (ii) the reduction in spray dryer capacity due to cold atomizing air entering the chamber, and (iii) very low nozzle efficiency. Re. 1. Where air compressors are required on site to supply the nozzle system, a sizeable investment is usually involved. Once installment is completed, the cost of producing compressed air becomes expensive as consumptions are high. In small dryers, for example, where similar spray characteristics can be achieved by both pneumatic nozzles and a rotating atomizer wheel, to achieve the same evaporative capacity from identical feeds successful operation of the nozzles may require 20 HP compressors compared with a 5 HP rotary atomizer drive. Performance of nozzles in straight competition with rotary atomizers suffers badly on power consumption. Re. 2. The reduction in available dryer evaporative capacity, due to cold atomizing medium entering the chamber can also be significant. There are many small spray dryer designs that can be operated successfully on either pneumatic nozzles or atomizer wheels, but under similar heat input, spray and feed conditions, the dryer evaporative capacity with pneumatic nozzles can be as much as 20 % lower than the evaporation capacity achieved by using an atomizer wheel. Re, 3. The low efficiency is borne out from the remarks above concerning air compressor operational costs. Defining efficiency as the ratio of energy required to create liquid bulk break-up into droplets divided by the input 228 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION of energy supplied to the nozzle, the energy input is high and the efficiency subsequently low. Efficiencies are of the order of a fraction of a percentage to produce large droplets of 100 micron size. To produce sprays of droplets of the order 10-20 micron, efficiencies are only a few hundreds of a percentage. In spite of some notable disadvantages, pneumatic nozzles are often used in spray dryers. Their ability to atomize high and low viscous feeds, and produce fine or coarse sprays of special size distribution are particularly attractive to industry. (j) Applications Pneumatic nozzles are used mainly to form very fine sprays of low viscous Newtonian liquids. All nozzle manufacturers offer nozzles that cover a wide range of capacities. Nozzles also find applications in atomizing highly viscous liquids, whether they exhibit Newtonian or non-Newtonian flow characteristics. Such feeds include slurries or pastes, gelatine, plastics, glues and pre-gelatinized corn starches. Pneumatic nozzles are suitable for products where flow properties cause sharp increases in viscosity with shear. Such products cannot be atomized in pressure nozzles, but are successfully handled in pneumatic nozzles, where atomization is achieved by application of very low shear stresses, e.g. certain p.v.c. emulsions. The ability of the nozzles to form fine or coarse sprays makes them ideal for use in small laboratory or pilot-plant dryers. Such flexibility is illustrated in table 6.24 by a 3 mm orifice internal mixing nozzle operating on a 60 Table 6.24. Tabulated Data Showing Pneumatic Nozzle Flexibility Feed material: 60 % solid clay slip Orifice diameter : 3 mm 1.2 metre diameter chamber Inlet dryer temperature (°C) Outlet dryer temperature (°C) Air rate (NM 3 /hr) Air pressure (atm) Feed rate (kg/min) Feed pressure (atm) Moisture content ( % H 2 O} Particle size analysis % > 500 micron > 250 micron % > 120 micron % > 60 micron (2) (1) Coarse Fine atomization atomization 375 105 3.4 1.75 0.9 1.6 1.4 375 105 1.9 1.5 1.2 08 5.3 0 4 38 86 4 26 68 94 229 solids clay slip (feed viscosity = 40 centipoise) in a 4 ft (1.2 m) diameter pilot plant dryer. Operational data to form a fine spray is given in column (1), together with the particle size distribution. A 33 % increase in feed rate accompanied by a 46 % reduction in air rate still maintained complete atomization conditions and produced a coarse spray. The coarse spray distribution is given in column (2). Atomization performance of many non-Newtonian liquids in small diameter dryers has been effectively reproduced with large capacities through duplication of scale-up nozzles. The scale-up ability has established usage of pneumatic nozzles in industrial-sized dryers. Use of pneumatic nozzles for heavy pastes has great potential as it offers marked advantages over alternative atomization techniques. Much development is being conducted into aspects of nozzle design for handling high paste throughputs. A typical case is the Baran (73) careless nozzle, reported to handle up to 8000 lb/hr (3600 kg/hr) of 1000 poise paste feeds. Areas to which this type of nozzle design has been successfully applied include titanium dioxide, calcium carbonate, clays, stearates, corn starch, organic and inorganic pigments. 6.6.4. Rotating Pneumatic Cup Atomizers (a) Introduction The combination of a rotating cup and an air flow directed at the cup rim forms a pneumatic cup atomizer. It is an atomizer development for specific cases of(a) obtaining very fine sprays from low viscous feeds and (b) atomizing high viscous liquids (that exhibit flow characteristics not ideal for conventional atomization techniques) to sprays of coarse mean size. The stages of atomization are shown diagrammatically in figure 6.63. The atomization mechanism follows the principles of liquid disintegration by high speed air jets. Liquid flow over the rotating cup produces a liquid film at the cup rim. The high speed air issuing from the air annulus in close proximity of the cup rim causes first film instability followed by film disintegration into droplets. The interaction between air and liquid causes excessive mixing around the cup. Hot or cold air, or steam can be used as the atomizing medium. The success of this atomizer is due to the rotating cup acting as a prefilming device, forming at the cup rim thin liquid sheets of uniform thickness, ideal for break-up into droplets by the impinging air flow. The theory of operation has been extensively reported by Frazer, Dombrowski and Routley (74). A rotating pneumatic cup atomizer is shown in figure 6.64. Feed flows to the rotating cup from a feed pipe mounted within the hollow atomizer spindle, A liquid distributor mounted at the spindle end, distributes the feed via circular holes on to the inner surface of the cup. A weir is sometimes incorporated in the inner cup surface design to assist even distribution of 230 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING 231 FEED PIPE CUP FEED LIQUID FLOW AIR ANNULUS AIR FLOW FEED FILM FILM INSTABILITY 11 1 L ■ , r 7 , •:.- LI QUID FILM DISINTEGRATION • / • / ?.. - ,.K \ AIR SWIRL VANES Figure 6.63. Atomization mechanism for a pneumatic cup atomizer, feed over the entire inner surface area. The liquid film streaming off the cup is impacted by air flowing from the air nozzle annulus. The air velocity is in the sonic range. Within the air nozzle, swirl motion is generated by directing air flow over inclined vanes. In the diagram sealed spindle bearings are shown. These bearings can be air cooled when steam or hot air is used as the atomizing medium. Spray angles from pneumatic cup atomizers are small. Spray droplets are carried rapidly forward with the momentum of the spray. Drying chambers require an extended vertical height to compensate the trajectory distance of droplets from the cup before effective spray-drying air contact is achieved. The effectiveness of the atomization mechanism enables difficult, high viscous liquids to be atomized at feed rates high enough to be of interest to industry where large air rates can be tolerated, i.e. Air—liquid mass ratios greater than two. In large dryers duplication of cups is possible, but is not applied if each cup operation requires excessive volumes of air. Where duplication is used, each cup has its own drying air supply. To prevent interference between sprays, a prominently parallel air flow through the chamber is created by a perforated plate air disperser. In dryers fitted with a single cup unit, an air disperser creating a rotary flow pattern in the chamber can be successfully used in tall narrow chambers. Air dispersers for pneumatic cup atomizers are shown in figure 6.65. LIJUID DISTRIBUTOR AIR ANNULUS CUP LiP . Figure 6.64. Pneumatic cup atomizer head. (b) Effect of Variables on Droplet Size The effects of variables on droplet size are similar to those discussed for pneumatic nozzles. Increasing the air flow to the cup rim at constant feed rate and cup rotation decreases the mean droplet size, and the overall spray angle is narrower. Increasing the feed rate increases the mean droplet size, 232 THE PROCESS STAGES OF SPRAY DRYING FEED ATOMIZATION FEED FEED 233 Table 6.25. Correlations for Predicting Droplet Size from Pneumatic Cup Atomizers 4 COOLING AIR '0' 21 R Dvs= 6 x 10_ + [ 1.40 0.5 [1 + Pa 0.59e •5 D„ = 6 x 10 -4 + [ 0 .5 p a (ad + 0 21 0.0651F 1 .5_ .44/1 1 LVI-(05Vi [ 0.0651 Mr] 1+ 10.5 5 (6,109) VR + 1) 10.5 (6.110) — V, + 1)] in cgs units. DRYING AIR the sheet thickness (s) at the cup lip, as obtained from equation (6.111). AIR AIR s= (a) PRODUCT PRODUC T PRODUCT ATOMIZING AIR CUP MO TOR DRIVE PEED BULK DRYING AIR THROUGH PERFORATED PLATE AIR DISPERSER SWIRLING DRYING AIR FLOW AROUND EACH CUP ATOMIZER 3.PNEUMATIC CUP ATOMIZERS PLACED EGUIDISTANT(601 FROM EACH OTHER (b) DRYING AIR Figure 6,65. Pneumatic cup atomizer and air disperser positioning in drying chamber. (a) Single atomizer arrangements. (b) Multi atomizer arrangements. but the effect is reduced in the presence of high air velocities. The air velocity has more effect on droplet size than the cup rotation speed. Increased cup speeds do not impart much more energy to the liquid due to liquid slippage over the cup surface. Droplet size of low viscous feeds appears little influenced by the air—liquid mass ratio for values of the ratio greater than 3 : 1. (c) Prediction of Mean Droplet Size The Sauter mean droplet size obtained from the rotating pneumatic cup atomizer can be calculated by equations (6.109) and (6.110). These equations are given in table 6.25. Equation (6.109) expresses the mean size in terms of [ 3Qv 1 113 2n V T sin 0 (6.111) where 0 = half angle of divergence of the cup lip. Equation (6.110) expresses the Sauter mean size in terms of the liquid flow rate and other operating variables. The correlations were developed over the following range of conditions : Feed, kinematic viscosity (v) surface tension (a) density (p) Feed flow rate Air velocity Air flow rate Cup speed Cup diameter Measured Sauter mean diameter Maximum diameter 5-165 cS 49-35 dynes/cm 50.5-52 lb/ft 3 (0.81-0.835 g/cm 3 ) 10-1000 lb/hr (4.55-455 kg/hr) 95-650 ft/sec (29-197 m/sec) 50-1000 lb/hr (23-455 kg/hr) 1500-6000 rev/min 4 in (10 cm) 24-320 micron 210-630 micron (d) Prediction of Droplet Size Distribution Frazer, Dombrowski and Routley (74) report that sprays formed from rotating pneumatic cups approximate to the Rosin—Rammler distribution. The Sauter mean diameter and the maximum droplet size in the spray depends upon the value of the mean size as given in table 6.26. EXAMPLE 6.17 A 6 cm pneumatic cup atomizer is fed with 100 kg/h of a 40 % solids plastic emulsion, and uses 180 kg/h of compressed air. The atomizer speed is 3500 rev/min. Air is directed 4 mm from the cup lip. The air annulus is 1 mm. Using the data given below, predict the spray characteristics. Data for equation (6.110): 3 a = 63.7 dyne/cm, p a = 1.21 x 10' g/cm , v R = 94.5, d = 6 cm, a = 0.4 17.3, Q = 26.2 cm 3 /s, M R = 1.8. C111, VT 1100 cm/s, Va = 190 m/s, VR = 234 THE PROCESS STAGES OF SPRAY DRYING ATOMIZATION Table 6.26. Relation between Sauter Mean Diameter and Maximum Spray Droplet Size Sauter mean diameter (D„ Rato Ratio (micron) maximum diameter (D „,„„) mean diameter D vs 10.0 80 6.0 4.5 4.0 3.4 2.8 24 2.1 2.0 20 30 40 60 80 100 150 200 250 300 Now D, = 6 x 10' + (A)(B)(C) ° ' S . A= r B [ C0'5= ' x 94.5' 1 ) ' (0.4 x 6 + 0.42)0'25 = 226 0.59 x 63-7 L(1.21 x 10 1+ 0 5 -3 ° 5 0.065 = 1.027 (1.8)1'5 10.5 26.2 [(1100) (0.5 x 17.3' — 17.3 + 1) 3 1.21 x 10 -5 D„ = 6 x 10 -4 + (226)(1.027)(1.21 x 10 -5 ) cm 39 micron From table 6.26 Dm ax = 6.2 D,,, a), = 242 micron 6.7. Sonic Atomization Interest in the possible use of sonic atomization in spray drying has been growing over the last decade. This has come about by the need to develop a technique which can deal with the increasing number of liquids that cannot be atomized successfully by wheels, nozzles or cups. Such liquids include the non-Newtonian, high viscous and long molecular chain structured 235 products that form only 'strings' or filaments from rotary atomizers (not individual droplets) and liquids that require excessive pressures for effective atomization in centrifugal pressure nozzles. Attention was drawn to the use of sonic energy, as the likely mechanism of atomization suggested the formation of uniform droplet sizes. Sonic nozzle development has not yet reached the stage where such nozzles are a real alternative to more conventional atomizers already established in spray drying. However the development is still at an early stage. The advantages of sonic nozzles operating at low pressures and having wide liquid channels suggest suitable use for abrasive and corrosive materials. Perhaps the most immediate development of sonic energy use in spray drying will be the employment of ultrasonics to promote increase drying rates (82). Already small-sized spray dryers have been fitted with a multiwhistle liquid atomizer and ultrasonic sources placed in the dryer walls at the level of the drying zone. A marked improvement in dryer capacity is claimed. The theory of sonic atomization is described by Antonevich (75). Patented nozzle designs are given in (81) (464) to (468). The four main types are the Hartmann mono whistle nozzle (80), stem jet nozzle (76), vortex whistle nozzle, and mechanical vibratory nozzle (77)(78)(470)(471). Prediction of spray characteristics is discussed by Peskin and Raco (79), Wilcox and Tate (80) and Popov (77). 6.8. Atomizer Selection The function of any atomizer is to produce as homogeneous a spray as possible. When selecting from the various types of atomizer available, consideration must be given to the design which produces economically the most favourable spray characteristics for a given set of operational conditions. 6.8.1. Selection based upon Desirability The most desirable characteristics of any atomizer can be listed as : a. simple construction b. designs conducive to easy maintenance c. available in both small and large sizes d. spray size distributions controllable through adjustment to atomizer operating conditions e. operated by standard pumping equipment, gravity feed or siphon feed systems .1. handle feed without internal wear. Certain atomizers, in spite of exhibiting some or all of these features, are still not suited to certain applications due to accompanying undesirable features. 236 ATOMIZATION THE PROCESS STAGES OF SPRAY DRYING These undesirable features could be (a) the necessary feed system not compatible with the method of atomizer operation, (b) droplet release characteristics from atomizer not compatible with dryer chamber design, (c) insufficient mounting space for atomizer. 6.8.2. Selection based upon Spray Characteristics With proper design and operation, nozzles and rotary atomizers can produce sprays having similar droplet size distribution. There is the general opinion that atomizer wheels produce sprays of greater homogeneity, but this is not always borne out in practice, especially at low feed rates, when fine sprays of similar characteristics can be produced by wheels and nozzles. A coarse droplet—particle requirement at industrial feed rates can generally best be achieved with a centrifugal pressure nozzle and a fine droplet—particle requirement with a rotary atomizer. Examples of the particle size distribution for spray dried silica and alumina based catalysts produced by rotary and nozzle atomization, as shown in figure 6.66, illustrate this. The unbroken lines indicate the two distributions to have similar form. The shaded areas _ 1 I 1 1 1 1 1 1 CUMULATIVE PERCENT LESS THAN D 99.5 95 I 1 1- 1 1 1 1 1 _ r _ .er 4 I... ip 00 – – _ 70 _ 90 gatIAI A III r lk 0 114 ■0"-". 41 otiAi M ArusT W . 11 i I I AS ;0111 1 r ll Iv SA1 tra I I I illif i: ROTARY ATOMIZER { wheel ) 411100 _ ANtrilillifir 50 govil ,fflot be 30 _ 10 _ _ I i I 1 1 I I I _ Ail or , NOZZLE ATOMIZER 4-ozig.---__...„,,ssow 1111 101.1—rf 'Aar er„m7A0 a lli tgi rigir t• opf 01 I 5 _ 10 – _ _ I {pressure) I 1 I 100 i i i .._ _ i 1000 PARTICLE SIZE . D. {micron) Figure 6.66. Particle size distributions of rotary and nozzle atomizers operating on silica and alumina based catalysts. 237 indicate the variation of particle size that can be obtained by adjustment to the atomizer operation. The shaded areas overlap indicating the two atomizers to produce similar sprays under specially selected conditions. 6.8.3. Selection Basis For a given spray drying application, the selection between rotary and nozzle atomizers involves the following considerations : 1. The feed capacity range of the atomizer where complete atomization is attained. 2. The power requirement of the atomizer to attain complete atomization of the feed (atomizer efficiency). 3. The droplet size distribution at identical feed rates. 4. The maximum and minimum droplet size levels (spray homogeneity). 5, The operational flexibility. 6. The drying chamber design, most suitable for atomizer operation. 7. The feed properties most suitable for atomizer operation. 8. The atomizer experience available on product in question. Re. 1. Designs of rotary and nozzle atomizers are available to cover all capacity requirements in the low—intermediate—high feed rate ranges. It is at very high capacities that rotating atomizer wheels emerge as the most favourable method, in spite of the ability to reach such capacities through duplication of nozzles in multi-nozzle atomizer systems. Re. 2. The power requirements of atomizers are of the same order for most spray drying conditions and rarely do such requirements have the ultimate say in atomizer selection. Power input to atomizers greatly exceeds the theoretical energy requirement for liquid bulk break-up into spray droplets (18)(30). Efficiencies are very low and are normally ignored or considered of secondary importance as long as the desired spray characteristics are being obtained at rated capacities. Thus the extremely low efficiencies of a three-fluid nozzle become of no consequence, if a high viscous liquid can be successfully atomized only by such a nozzle. Re. 3. Droplet size distribution from rotary and nozzle atomizers can have similar characteristics at low to intermediate feed rates even though the mathematical laws they follow are not always the same. At high feed rates spray homogeneity is generally greater with rotary atomizers. Re. 4. It is often the range in which the maximum, minimum or mean sizes fall that is the important performance criteria. Vaned atomizer wheels, two-fluid nozzles and pneumatic-cup atomizers are favoured for the finest spray requirements, vaned atomizer wheels and pressure nozzles for general use in the intermediate size range, and vaneless discs, or pressure nozzles for coarse sprays. Re. 5. Atomization by rotary atomizers is generally more flexible than nozzle atomization from the operational standpoint. For a given rotary 238 THE PROCESS STAGES OF SPRAY DRYING atomizer application, a wheel might handle wide variations of feed rate without much variation in the particle size of the product, and without the necessity of changing dryer operating conditions. Only alteration of wheel speed is required. The extra power requirement for any speed increase is normally available. For a given nozzle application, increase in dryer capacity requires an increase in feed pressure, but there is an accompanying change in the spray size distribution. When the spray characteristics are strictly specified duplication of nozzles is required. If the available pressure is limited, but spray characteristics are not critical, exchange of nozzle orifice size will suffice. Re. 6. When selecting atomizers, dryer design plays an important part. From this viewpoint, nozzles are the more adaptable. The confined nature of nozzle sprays enables any nozzle positioning in either co-current, countercurrent or mixed flow drying chambers with air dispersers creating rotating or parallel air patterns. Rotary atomizers generally require a rotating air pattern. Re. 7. Atomizer wheels and nozzles are available to atomize low viscous, non-corrosive and non-abrasive liquids with equal success. Wheels are suited for handling corrosive and abrasive slurries and powder feeds (figure 6.67). For products that create pumping problems, under high pressure, wheels are normally first choice, although pneumatic nozzles can also handle such feeds. Often the pressure requirement of centrifugal pressure nozzles is too high. A standard pneumatic nozzle might produce a 60 micron mean droplet size operating at 100 psig (7 atm) at a feed rate of 10 lb/min (4.5 kg/min). A centrifugal pressure nozzle may well require 1000-5000 psig (7-35 atm) to create the same spray conditions. Pneumatic nozzles also provide the best atomizing technique for liquids of long molecular chain structure. These are usually high viscous and non-Newtonian materials. Many high viscous Newtonian feeds can be atomized by wheels and nozzles, following preheat for maximum reduction of viscosity. There are circumstances where each type of atomizer is unsuitable. Should the feed contain fibres, pressure nozzles are unsuitable. Should the feed concentrate be unable to withstand impact, or the feed capacity be met only if vast quantities of atomizing air are available, two-fluid nozzles become unsuitable. Should the feed concentrate resemble a long-chained polymer, which forms threads and not droplets from vaned atomizer wheels, this technique becomes unsuitable. Re. 8. Selection of an atomizer for a new spray dryer installation is based normally on past experience of spray drying the product. In cases where rotary and nozzle atomizers can be used with equal success, e.g. many milk products, dryer manufacturers favour either one system or the other system. Manufacturers will state their preference as the best method. The favoured ATOMIZATION 239 method is often shown by the range of drying chamber designs offered as standard by a manufacturer. Preferences have led to milk dryers in the United States oi America being invariably fitted with nozzle atomization, whereas in Europe rotary atomizers show much greater prominence. However, there can be differences in the dried properties (e.g. bulk density, particle shape) of product produced from nozzle or rotary atomizers. The extent of these differences depends entirely on the product properties and product treatment within the atomizer. With new products there is no previous plant experience on which to base atomizer selection. However, any new application is developed through laboratory and pilot-plant testing, the results of which decide virtually the most suitable atomization technique. Most spray dryer manufacturers have extensive laboratory facilities equipped with units with both rotary and nozzle atomization. The outcome of tests with various atomizing methods gives an unbiased selection. The most suitable atomizer at testing levels must have the same performance when scaled up to handle industrial capacities if the choice is to be of any value. In conclusion it is fair to point out that a clear cut choice between nozzle and rotary atomization is rare. Circumstances arising from the projecting of spray dryers usually dictate the atomizer choice (520). If the feed is corrosive or abrasive, an atomizer wheel virtually decides itself, being a low LIQUID FLOW P - POWDER FLOW L- Figure 6.67. Modifications of the atomizer drive to handle liquid, powder or liquid—powder feeds. 240 THE PROCESS STAGES OF SPRAY DRYING pressure device with easy incorporation of wear resistant parts for prolonged trouble-free operation. If dried product quality is well defined, the specifications may automatically call for a certain nozzle or special wheel design. It may even call for use of dual atomizer systems, i.e. systems comprising (a) both a rotary atomizer and nozzle mounted in the drying chamber (83), (b) mounting of nozzles having different orifice and swirl chamber sizes, or (c) atomizer wheels having tiers elliptically shaped or of different diameters. If a range of products are to be handled in the same dryer, atomizer flexibility is essential. Here the rotary atomizer is the usual preference since by mounting different wheel designs on the atomizer drive, various feeds can be handled (figure 6.67) and different product specifications met (see p. 145). If the projected operation is one of very high capacity, again the rotary atomizer is the favoured choice, although multi-nozzle arrangements operate successfully on filtered feeds. However, once faced with tens of tons feed per hour rotary atomizers offer substantial operational advantages. Of course, it need not be the feed and dried product properties that decide the issue. Where dryer rebuilding is planned either to increase capacity or handle different products, choice of atomizer is limited to that which fits the existing dryer chamber design. The chamber dimensions, position of exhaust air duct in relation to air disperser often decide the atomizer choice. The arguments for and against the choice of rotary and nozzle atomization are many and varied, but fortunately designs of atomizer have reached such sophistication to enable hundreds of products to be successfully spray dried (see chapter 13). 7 Spray-Air Contact (Mixing and Flow) 7.1. Introduction The prediction and control of spray—air movement within the spray drying chamber are important requirements for dryer design and performance. The manner in which the spray, on leaving the atomizer combines with the drying air determines the rate and extent of drying. The resulting spray—air movement determines the time each droplet remains in the chamber. Drying chamber and air disperser design must create a flow pattern, which prevents the deposition of partially dried product at the wall and on the atomizer. Wall deposits are caused by droplets travelling too rapidly to the wall, thereby not allowing sufficient drying time to elapse. Atomizer deposits result from local eddies. Eddies also cause re-entry of dried particles back into the hottest air regions of the dryer, and even into the air disperser where particles become scorched leading to contamination of the finished dried product. Much has still to be understood about how operating and design variables can best be combined to produce the spray—air movement for optimum drying conditions. The range of dryer designs and the unknown interdependence of the variables prevents a general relation being formed to express their combined effect on spray—air movement. General reviews of spray—air movement in spray dryers appear in the literature (1)(2)(35) (84)(85)(86)(87). Arising from such studies, fine sprays can be considered to move under the complete influence of the air flow throughout most of the dryer volume. Once small droplets have left the atomizer, they attain the velocity of the surrounding air in the proximity of the atomizer. How far droplets travel until fully influenced by the air flow depends upon the droplet size, shape and density. However, little data is available relating operating variables (air rate, feed rate, atomizer operation and location) to the distance 242 THE PROCESS STAGES OF SPRAY DRYING small droplets travel prior to attaining local air velocities. Coarse sprays are more independent of the air flow. Droplet/particle size, form and density determine product fall through the air. The amount of published data on spray—air movement is limited and is applicable mainly to small dryers. Air flow determination depends upon a suitable experimental technique, and few are considered successful. Any probing device automatically interferes with normal flow conditions, especially in small diameter dryers. Data for small diameter dryers have mostly been obtained from visual observations of light powder suspended in air streams. Powder movement was then considered representative of conditions existing during dryer operation. The common approach to droplet movement is to calculate droplet trajectory from the atomizer to the chamber wall using stepwise methods. Air flow data is required and this is either predicted or obtained experimentally in equipment having analogous flow characteristics. Air velocity measurements in pilot-plant size dryers have been conducted using anemometer methods. In industrial size dryers gas tracer techniques have been shown possible (88)(483) and holography appears a new method of the future. Spray—air movement is classified according to the dryer chamber layout, i.e. a 'co-current', `counter-current' or 'mixed flow' dryer with associated atomizer (see chapter 5). The designation of 'co-current flow', 'countercurrent flow' or 'mixed flow' to spray—air movement in a dryer is in fact not a true representation of actual conditions. For the case of a 'co-current flow' dryer with rotary atomizer (figure 5.2), the spray leaves the atomizer to be contacted obliquely by the entering drying air. Furthermore eddies within the drying chamber, around the air disperser, and at the walls create local areas of counter-current flow between spray and air. Spray—air movement is governed by air disperser location and design, atomizer location and operation, spray droplet behaviour when drying, chamber dimensions, and method of powder—air discharge. However, it is the air disperser that determines spray—air movement during the critical first period of droplet drying. Correct air dispersing stands out as an essential for obtaining a successful spray dryer operation. Air dispersers were introduced to the reader in chapter 5. Air dispersers are shown in figures 7.1-7.4. Figure 7.1 shows three arrangements in co-current flow dryers with rotary atomizers. Figure 7.3 shows arrangements for co-current flow nozzle dryers. In figure 7.1(a) the air enters directly above the atomizer wheel. The air flow is divided within the air disperser to give (a) rotational flow around the atomizer and (b) a local flow down around the wheel edge to depress the spray into an 'umbrella' cloud formation. This air disperser design gives a SPRAY—AIR CONTACT (MIXING AND FLOW) 243 HOT AIR I-tOT COOL AIR VANED APEX Figure 7.1. Air disperser for rotary atomizers. In co-current flow dryers. (a) Ceiling air disperser, volute inlet for hot air. Air rotation controlled by angled vanes. Spray pattern controlled by straightening cone. Rotary air flow in chamber. (b) Ceiling air disperser, volute inlet for hot air, Tangential inlet for hot/cool air around walls. Rotary air flow in chamber. (c) Central air disperser, air rotation controlled by angled vanes. Rotary air flow in chamber. good control over radial droplet trajectory, although precise adjustment of the air disperser vanes is required to prevent pronounced recirculation of air into the top corners of the chamber. An actual air disperser and atomizer are shown in figure 7.2. Alternative air disperser designs shown are (1) tangential air entry at the top corners of the chamber, giving high wall velocities (figure 7.1(b)), and (2) the entry of air vertically upwards underneath the wheel (figure 7.1(e)). Introduction of air under the atomizer wheel is particularly advantageous in drying operations involving very high inlet air temperatures, i.e. of the order 1400-1600°F (760-870°C). Hot air can be readily introduced into the drying chamber without resorting to refractory lined ductwork. The atomizer drive and chamber roof are also protected, as neither is directly exposed to the high air temperature. Atomizer cooling and roof construction of the drying chamber are simplified. The air disperser in figure 7.1(c) is a vaned apex placed on top of an air-cooled duct. The vanes create strong circulating air flow around the atomizer. The initial contact between air and spray can be co-contact (i.e. atomizer wheel and air rotation in the same direction) or counter-contact (rotations 244 SPRAY—AIR CONTACT (MIXING AND FLOW) THE PROCESS STAGES OF SPRAY DRYING 245 b. a. ROT AIR PERFORATED SHEET NOZZLE H11 1 11 H M I STRAIGHTENING VANES HOT AIR PERFORATED SHEET HOT AIR HOT AIR Figure 7.2. Ceiling air disperser (type (a) figure 7.1) with rotary (vaned wheel) atomizer in co-current flow dryer. in opposite direction). A more controlled air flow results from co-contacting, but the greater mixing created by counter-contact enables coarser sprays to be dried per given chamber size. Wall impingement of product often decreases, as counter-contact acts to further reduce the radial trajectory of spray. This increases fractionally the time the spray droplets remain suspended in the air flow, Such advantage is offset to a degree by the greater tendency for deposit formation on the surfaces of the atomizer. Air dispersers for co-current flow dryers with nozzle atomization create rotary or non-rotary air flow in drying chambers depending upon dryer design. Figure 7.3(a) shows four air dispersers creating rotary air flow. Type (i) is flexible for both nozzle and rotary atomizer use. Type (ii) is in two parts, where a central streamline flow promotes immediate contact between spray and hot air, prior to the spray coming under the full influence of the rotary air flow created by the other part. Type (iii) illustrates the use of wall entry of hot air. Type (iv) shows a plenum air disperser for horizontal (hox type) dryers. Each nozzle has its own hot air supply. Figure 7.3(b) represents three air dispersers creating parallel (streamline) flow. Perforated plates or straightening vanes are used. Air is dispersed over the entire cross-sectional area of the drying chamber, types (i) and (ii), or concentrated just around the PERFORATED SHEETS Ill RIAU/ t h0 Figure 7.3. Air disperser for nozzle atomizers in co-current flow dryers. (a) Creating rotary air flow in chamber; (i) ceiling air disperser, volute inlet for hot air. Air rotation controlled by angled vanes (vertical dryer); (ii) ceiling air disperser, (two-part) tangential entry to outer part. Streamline (Perforated plate) in inner part (vertical dryer); (iii) wall air disperser, tangential or volute inlet for hot air (vertical dryer); (iv) end wall air disperser, plenum inlet (swirl plate, horizontal dryer). (b) Creating parallel (streamline) air flow in chamber (vertical drye•); (i)perforated plate (over dryer cross-sectional area, vertical dryer); (ii) straightening vanes (over dryer cross-sectional area, vertical dryer); (iii) perforated roof (vertical dryer). 246 THE PROCESS STAGES OF SPRAY DRYING SPRAY—AIR CONTACT (MIXING AND FLOW) 247 HOT AIR (o ) NOT AIR (a) a, b. b. a, C. d. Figure 7,4. Air disperser for counter-current flow dryers. (a) Wall air disperser, tangential or volute inlet for hot air. (b) Central air disperser, angled vaned inlet for hot air, (c) Wall bustle (plenum) air disperser, angled vaned inlet for hot air (vertical vanes), (d) wall bustle (plenum) air disperser, angled vaned inlet for hot air (horizontal vanes). C. nozzle, as shown in the perforated roof disperser, type (iii). Dispersion of air around the nozzle(s) leads to faster drying rates and better utilization of the chamber volume. In type (iii) use of 4-5 perforated sheets can create plugflow conditions. The air pattern is controlled by the spacing of the sheets. Air dispersers for counter-current flow are shown in figure 7.4. Although tangential entry at wall (type (a)), and central dispersers (type (b)) are known, air dispersers of the bustle (plenum) type are generally used (types (c) and (d)). The bustle is located at the base of the cylindrical chamber section. Air enters with a rotary motion through angled inlet tuyeres, but this motion becomes depressed further up the chamber. Correct adjustment of the air disperser is necessary to prevent hot air by-passing droplet fall. With optimum spray—air contact, counter-current flow dryers give a most efficient utilization of heat available in the drying air. Air dispersers for mixed flow dryers are shown in figure 7.5. Ceiling or base dispersers are used depending upon the nozzle positioning. Type (a) shows the 'cyclone-type' dryer with tangential air inlet around a top- d, Figure 7.5. Air dispersers and atomizers in mixed flow dryers. (a) Wall air disperser, tangential or volute inlet for hot air (nozzle or cup atomizer). (b) Ceiling air disperser, volute inlet for hot air (nozzle atomizer). (c) Base central air disperser, tangential inlet for hot air (nozzle, wheel atomizer). (d) Base central air disperser, swirl vanes for inlet hot air (nozzle atomizer). mounted nozzle. Type (b) shows the 'fountain-type' dryer with a ceiling air disperser. Types (c) and (d) show base-mounted nozzle(s) surrounded by the air disperser. Specialized patented air disperser designs are covered in references (404) to (417). 7.2. General Principles The manner of spray—air flow characterizes the droplet population throughout the chamber and bears important relation to the evaporation rate of the spray, the optimum residence time of droplets in a hot atmosphere and the extent of wall deposit formation. 248 SPRAY—AIR CONTACT (MIXING AND FLOW) THE PROCESS STAGES OF SPRAY DRYING Whatever the mode of atomization, each droplet in the resulting spray is ejected at a velocity greatly in excess of the air velocities within the chamber. However, droplet kinetic energy is soon dissipated by air friction, and direct penetration is limited to short distances from the atomizer. In industrial sized dryers, wall deposits are rarely caused by direct throw of product to the wall, unless atomization has been incomplete. The droplets become influenced by the surrounding air flow, and movement is governed by the design of air disperser. Any attempt to calculate chamber dimension requirements is dependent on droplet path data and rate of drying. Droplet travel in cylindrical (vertical) spray dryers from the time of release from the atomizer to the point of contact with the chamber wall can be regarded as one- or two-dimensional motion from a nozzle atomizer operating in a non-rotary air flow, and as three-dimensional motion from a rotary atomizer operating in a rotary air flow. It is possible to derive theoretical correlations to represent droplet motion. The simplest correlations consider droplet mass and sphericity constant, but as droplet mass and shape change during passage through the dryer, actual travel is far from that predicted. Droplet motion under evaporating conditions must be considered by taking into account factors which affect droplet trajectory and heat and mass transfer. This leads to complex correlations. Certain assumptions to the spray drying process are made to render these correlations more workable. These include (a) heat transfer between droplet and air is by forced convection, (b) droplets constituting the spray are spherical, (c) spray is homogeneous, (d) the chance of coalescence and break-up of droplets during trajectory is disregarded, (e) for dryers with rotary air flow, the air proceeds through the dryer as a perfect cyclone (velocity is constant in the axial direction but varies in the tangeitial direction), (f) for dryers with non-rotary air flow the air proceeds through the dryer in parallel streamline flow. For droplets moving relative to air there is a resisting force due to friction between air and surface of the droplets (friction drag) and a drag force related to droplet shape. The resulting relative movement between droplet and air is dependent upon the variation in the resisting force and is controlled by the extent of change of the droplet's physical properties during evaporation. The basic principles of spray movement in spray dryers can be illustrated with reference to a single droplet. At any given instant of droplet travel in a vertical plane the forces acting on the droplet can be expressed as 6 2 = D3 (p — pPa)g )g — C D a V r e dt 6 2 droplet and air, A = area (= 70 2 /4 for spherical droplets), Vre , = droplet velocity relative to air. When gravitational forces and drag forces are equal droplet acceleration becomes zero and the droplet velocity is constant. The constant velocity is termed the terminal settling velocity. Under these conditions the total resisting force (F) can be expressed in terms of particle size, air density and drag coefficient 2 (7.2) F = 1CDPR(Vrei) A The value of the drag coefficient is dependent upon the droplet Reynolds Number (Re) = (DV p a I kt a) as shown in table 7.1. Table 7.1. Relation between Reynolds Number (Re) and Drag Coefficient (C D ) (For Spherical Droplets) Laminar (streamline) (St okian flow) Semi-turbulent (transitional flow) Turbulent Cp Re Flow region less than 0.2 24R e - from 0.2 to 500/1000 Approx : 0.4 + 40Re -1 greater than 1000 constant 0.44 The drag forces on droplets can be expressed over a wide range of velocities by using the fluid flow representation of plotting the droplet Reynolds Number (where droplet velocity is relative to air) and the dimensionless group (R' p a V 2 ). R' is the force per unit projected area of droplet in a plane 90 degrees to the droplet motion. The plot is shown in figure 7.6. From equation (7.2) (7.3) F = Ri A and ( R! 1 p y 2 ) = 2- CD (7.4) For complete treatment of droplet/particle movement in air, the reader is referred to Coulson and Richardson, Vol. 2, chapter 4 (89). Droplet/particle movement in turbulent flows is reported by Clift and Gativin (486). 73. Droplet Trajectory Characteristics dV D3 249 (7.1) where D = droplet diameter, C D =- drag coefficient, p w p a = densities of 7.3.1. From Rotary Atomizers (Atomizer Wheels) Droplet trajectory, following horizontal release from the atomizer is effected initially by the air swirl around the wheel (caused by wheel rotation) 250 SPRAY—AIR CONTACT (MIXING AND FLOW) THE PROCESS STAGES OF SPRAY DRYING drawn up by Herring and Marshall (37). Comparison between predicted trajectory and actual dryer performance suggested equation (7.7) to be a conservative estimate of droplet penetration. This was explained as the relation does not consider reduction in droplet density during evaporation or the effect of drying air flow. In equation (7.7) d is in, M is lb/min, N is rev/min. Of the three equations quoted equation (7.6) is generally preferred as it refers to maximum radial trajectory in still air conditions. 10 4 10 3 In 0 IN > Ec k. "k".. 251 10 2 10 10 0 Table 7.2. Spray Trajectory Relations for Rotary Atomizers 10 -2 I 10 -3 10 -2 10 -1 10 0 10 1 10 2 10 3 10 4 10 5 10 REYNOLDS NUMBER f Re i t 6 10 7 10 Author 8 10 Friedman, Gluckert, Marshall Reference (20) R 10 = 04 ( log scale 2 and finally by the drying air flow. In small test dryers, wheel rotation contributes greatly to the overall flow pattern and droplet trajectory in the chamber, but this is not so in industrial dryers as the influence of wheel rotation declines rapidly with radial distance. Air flow and droplet trajectory are governed primarily by the air disperser. The radial travel of droplets depends upon wheel design and speed, feed rate, air disperser design and location. The effect of the operating variables (atomizer dimensions, and speed, feed rate) on radial trajectory of sprays has been studied by various workers (20) (26) (28) (37). Results were expressed as the radial distance a given percentage of the spray travels while falling a given distance. Relations expressing radial trajectories are given in table 7.2. Maximum or near-maximum trajectory decreases with atomizer speed and increases with feed rate (other variables held constant). The relation by Friedman, Gluckert and Marshall (20) (where r is ft, M is lb/min and N is rev/min) was established from 26 experimental runs within the range of operating variables given in chapter 6, table 6.5. The effect of containing dryer walls was not considered. However, the relation was proposed as being useful in assessing the variations in trajectories when altering atomization conditions. The relation by Frazer, Eisenklam and Dombrowski (28) (where d is ft, M is lb/hr and N is rev/min) was established within a range of variables given in chapter 6, table 6.5. Arising from their work on droplet penetration, a cumulative weight distribution curve for water droplets at any radial distance 3 ft beneath the atomizer wheel was drawn up. Cumulative weight distribution curves were also dN.11.4 .O.25 2 Frazer, Eisenklam, Dombrowski (28) R. = 7.2d °.21 /14 N o•16 Herring, Marshall (37) R9 9 12e 2 J14 ° • N O. 16 Figure 7.6. Plot of R'IpV against Reynolds number for spherical particles. Equation number Equation (7,5) • (7.6) (7.7) Notation: d = wheel/disc diameter; M = feed rate, N = atomizer speed. Rio = radial distance in feet 50% of spray is thrown before falling 10 in below atomizer. R 99 = radial distance in feet, which includes 99 of the mass of the spray. Rmax = radial distance in feet at which 99 % of the spray falls 3 ft below the atomizer. For units and range of variables see table 6.5. 7.3.2. From Nozzle Atomizers Spray droplets on emerging from the nozzle swirl chamber and orifice are ejected forward with a high velocity component in the direction of the nozzle axis. Droplets from pressure nozzles decelerate rapidly. Droplets from pneumatic nozzles do not decelerate so rapidly as the droplets are carried forward in the dispersing atomizing air flow. With small droplets, radial velocity component on release is low, and spray trajectory to the wall is limited. This enables drying towers of a narrow diameter to be used with nozzle atomization. 7.4. Droplet Movement in Drying Chambers Droplet movement in the drying chamber consists of (1) droplet release from the atomizer, (2) droplet deceleration and (3) free falling motion or motion under the influence of the drying air flow in the chamber. 7.4.1. Droplet Release Velocity Droplet release from rotary and nozzle atomizers is described in chapter 6. 252 THE PROCESS STAGES OF SPRAY DRYING SPRAY-AIR CONTACT (MIXING AND 7.4.2. Droplet Deceleration Droplets leaving an atomizer at velocities in excess of the surrounding air decelerate rapidly due to frictional forces acting on the droplet surfaces. The rate of deceleration determines the penetration of droplets through the air surrounding the atomizer. Giffen and Muraszew (18) drew up deceleration equations for single droplets, discharged into still air conditions where gravity is neglected. Once the droplet has been discharged from the atomizer, the droplet velocity decreases, and the droplet passes first through a turbulent, then a semi-turbulent to a laminar flow region. If the droplet diameter is large, a laminar flow might not be experienced due to a high terminal velocity. Deceleration in each flow region is given by dV = dt 18y a Laminar flow (7.8a) dV = 0.3pa 2 30p a v dt Dp, V D 2 pw Semi-turbulent flow (7.8b) dV dt Turbulent flow (7.8c) D2 pw _ Dp w Calculation of droplet motion during deceleration requires use of the relation 2 between the droplet Reynolds number and the dimensionless group R' /p a V , see figure 7.6. Time and distance travelled by droplet during deceleration is obtained by integration of equations (7.9) and (7.10). (b) Droplet Deceleration from Nozzle Atomizers For a droplet discharged from nozzle atomizers, whether in the upward or downward direction, equation (7.10) can be used to develop the droplet motion in the vertical plane. The cone angle will give a horizontal velocity component, and motion in this direction is given by equation (7.9). If spray discharge is upwards, both gravity and air frictional forces act together in retarding the motion of the droplet in the vertical plane until the droplet is brought to rest. Once the droplet begins to fall, gravity and air frictional forces are in opposition. For nozzles of small cone angle, movement of all particles is prominently in the vertical plane, and droplet motion can be considered one-dimensional in a gravitational field. For a droplet moving downward in one-dimensional motion, equation (7.10) can be rewritten d in Integration of equations (7.8a, b, c) yield the deceleration time and droplet penetration during each flow region. The above equations are often quoted but they have limited practical use, owing to the simple system they describe. More precise methods (though still having important practical limitations) are available to describe droplet deceleration from rotary to nozzle atomizers. (a) Droplet Deceleration from Rotary Atomizers For a droplet leaving the edge of a rotary atomizer, the deceleration can be expressed as equations of motion in the horizontal and vertical planes. For the case of horizontal droplet release at a velocity Uh from the wheel/ disc edge, gravity acts immediately on the droplet giving a vertical velocity component U. The forces acting on the droplet are the apparent weight of the droplet mg(1 p a/p w ) and the drag force R'A. Equations of motion in the horizontal direction become dUh = dt Pa V2 p aAU h (U )2; + UD1 I 2 (7.9) Equation of motion in the vertical direction dU, — dt R' p a T7 p a U,(U t2, + UD112 + mg(1 Pa Pw ) (7.10) FLOW) 253 Ri Uv C ..- — A) 2 Ap a U + mg (1 — Pw dt pa V v (7.11) for spherical droplets, equation (7.11) becomes [1.5pa R. ' U„ Pa 1 + g ( 1 — —) 2 U. Dp w dt = pa V Pw (7.12) Integration of equation (7.12) yields the deceleration time of droplet travel. By substituting U., = Rega/Dp a in equation (7.12) R' 11.5p a \ I Re 2 14\ 14, d(Re) = DPa dt 2 2 p a V k Dp„ \ D P! 1 +g Pwi (7.13) Re-arranging and integrating R t= " FDpa(N Pa)g fRei L Pat). 1tt a l R' g Re D 2 p w kp a V 2 dRe (7.14) Lapple and Shepherd (90) expressed equation (7.11) in terms of the drag 2 coefficient (C D ) using equation (7.4) [C D = 2(re /p a V )]. Equation (7.11) can be written in terms of CD and droplet mass. dU, dt p a C D Aq + g p, — Pa k 2m P. (7.15) 254 THE PROCESS STAGES OF SPRAY DRYING By expressing U, in terms of Reynolds number, equation (7.15) becomes P. A dt = ( dRe - C D Re 2 ) (7.16) 2Dm (/) is the maximum value of C D Re 2 which a droplet of size D can attain when falling freely. For spherical particles at terminal velocity 4 g =3 /4 Integration of equation (7.17) gives /t a il t 2Dm 255 Values of K for values of Z between 0-1.0 vary from unity at laminar flow conditions, to 0.5 at extremely turbulent conditions. For conditions likely to occur in the spray drying operation, K values will range from 0.8-1.0. Some typical K values are given in table 7.3 for values of Z less than unity. A complete list of values is given elsewhere (90). SPRAY-AIR CONTACT (MIXING AND FLOW) Pa(Pw Pa)D3 Table 7.3. Values of K Factor Values of K for following values of 0 (7.17) R 2 e f (4) - C Re 2 ) -1 dRe D where Re l. , Re x is droplet Reynolds number on release from atomizer and after time t. Equation (7.18) is an easier form of equation (7.14) to apply. For laminar flow region (C D = 24Re -1 ) equation (7.18) becomes upon integration (for spherical droplets) t= p s D 2 17, V„\ (7.19) 18p a 17f. - it aA t = 3 p a t = [(4) / + Re 2 C D1- / 2 )(41 I / 2 In (01/2 R e2 c1/2)(01/2 2Dm 4D2pw 2(CDO) 1/2 Re C p a A. 2Dm t 3p t K 4D 2p w - CDRe 1- 1 04 0 1.00 0.98 0.90 1.00 0.96 0.83 1.00 0.95 0.76 Calculate the time to decelerate a spherical 200 micron (6.5 x 10 -4 ft) droplet sprayed down a dryer tower from a nozzle at 300 ft/sec. A nonrotating air flow exists down the tower. Assume droplet density and diameter undergoes no appreciable change during deceleration. Data: p w = 62.3 lb/ft' p a = 0.068 lb/ft' = 1.3 x 10 -5 lb/ft sec 112 R ei c1:12) (7.20) Equation (7.20) can be applied to droplet discharge from a nozzle at high velocity. To enable use of equation (7.18) over the entire droplet velocity range, Lapple and Shepherd (90) introduced a factor K that enables direct calculation of the velocity-time relation in the semi-turbulent flow region. Equation (7.18) written in terms of the factor K becomes : 2. In (1 - Z 1 \ 10 3 EXAMPLE 7.1 where V is the droplet velocity after time t, and Vt is the terminal velocity. For the turbulent flow region, CD = constant (0.44). Equation (7.18) becomes 1 2 10 2 0.5 1.0 (7.18) R e1 Z2 (7.21) Subscripts 1, 2 indicate initial and final conditions. CD, Re, are values at final condition, and C Z = [Re(1 ) 11 1 Z2 represents a measure of the fractional approach to terminal velocity. Reynolds number of droplet on release from nozzle = 1020. Consider droplet motion to be in turbulent region until Re = 500 or V = 147 ft/sec. Motion in Turbulent Region CD = 0.44 Use the equation (7.20) to calculate time to reach 147 ft/sec = 290 (calculated from equation (7.17) using above data) Deceleration time in turbulent flow region is given by equation (7.20) t 4(6.5 x 10 -4 ) 2 62.3 In A 2(0.44 x 290) 1 / 2 x 3(1.3 x 10-5) where 2 A= [290) 1 / 2 + 500(0.44) 1 / 2 (290) 1 / 2 - 1020(0.44) 1 / 1 2 1 2 x (290) / - 500(0.44) / (290) 1 / 2 + 1020(0.44) 1 / 2 ] t = 7.5 x 10 -3 sec (negligible) 256 THE PROCESS STAGES OF SPRAY DRYING SPRAY—AIR CONTACT (MIXING AND FLOW) o Terminal velocity conditions can be shown to be in the semi-turbulent flow 2 region (0.2 < Re < 500). Now 0 = maximum value of C D Re at terminal velocity conditions. From graph of C D Re 2 against Re (figure 7.7). Re = 7.2 (semi-turbulent region). I U Motion in the Semi-Turbulent Region Time of travel is given by equation (7.21). Value of Z, (at Re = 500) CD = 0.48 (from table 7.1). Now 257 4 1 01 3X Z = Re(C,10) 112 = 500(0.48/290) 1 / 2 = 20.4 DRAG COEFFMIENT - ( REYNOLDS Zi = 414 Value of Z2 Re = 7.2 = (290/C D ) 112 Therefore CD = 545 5.45) 1/2 Z2 = = 0.986 290 7.2 10 0.972 Value of K is obtained from table 7.3. At Zz = 0.972 (0 = 290) K t = 0.9 10 1 4(6.5 x 10 -.4 ) 2 62.3i 0.9 ) ln ( 1 — 414 3(1.3 x 10 -5 ) 1(5.45)(7.2) 1 — 0.972) = 5 x 10 -1 sec Deceleration time to terminal velocity I sec le 7.4.3. Terminal Velocity (Spherical Droplets) Terminal velocity conditions occur when the force of gravity acting on the droplet is counter-balanced by the air frictional forces. The left-hand side of equation (7.1) becomes zero, and equating the two forces Tc 6 1 7 D2 2 D 3 (P,,, P a)g = — CDPa( 4 )V (7.22) REYNOLDS NUMBER 4 Vf = [ (Pw Pa)gpi 3 C Dp a ( Re ) 2 Figure 7.7. Piot of C 0 Re against Re for spherical particles, air friction (drag) forces (F) can be expressed : F = 3ny a DT/f 2 The terminal velocity Tif is expressed by 10 1 (7.24) The terminal velocity in terms of measurable variables ll2 (7.23) When values of yr correspond to a droplet Reynolds number less than 0.2, V 2 9 = D 6 , — Pa) 181.ta (7.25) When droplet motion at terminal velocity corresponds to a Reynolds number 258 THE PROCESS STAGES OF SPRAY DRYING SPRAY-AIR CONTACT (MIXING AND FLOW) or within the range 0.2-500, the air frictional (drag) forces (F) equal (357) F = 37Ipa DV(1 + 0.15Re ° 87 ) (7.26) Droplets formed during spray drying rarely feature sizes and densities to give terminal velocity at high Reynolds numbers. Terminal velocities can well be within the semi-turbulent flow region, in which case equation (7.27) (in f.p.s. units) may be applied (91). V= 0.153D 1 ' 14 g" i (p, 0900.290100.4 (7. 27) Terminal velocities of droplets in spray drying chambers deviate from those in the ideal conditions assumed above. Deviation from ideal conditions occurs through : (a) Interference Between Droplets and Between Droplet and Chamber Wall Effects Droplet Motion. Air movement associated with the presence of a large number of droplets discharged from an atomizer over extended time intervals differs from air movement surrounding a single droplet. The leading droplet of a spray gives energy to the surrounding air. The resulting forward air movement reduces the air resistance acting on following droplet. The overall effect is to create greater droplet penetration from the atomizer. (b) Droplets are Liquid therefore not Rigid. Liquid droplets are subjected to deformation due to various pressures acting over the surface, and internal circulation of liquid within the droplet. Deformations cause increase in the drag force, while internal circulation can act to reduce the drag by reducing the velocity gradient at the droplet surface. (c) Droplets are often not Spherical. Deviation's from sphericity can be allowed for by incorporating a shape factor. The shape factor is defined as the ratio of diameter - of sphere having the same volume to the diameter of sphere having the same surface area For spray dried powders having a high proportion of spheres (i.e. ceramics) the shape factor approaches 0.95. For majority of powders where shapes tend to be spherical and not elongated, the shape factor ranges between 0.5 and 0.85. The shape factor must be estimated from microscopic droplet analysis. (d) Droplets change Shape during Drying and can change from Solid -io Porous and Hollow Forms. If droplet drying is rapid, hollow spheres can be formed prior to the establishment of terminal velocity conditions. In applying the terminal velocity equation, correction to the particle density must be carried out. The density of a hollow particle is given by surface area x wall thickness (b,,) x wall density particle volume 259 PD 7I D2Pwanbw — _k n.)) 3 (7.28) D (p 0 replaces p w in equation (7.25) for particle travel at terminal velocity.) Prediction of Terminal Velocity when Drag Coefficients are Unknown In cases where droplet sizes are large enough to produce a terminal velocity outside laminar flow conditions, terminal velocities are best determined graphically. Solving for the drag coefficient in equation (7.23) and expressing in logarithmic form log C D = log ( 4g(P 3w—aPa) D) — 2 log Vf Pa (7.29) Expressing the Reynolds number at terminal velocity in logarithmic form Dpa log Re = log /La + log Vf (7.30) Eliminate Vf from (7.29) and (7.30) log CD 2log Re + log [4gD 3 p a (p, — p a )] 3 /4 (7.31) Equation (7.31) gives a straight-line equation of slope 2. Passing through Re = 1, therefore CD — (4gD 3 p a(p, — p a)) (7.32) A similar expression can be obtained wlire droplet size , D does not appear in the second term of the right-hand side of ±quation (7.31). By substituting in iRettar D3= Pe Vf and separating equation (7.31) becomes 469‘, log CD = log Re + log ( POtta) 3p17,31. (7.33) Hence to calculate Vf where CD is unknown, equation (7.33) is plotted on a CD—Re plot (figure 7.8). The terminal velocity is calculated from the point of intersection of the two curves. THE PROCESS STAGES OF SPRAY DRYING SPRAY-AIR CONTACT (MIXING AND FLOW) 261 EXAMPLE 7.2 In a counter-current flow spray dryer with a nozzle spraying down the chamber, a coarse particle size is being produced. All particles above 200 micron are to fall to the chamber base for direct product discharge. What is the maximum velocity of drying air up the dryer to obtain this size separation? Data: Particle size 200 micron = 6.5 x 10 -4 ft Average air temperature over the majority of dryer height = 176°F (80°C). o Figure 7.8. Plot of drag coefficient against Reynolds number. 260 Air viscosity = = 1.4 x 10 -5 lb/ft sec. Air density = (p a ) = 6.26 x 10 -2 lb/ft 3 . Particle density = (PD) = 63.8 lb/ft 3 . Air velocity must not exceed the particle terminal falling velocity. Using equation (7.32) (Pr) CD 4 x 32.2(6.5 x 10 -4 ) 3 (6.26 x 10 -2 )(63.8 - 0.0626) 3(1.4 x 10 -5 ) 2 = 246.4 Referring to figure 7.8. At C D = 246.4 and Re = 1 draw line of slope - 2. At intersection with the ' a— Re curve, the Reynolds number = 6.6 (semi-turbulent motion). Theret ore Re = 6.6 = Dp aV f ha -5 V f IN3f1333(n DYHO = 6.6(1.4 x 10 ) = 2.36 ft/sec (6.56 x 10 -4 )(6.26 x 10 -2 ) The air velocity must be less than Vf . 7.4.4. Droplet Movement: Distance-Time Relationships Distance-time relationships can be drawn up for droplet travel. in one- or two-dimensional motion using equations (7.9) and (7.10) where droplet velocities are relative to the air. (a) Droplet Movement in Non-rotating Air (i) Motion from Rotary Atomizers. Two-dimensional motion results from droplets released from the edge of a rotating wheel. The release velocity is sufficient to produce initial droplet motion in the turbulent flow region. Under these conditions the distance-time relation in the horizontal plane is expressed by Coulson and Richardson (89). 262 SPRAY—AIR CONTACT (MIXING AND FLOW) 263 THE PROCESS STAGES OF SPRAY DRYING Sh = 1 1n ( Uh ct + 1) (7.34) where Sh = distance travelled in horizontal direction, and c= 0.33p a/Dp w . When droplet enters the semi-turbulent region, no simple function 2 between Reynolds number and the dimensionless group (IV/p a V ) exists in this range and the distance travelled in the horizontal plane is calculated by graphical integration techniques. Equation (7.9) can be written, neglecting the effect of gravity and resultant velocity component in the vertical plane m d Uh R' = Pa y R' x — dt = pay' P 1 8pat \ D 2 p, (7.40) ( 1 —* 0 13 2 p w therefore Sh(max) D 2 p„Uh 18pa (7.41) d Uh = T18/1, dt Uh D2p, (7.42) integrating : (7.37) Dp w By definition : Uh = Re(p./DP a ) = dsldt and by substitution into equation (7.36) and subsequently integrating, a relation is obtained between t and Re. 3 18 exp (7.36) ) dU h ^ 3 x C D p a U il 2D 2 p, 1' 2 exp ( The maximum radial distance is attained when h In terms of the drag coefficient dt 18 m,, D 2 pw(1 The droplet velocity during streamline flow is represented by substituting CD = 24/Re into equation (7.37). 1.5p a — Dp, Uh Sh (7.35) , Ap a U? which, for the case of a spherical droplet dU h Once droplet motion lies within the laminar flow region droplet travel in the horizontal direction is given directly by (42) 1 dRe (R ! PaV2)(Re)2 (7.39) Values of Uh can be determined, and by further graphical integration the droplet travel in the horizontal direction obtained in terms of t.- Graphical integration is a time-consuming operation, and often it is avoided through neglecting time of droplet travel in the semi-turbulent region. This is considered valid for small droplet sizes, which undergo virtually instantaneous deceleration, and time intervals in this region are extremely short. Where time and distance of travel in the semi-turbulent region can be significant, e.g. for large droplet systems, the time increment method by Lapple and Shepherd (90) based on equation (7.37) is the most manageable. 18 at ± constant (C) D 2 p, (7.43) at t = 0, C = log Ue where U e is the droplet velocity entering the laminar region. Hence Uh = U. exp ( (7.38) Equation (7.38) is integrated graphically between the limits to obtain t as a 12 function of Re, where values of (K/p a I ) can be calculated from (357) ( R' ° 687 = 12Re -1 (1 + 0.15Re) ' 2 PaY log Uh = 18p t (7.44) 2 D pw Droplet travel in the vertical direction is negligible in the turbulent and semi-turbulent flow regions. With no vertical velocity component imparted upon the droplet on release, vertical travel will be within the laminar flow region. Distance travelled (S y) in the vertical direction can be expressed (89) Sv = bt a U,, a b b + 2 a a UV \ a) —at (7.45) where U,, is velocity entering the laminar flow region. In this case U„ = 0; a = 1812 a/D 2 p.„,; b = g(1 — p al l%) The velocity relation at any given time is obtained by integrating equation (7.15) following substitution of CD = 24/Re. For the case of a spray drying operation p, » p a . Hence dU,=g dt (18paUvl pD2 (7.46) 264 THE PROCESS STAGES OF SPRAY DRYING SPRAY-AIR CONTACT (MIXING AND FLOW) On integration using the integration factor J 1811 p‘vD 22 and introducing the values a, b, as defined above : Elv = b + j, a k 17\ a (7.47) Distance-Time Relationships by the Method of Lapple and Shepherd (90) The difficulty in dealing with the semi-turbulent region in the above analysis can be overcome by the method of Lapple and Shepherd. This involves calculating travel in small selected time intervals using corresponding values of the drag coefficient to express the flow region characteristics. The calculation is based upon equations (7.9) and (7.10) expressed in terms of the drag coefficient. [3pa C D U U h ] dt 4p, D (7.48) (p„, - P a) 3p„CDUU,1 dt dU, =[g 4p,„D Pw (7.49) dU h = 2 where U is the resultant velocity (U ii + UD 1 / . The method is as follows : (i) A time increment is selected. (ii) The droplet release velocity from the atomizer is calculated. Using this velocity, the droplet Reynolds number is determined, and by referring to figure 7.8 the corresponding value of the drag coefficient (C D ) is obtained, (iii) The value of C D is substituted in equations (7.48) and (7.49) (dU h )(dU,) are then computed, where for the initial time increment U = Uh , U, = a (iv) Using the values of (dU h )(dU,) calculated in step 3, a velocity is estimated at the end of the time increment. (v) Values of (dUh ) and (dU,) are re-calculated using velocity conditions at the end of the time interval. (vi) Values of (dU h ) and (dU,) calculated for conditions at the commencement and termination of the time increment are then averaged. The average value is used to obtain the second estimation of the droplet velocity at the end of the time increment. The procedure is repeated until the calculated average velocity increments (dU h )(dU,)correspond to those used in determining the velocity at the end of the time increment. (vii) Movement in the next time increment is considered and the above procedure is repeated where the velocities at the end of the first time increment is used as the initial velocities in the next time increment. 265 (viii) Calculations continue until velocities are reduced to terminal velocity values. The velocity-time relationship is thus calculated. (ix) The distance-time relationship is finally calculated by graphical integration where s u dt. An excessive number of trial and error approximations are required to compute maximum radial distances using the above method. The procedure can be simplified by using direct relationships (equations (7.40)-(7.47)) between droplet velocity and time in the later stages of droplet motion within the laminar flow region, Deceleration of small droplets is very rapid and velocities in the laminar region are obtained for many droplets after fractions of a second. The number of trial and error approximations is restricted to dealing only with the first 0-010-0.02 sec of motion. This is illustrated in example 7.3. Villadsen (92) has illustrated the Lapple and Shepherd method for a droplet of 109 micron diameter. Rapid deceleration is again illustrated. For a release velocity of 440 ft/sec (132 m/sec), the velocity in the horizontal direction reduces to 25.5 ft/sec (7.8 m/sec) in 0.04 seconds, during which time the droplet gains a vertical velocity of 0.23 ft/sec (0.07 m/sec). EXAMPLE 7.3 Calculate the droplet trajectory over the first 0.04 seconds of a 60 micron (1.97 x 10 -4 ft) droplet leaving a rotary atomizer. The wheel peripheral velocity is 350 ft/sec. Consider the droplet aqueous, and the air viscosity 1.3 x 10 -5 lb/ft sec. To apply the Lapple and Shepherd method, still air conditions are assumed. Data: Droplet release velocity = 350 ft/sec Therefore 10 4 )(0-067) Reynolds number = (1.97 x U = 1.02U. (1.3 x 10-) Substituting data in equations (7.48) and (7.49) Uh r3x 0.067 CDUUh L4 x 62.3(1.97 x 10-4) At (a) = 4.1CD UUh At AU = [ 32.2 62.3 --0.067 \ 62.3 = [32.2 - 4.1C D UUJAt At U h = 350 ft/sec, U„ = 0. 3 x 0.067C D U tiv 4 x 62.3(1.97 x 10-4) At (b) 266 THE PROCESS STAGES OF SPRAY DRYING SPRAY AIR CONTACT (MIXING AND FLOW) Motion in the horizontal direction 267 Re = 1.02 x 350 = 356 Now 0.016 0 0.0143, i.e. estimation not correct. Let U. = 0.013, UU, = 3.0, CD = 0.74 CD = 0.62 (from figure 7.8) AU, = (32.2 - 41 x 0.74 x 3)0.0005 = 0.0115 ft/sec U = Uh as Average increment U, = 0 Selected time increment (At) = 0.0005 sec. Substitute data in equation (a) to calculate velocity increment AU h . 0.0115 + 0.0160 - 00135 2 AU, = -4.1 x 0.62 x 350 2 x 0.0005 = -156 ft/sec 0.0130 0.0135, therefore estimation of correct order. Proceed to next increment. Variation of U h with t, and U,, with t are plotted. Areas under the curves give the distance travelled. Results are tabulated in table 7.4. Accuracy of results depends on the closeness of the velocity estimations. Estimate velocity at end of time increment. Suppose Uh after 0.0005 sec is 200 ft/sec, Re = 205C, = 0.77 substitute in equation (a), AU, = 4.1 x 0.77 x 200 2 x 0.0005 63 ft/sec Average velocity increment (156 -4- 63) AU h = - 109 Table 7.4. Theoretical Droplet Trajectories in Example 7.3 (from rotatory atomizer) 2 now 350 - 109 = 241. However 241 0 200, i.e. estimation not correct. Suppose U, = 230 ft/sec after 00005 sec. Re = 235, A Uh = U = Uh = 230 CD = 0-74, 2 - 4-1 x 0.73 x 230 x 0.0005 = - 80 ft/sec Average increment - (156 + 80) = 2 - 118 Now 350 - 118 = 232, 232 230, therefore estimation of correct order. For the next time increment, Uh = 230 ft/sec, At = 0.0005 sec. Repeat above procedure. Motion in the vertical direction At t = 0, U, = 0. Therefore to calculate U, after 0.0005 sec, substitute in equation (b) U, = 32.2 x 0.0005 = 0.016 ft/sec Let U, = 0.01, UU, = 230 x 0.01 = 2.3, CD = 0-74. Therefore U„ = (32.2 - 4.1 x 0.74 x 2.3)0.0005 = 0.0126 ft/sec Average increment 0-016 + 0-0126 - 0-0143 ft/sec 2 Droplet velocity (ft/sec) Distance travelled (ft) Time (sec) Horizontal Vertical Horizontal 0 0.0005 350 230 0 0.013 0 0.15 0 0.001 165 0.045 0.27 - 0002 0.004 0.006 90 50 30 0.085 0.120 0.146 043 057 0.65 00001 0.0003 00006 0-008 0.010 0.012 0.014 , 20 15 11.5 8.8 0.168 0.185 0.200 0.214 0.71 0.76 0.79 081 0.0009 0-0012 0.0016 0.0020 Vertical . Example 7.3 exemplifies the rapid deceleration of a droplet after release from the atomizer. In 0.014 seconds the horizontal droplet velocity decreases to 8.8 ft/sec (2.7 m/sec). The radial distance of travel is less than one foot. The velocity gained in the vertical direction and the distance travelled is seen in table 7.4 to be negligible during this period. (ii) Motion from Nozzle Atomizers Nozzle point upward. For spray ejection upwards into a spray drying chamber, the droplet velocities from the nozzle are sufficient for the larger droplet sizes in the nozzle spray to be in turbulent motion. For the basic case of one-dimensional motion in a gravitation field (air flow has no rotation) droplet motion from the nozzle is expressed by Coulson and 268 SPRAY-AIR CONTACT (MIXING AND FLOW) THE PROCESS STAGES OF SPRAY DRYING Richardson (89) as 1 S, = -- In (cos f ct c U, — sin f et) f (7.50) (in consistent units). Where U,, = velocity of droplet leaving nozzle, and = ( D(p, p a)4 112 0.33p a (7.51) Deceleration of the droplet takes place and when the droplet is in semiturbulent motion, time can be expressed in terms of the Reynolds number as R eg [ ( Dpa(p p jg) Re y + ( 3-112 ' x (7.52) t 2D p, paUZ v The Reynolds number is a function of t from which the vertical velocity can be obtained. By further graphical integration the distance moved for a required time interval is calculated. Deceleration continues until the droplet experiences laminar flow. Form drag is negligible and the droplet is brought to rest due to skin friction forces only. While the droplet comes to rest and then accelerates within laminar conditions the distance-time relation (irrespective of sense) is given by equation (7.45). As the droplet accelerates within semi-turbulent conditions the distance ti me relationship form is similar to equation (7.52) except for a change of sign. If the droplet is still large and heavy enough (even though evaporation reduces weight during motion), to reach turbulent conditions, motion is given by 1 S, rt + - 1n — f + u, + (f ' u„) e -21- 1 c 2f ' { (7.53) One-dimensional motion in the vertical plane occurs in nozzle drying towers incorporating non-rotary air flow. Equations (7.50)-(7.53) are used for the case of nozzle placed to face up the drying tower. Nozzle pointing downward. For nozzles placed at the top of the dryer, equations (7.52)-(7.53) express the downward motion. The equation is selected according to the droplet Reynolds number. All velocity values used in the equations are relative to the surrounding drying air velocity. To calculate both vertical and radial movement (due to droplets leaving nozzle with a radial velocity component fixed by the nozzle spray angle), the Lapple and Shepherd (90) method can be used (equations (7.48) and (7.49)). Example 7.4 illustrates use of the Lapple and Shepherd method in calculating droplet trajectories from a nozzle atomizer. Movement in the vertical 269 direction is more substantial as the droplet leaves the nozzle with a high axial release velocity. Results are presented in table 7.5 which gives the time the chosen droplet size takes to complete its radial travel. EXAMPLE 7.4 A co-current nozzle tower 8 ft 6 in diameter and 16 ft 5 in cylindrical height is to be adopted for.the spray drying of a slurry. A coarse particle size is required and a centrifugal nozzle has been' selected. At the required feed rate of 2.35 US gal/min, the cone angle is 90°. The largest droplet size formed in the nozzle spray is estimated not greater than 500 micron. Assuming that the drying air flow is non-rotary and of very low velocity and any particle shape change that might occur is negligible, predict whether direct i mpingement of clay slurry on the wall of the dryer will result with the given nozzle. Data: The initial vertical velocity of the spray droplets follows the relation (57) = 4.07 x 10 -1 Q da ft/sec Q = feed rate (US gal min), d, = orifice diameter (in), density of air (p a ) = 3 0.0523 lb/ft', density of slurry (p,„) = 93.5 lb/ft , air viscosity CUa) = 1.546 x -5 10 lb/ft se; nozzle orifice diameter = 0.138 in. The chance of impingement at the wall is best considered by calculating trajectories at conditions of greatest droplet travel, i.e. no reduction in droplet density. Procedure : Diameter of largest droplet 500 micron = 0.00164 ft, initial droplet velocity in the vertical direction (V,), (from given relation) V, 50 ft/sec, nozzle cone angle = 90°, initial droplet velocity in the horizontal direction = 50 tan 90/2 = 50 ft/sec. For motion in the horizontal direction Substitution of data in equation (7.48) ❑ U h = -0.256C D UU hAt For motion in the vertical direction (equation (7.49)) AU, = [32.2 - 0.256C,UU h ]At The Reynolds number 5.55 U where LP = LIZ + U, 2 Values of CD obtained for values of Re from figure 7.8. Applying the Lapple and Shepherd method: For time intervals of 0.01 sec, adopting trial and error procedures as illustrated in example 7.3, U h decreases to 44.3 ft/sec (13.5 m/sec) and U, 270 SPRAY—AIR CONTACT (MIXING AND now) 271 THE PROCESS STAGES OF SPRAY DRYING try rn r- rr- r4, C4 Ch t■ 4D 47 et 00 C.A Ch CD DO 00 C7 qp ma et N Q CR t- 4O VI et 1-1 VI r■ DO 47 CD er r- CN aet et 'Noo0" Cp et ,t rn vD 00 C C vp N 00 00 Do on 00 00 0' CD CD CD 6 .4 6 CD ,4 CD CD C5 C7 6 c5 c5 c5 6a '' 1" 0 "..0 un Ch Ch Ch CD m- N N CD N rn 4 , r DO N o0 c!N N vn eh (:!r N u? VD N N DO 00 00 DO 6 6 T... *4 N 0.1 4 41 vn v5 VD vb v5 v5 v5 v5 v5 4D j 4 .5? 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C4 , 00 0 Ô-000 c5 o CD CD 6 CD 6 C7 T, 4 decreases to 44.6 ft/sec (13.6 m/sec). The droplet travel is given in table 7.5 covering the entire trajectory until radial travel ceases. After 1.2 sec the maximum outward travel is reached, namely 6.84 ft (2.1 m). Downward travel during this period is 14.5 ft (4.3 m). Considering that evaporation of moisture from the droplet during the actual drying process will act to reduce trajectory distances, the dryer dimensions are concluded large enough to prevent direct impingement of the spray cloud on the dryer wall. (b) Droplet Movement in Rotating Air (Spiral Air Flow) (Droplet in a Centrifugal Field) The above analysis and worked examples show droplet movement to be very small during deceleration from any atomizer. Droplet path of travel can be considered to be that of the air flow pattern in the chamber. If a spiral air flow is created by the air disperser, droplets will travel as if they were in a centrifugal field. The general equations for a droplet moving in a rotating air flow is given by (90) dU i. dt dU, dt t11\ 2 r cr a lq \ -1 ip a C D AU f U r \ 2m U ,U,\ • [P.CDAUPt — Ut)] 2m r (7.54) (7.55) where U rdroplet velocity in the radial direction, U, = droplet velocity in velocity relative to air, li t = air = the tangential direction, Uf droplet droplet mass. m --velocity in the tangential direction, It has been shown that if a rotating vaned (i) Large Chamber Diameters. atomizer wheel is used in conjunction with a rotating (spiral) air flow pattern, spray droplets become fully influenced by the air flow in less than six wheel diameters from the atomizer edge (38). For large chambers, local flow effects around the wheel (caused by pumping effect of the wheel) on droplet travel can be disregarded. Droplet motion in dryer designs having diameters greater than six wheel diameters (i.e. all models above laboratory size) can be simplified to a consideration of droplet retention in a fully formed rotating (spiral) flow. The time for a droplet of given size to travel radially to the chamber wall under the influence of centrifugal forces can be calculated. Equations (7.54) and (7.55) can be simplified for the case of spherical droplets and laminar flow conditions. As the spiral air flow is the governing influence on droplet travel during the greater part of the droplet residence time in the drying chamber, motion 272 THE PROCESS STAGES OP SPRAY DRYING SPRAY—AIR CONTACT (MIXING AND FLOW) for a spherical droplet can be represented as (90) dU r dr — WIF r dU, dt ,U Pa w IL ;X fq.)1 2 U, [181.1a (V, U r) D 2 p v, r [18,12.a U r] 2 (3,1) (7.56) (7.57) for movement in the radial and tangential directions. Since droplet travel becomes rapidly influenced by the air pattern, droplet tangential velocity ( U t ) approximates to air tangential velocity component (14). For droplet travel in chambers larger than pilot-size models, the droplet radial velocity is small due to the more extensive chamber diameters used and the mode of air disperser selected. A further simplification can be made by neglecting the tangential and radial acceleration. Droplet radial velocity reduces to ur = V 2 69 , — POD 2 ' 18 P a r (7.58) Equation (7.58) is the form of Stokes' Law for constant settling rate conditions in a centrifugal field. The tangential velocity (14) is dependent upon chamber size and air disperser design. V is normally estimated. Data from an experimental determination of the air pattern is rarely available, but Edeling (93) has proposed the approximate relation for tangential velocity in a chamber with rotating air flow. )0.5 (7.59) Y= Vt(wall)( — R c The time (At) for radial travel between two points r„ r 2 can be deduced from the radial and tangential. components. Now U, = dr/dt, V = Substituting in equation (7.58) and integrating, the resulting correlation is t= 18kt a in (r,/r,) D 20) 2 (Pw — Pa) (7.60) where o) = average angular velocity. The subscripts 1 and 2 refer to initial and final conditions so that r 1 and r2 are the distances of the droplets from the centre of rotation at given times. When applying equation (7.60) radial increments (r 2 r 1 ) must be small to avoid errors in co. Application of equations (7.58) and (7.60) represents the theoretical case. Although calculated values provide valuable information for estimating trajectory paths and times, it must be stressed that irregularities within the 273 air flow pattern, changes in droplet properties as droplets undergo evaporation, and interference between droplets in the spray all act to produce an actual trajectory differing from that theoretically predicted. (ii) For Small Diameter Chambers. For droplet travel in small drying chambers, the above analysis does not strictly apply. The droplet trajectory to the chamber wall is more likely to be completed without the drying air flow exerting so much influence. Evaluation of trajectories from rotary atomizers and nozzles has been reported by Gluckert (94) for the case of chamber diameters under 5 ft (1.5 m). Droplet travel was assumed to follow the induced air flow from the atomizer. Air movement caused by the atomizer becomes the controlling factor in the trajectory path, not the drying air flow through the air disperser. Gluckert measured the induced air flow. Trajectories are expressed by equations (7.61-7.65). Observed trajectories for droplets issuing from rotary atomizers were represented in terms of the radial velocity of the induced air flow. The radial 7 velocity was expressed as the fraction of the initial velocity (1 /V,), where V is the induced air stream velocity (ft/hr) and V 0 is the droplet release velocity from the atomizer (ft/hr), R is the radial distance from centre of chamber (ft), r d is the rotary atomizer wheel/disc radius (ft). The trajectory is expressed as [ b' V = 1.2 vo (R . rd1"2 r id ) (7.61) x — R where b' = width of annular-slot air orifice (ft) — ( ML ) p a nDV The trajectory was represented as a straight line on plotting V Vo against R (R r d }\ x rd b' — ( The trajectory time (t) to the chamber wall was determined on integration of equation (7.61) (R, = chamber radius (ft)) t r(it c r d /2) 2 2.4 V0 (hir d ) 112 ] L (7.62) Observed trajectories for droplets issuing from pressure nozzles were evaluated (94) from measurements of air flow produced by momentum transfer from the spray to the surrounding air. The resulting trajectory 274 THE PROCESS STAGES OF SPRAY DRYING SPRAY-AIR CONTACT (MIXING AND FLOW) equation was given by (Y = distance from atomizer (ft), cr o = do( 9 .11),) 112 ft) V ,do Vito and the trajectory time given by: 64 \ 2/3 V 2/3 6.4K o cro (7.63) (7.64) (v = drying chamber volume (ft 3 )), Vv ❑ = axial velocity of liquid at nozzle orifice (ft/hr). Observed trajectories for droplets issuing from two-fluid (pneumatic) nozzles were evaluated from the atomizing air-flow. The reduction in droplet/air velocity in the axial direction was represented by 4 = 6.2 (7.65) where V, = velocity of atomizing air at nozzle orifice (ft/hr). Equation (7.65) is for nozzles operating with air velocities at the nozzle of 1000 ft/sec (305 m/sec). Residence time (t) of droplets in the air stream per given distance from the effective nozzle orifice (4) is given by : t 17 ,2 12.4 VA (7.66) where Y,. = distance from nozzle to position four chamber diameters away (ft). 7.4.5. Product Deposition on Chamber Walls Product formation at the chamber wall falls into three main categories. (1) Semi-wet deposits caused by the coarse droplets of the spray travelling to the wall in a time insufficient for such droplets to acquire dry surfaces. (2) Sticky deposits caused by the nature of the product at the temperature of the dryer. (3) Surface dusting of wall by dry powder. Semi-wet deposits occur on wall areas in direct path of droplets released from the atomizer. These deposits can build up to break off as wet lumps or stream down the wall. Deposits are caused by the very coarse droplets in a spray or by incomplete atomization. Elimination of the deposits requires correction to atomizer performance. The drying air flow has limited influence. Sticky products occur over the whole chamber wall surface as swirling powder within the chamber makes contact of product with the confining walls inevitable. With many of these products, deposits build-up to a certain thickness and then fall off to leave the chamber wall clean. Surface dusting also results from the inevitable contact between dried particles and wall. The degree of dusting depends upon the geometry of 275 the wall, wall cleanliness, local air velocity and any electrostatic forces between particle and the wall. Dusting does not form hard layers and powder can be easily removed by an air hose or light brushing. Retention of product at the chamber wall over lengthy time intervals is undesirable. It affects product quality and contributes to more frequent dryer shut down for cleaning. Deposits on the wall can become scorched and when dislodged, mix in and contaminate the entire product. Hard layers often prove difficult to remove. Deposits contribute directly to economic loss in the form of non-saleable product and loss of production due to extended dryer shut down periods for cleaning. Whilst the vast majority of spray dryers operate without chamber wall deposits, there are a range of products that require a limited retention time on the wall to complete moisture evaporation. Such products offer great resistance to moisture removal at low moisture levels, and thus to acquire a dry powder, wall residence times up to 5 minutes may be required (e.g. fruit and vegetable powders). Products that are spray dried in this way form porous agglomerates at the wall. They build up to a certain thickness and then constantly break away from the wall in the form of nodules. The control of such operations is delicate as degradation of the product can easily occur if drying conditions do not produce product properties conducive to continual and frequent break-away of product from the wall. Wall cooling is necessary. Wall deposits are more of a problem in small sized drying chambers where radial distances from the atomizer and droplet residence times are short. However, little data has been published on wall impingement characteristics. (a) In Small Chambers Deposits are always liable in the region of the atomizer wheel level due to the proximity of the wall to the ejected droplets. Region of semi-wet deposition in small co-current flow dryers with rotary atomizers has been reported by the author (95). Impingement at the wall is represented as an impingement profile using spray rake equipment. The profile represents the quantity of droplets contacting the wall. Impingement is pronounced at the roof and atomizer wheel levels. Variations in wheel speed, feed rate, air rate and atomizer location alter the degree and areas of maximum impingement. For a fixed atomizer position, increase in wheel speed acts to decrease impingement at the top of dryer wall and increase impingement below atomizer 'level for low feed rates. At higher feed rates, maximum spray intensity occurs at the dryer roof level. In some cases a second area of heavy deposits forms at the wheel level. The position of this minimum i mpingement region changes with wheel speed. At low speeds, minimum position is at the dryer roof. At high speeds it coincides with the wheel 276 SPRAY—AIR CONTACT (MIXING AND FLOW) THE PROCESS STAGES OF SPRAY DRYING level, For increase in feed rate, impingement increases at and above wheel level. Impingement below this level decreases. For increase in air flow, i mpingement above wheel level decreases. There is an increase in the percentage of the feed impinging at the dryer wall due to the increased air flow creating increased rotation in the chamber. Regions of semi-wet deposition in nozzle dryers depend upon the nozzle mounting and drying air flow. The location and forward direction of nozzles has important influence. For a pressure nozzle at the top of a co-current flow dryer the issuing spray expands on leaving the nozzle. The downward drying air velocity, the nozzle feed rate and nozzle cone angle determine the extent of spray expansion, and the level beneath the nozzle where presence of spray at the dryer wall first occurs. For a two-fluid nozzle likely impingement areas are lower down the dryer. Two-fluid nozzles have a narrower cone angle, and the high speed atomizing air projects the spray forward at higher velocities. The spray expands as it entrains the surrounding air. Spray droplets move outwards to the dryer walls. Even though areas of impingement are further down the dryer, semi-wet deposits are more likely to occur than with pressure nozzles. The atomizer air that surrounds the droplets on spray expansion prevents intimate contact between hot drying air and spray, and lower initial evaporation rates result. Sprays from a pressure nozzle become more quickly under the influence of the air flow, obtain better mixing and evaporate more quickly than sprays from a two-fluid nozzle. For nozzles in fountain-type dryers areas of likely impingement occur at the top of the dryer cone. The larger particles in the spray will fall too quickly out of the air flow on to the chamber cone. These larger droplets may be moist as insufficient evaporation time has elapsed during fall to the wall. A moist layer forms, which is accentuated by dry powder falling and adhering to the moist particles. This can lead to chamber conditions prone to heavy cone deposits. Areas of likely impingement of partially dry product in small sized dryers are shown in figure 7.9. (b) In Large Chambers Impingement areas of partially dry product in large drying chambers are much easier to control than in the smaller designs. The increased chamber size enables longer airborne residence times for droplet drying. The influence of the atomizer on droplet travel becomes minimal and thus wall impingement of product can be counteracted by control of the drying air velocity and direction. Such control is carried out by using the means of adjustment designed into air dispensers for large chambers. For co-current dryers with rotary atomizers and ceiling air disperser air rotation or spray depression (umbrella shaped spray cloud) is controlled 277 C >0044.0( AREAS OF LIKELY IMPINGEMENT Figure 7.9. Areas of likely wall impingement of partially dry product in small dryers. A. Pressure nozzle (hollow cone), co-current flow. B. Two-fluid nozzle, co-current flow. C. Rotating disc/ wheel, co-current flow. D. Pressure nozzle, mixed flow. to eliminate areas of semi-wet deposits (see figure 7.10). For co-current nozzle dryers with non-rotary air flow, the air disperser is a perforated sheet or straightening-vanes. Limited adjustment to the air disperser is available for control of the dryer air flow pattern. The location of the perforated holes in the sheet and distance between sheets can be re-arranged to limit any local eddy flow around the atomizer. However, the nozzle positioning is flexible. Slight re-positioning of the nozzles or change of direction of projection is readily accomplished, and thus spray can be directed away for areas of wall impingement. For nozzles in clusters and 278 THE PROCESS STAGES OF SPRAY DRYING located centrally in the top of the chamber within a ceiling air disperser creating air rotation, a wide range of impingement control is available. The ability to control the rotation at the air disperser and the ability to reposition the nozzles offers great scope for operating dryers without wall impingement of partially dried product. 8 Drying of Droplets/Sprays AIR 8.1. Introduction Figure 7.10. Impingement area control by air disperser adjustment in large dryers with rotary atomization. A. Impingement on roof and upper wall due to excessive air rotation, insufficient spray cloud depression. B. Impingement on lower wall and cone due to excessive spray cloud depression, insufficient air rotation. For the vast majority of products, there is no tendency for powder to adhere to the chamber wall if sufficiently dry. For these products, once drying over extended time periods is completed the chamber can be cleaned by an air sweep (permitting air to flow over wall surfaces) or by a light brush-down. For products having tendencies to adhere to chamber wall, forms of vibratory devices are mounted on the dryer to periodically dislodge powder. For products that have stickiness characteristics, whether it be due to moisture or heat, wall deposits will occur irrespective of air flow pattern control. If vibratory devices on the chamber walls are inadequate, introduction of secondary air around the walls can assist, or an air broom system can be used (figure 5.12). The evaporation of volatiles (usually water) from a spray involves simultaneous heat and mass transfer. With the contact between atomized droplets and drying air, heat is transferred by convection from the air to the droplets, and converted to latent heat during moisture evaporation. The vaporized moisture is transported into the air by convection through the boundary layer that surrounds each droplet. The velocity of droplets leaving the atomizer differs greatly from the velocity of the surrounding air and, simultaneously with heat and mass transfer, there will be an exchange of momentum between the droplets and the surroundings. The rate of heat and mass transfer is a function of temperature, humidity and transport properties of the air surrounding each droplet. It is also a function of droplet diameter and relative velocity between droplet and air. Models to describe the droplet drying are to be found in many publications on drying. Drying principles, factors controlling drying rates and drying characteristics of droplets have been introduced to the reader in chapter 3. The evaporation history for spray droplets commences with moisture removal at near constant rate and constant droplet surface temperature (first period of drying) followed by a decline in removal rate until drying is complete (second or falling rate drying period). The rate begins to fall off once the droplet moisture content is reduced to a level known as the critical moisture content. The majority of droplet moisture is removed during the first period of drying. Moisture migrates from the droplet interior at a rate great enough to maintain surface saturation. The wet bulb temperature represents the droplet temperature. The evaporation rate can be considered constant, although this is not strictly true. In the spray drying operation droplet 280 DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING evaporation commences with the immediate spray—air contact, and the rapid transfer of moisture into the air is accompanied by lowering of the air temperature. Any air temperature lowering reduces the driving force for heat transfer, and the evaporation rate can begin to fall of even though surface saturation is being maintained. However, it is common to refer to the initial phase of droplet drying as the constant rate drying period. Moisture migration lowers the moisture level within the droplet and a point is eventually reached when the rate of migration to the surface becomes the limiting factor in the drying rate. Surface wetness can no longer be maintained, and a falling-off in drying rate results. The rate of moisture migration is effected by the temperature of the surrounding air. If the air temperature is so high that the temperature driving forces permit evaporation to commence at a rate where migration of moisture cannot maintain surface wetness from the start, the droplet will experience little constant rate drying. A dried layer will form instantaneously at the droplet surface. This dried layer presents a formidable barrier to moisture transfer, and acts to retain moisture within the droplet. Thus inlet drying temperatures can readily influence the dried product characteristics. Increase in inlet air temperature often results in a rapid formation of the dried outer layer. This submits the droplet to higher surface temperatures than when lower inlet air temperatures are used. A lower air temperature would mean a lower initial drying rate, with the maintenance of a surface temperature (equivalent to the wet bulb temperature) over longer time periods. cc LU >— o w x IL/_ z Cr a 8.2. Evaporation of Pure Liquid Droplets < <ow CC c The actual evaporation time for droplets contacted at a fixed air temperature depends upon droplet shape, chemical composition, physical structure and solids concentration. The actual time is the sum of the constant rate and the falling rate periods until the desired moisture level is reached. The general drying characteristics are illustrated by a drying rate curve, as shown in figure 8.1. In phase A.B, the drying rate is established immediately the droplet contacts the drying air. There follows a slight increase in droplet surface temperature, and the drying rate increases in the milliseconds required for heat transfer across the droplet—air interface to establish equilibrium. In phase B.C, conditions of dynamic equilibrium are represented. Drying proceeds at constant rate, which is the highest rate achieved during the entire droplet evaporation history. Droplet surface is maintained saturated by adequate migration of moisture from within the droplet to the surface. In phase C.D, at point C, the critical point is reached and moisture within the droplet can no longer maintain surface saturation. Drying rate begins to fall, initiating the falling rate drying period. This period can form more than one phase, if local areas of wetness remain on the droplet surface. Phase C.D continues until no areas of wetness remain. In phase D.E, resistance to mass transfer is wholly in the solid layer. Evaporation continues at a decreasing rate until the droplet acquires a moisture content in equilibrium with the surrounding air. Approach to the equilibrium moisture content E is slow. In the spray drying operation, product is usually removed from the dryer before the equilibrium moisture content is reached. Droplet temperature rises throughout the two phases of the falling rate period. Figure 8.1 is diagrammatic. Drying curves in reality have no sharply defined points. Some of the drying zones as shown may not even occur. For example, in the spray drying of products that are heat sensitive, the applied air temperatures are low and the phase A.B can well extend until the critical point is reached. The drying in this case can be said not to feature the customary constant rate period. W 1.L1 o 281 o- E MOISTURE CONTENT (1-11 Figure 8.1. Drying rate curve. ( WEIGHT OF MOISTURE PER UNIT WEIGHT OF BONE DRY PRODUCT ) Conclusions drawn from studies on the evaporation of pure liquid droplets form the basis for understanding the spray drying evaporation mechanisms. The ideal case of evaporation of single pure liquid droplets can be modified to deal with the deviations in the basic theory necessary to include the presence of dissolved or insoluble solids. The extent of moisture removal from a droplet present in a spray dryer depends upon the mechanism governing the rate of evaporation and the 282 DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING residence time during which evaporation takes place. The residence time results from the spray—air movement set up in the drying chamber. For the greater part of droplet travel in the chamber, the droplets are completely influenced by the air flow, and the relative velocities between droplet and air is very low. The boundary layer theory states evaporation rates for a droplet moving with zero relative velocity is identical to evaporation in still-air conditions. Thus the mechanism of evaporation that is still-air based upon boundary layer theory can be justifiably applied to many spray drying conditions. In the case where droplets move relative to the surrounding air, the resulting flow conditions around the moving droplet influence the evaporation rate. In calculating transfer rates, these flow conditions plus the properties of the droplet are represented in combinations of the dimensionless groups 283 droplet in still air can be expressed as Sh = 2.0 (8.1b) following the heat and mass transfer analogy (98). For pure liquid droplets, equation (8.1) predicts that the rate of change of the droplet surface will remain constant during evaporation. The evaporation rate (c1147 Idt) in terms of mass transfer can be expressed from equations (3.6) and (8.1), by substituting K = ,12) D and A= dW — = 277D,D(P,B — p,,) (8.2) dt Group Significance Symbol Reynolds (Re) inertia force viscous force D„ p a where ./), B = water vapour pressure at temperature of saturated droplet surface, p w = partial pressure of water vapour in surrounding air. For air—water system at atmospheric pressure ila D, = 0.258 cm 2 /sec at 26°C Prandlt (Pr) kinematic diffusivity thermal diffusivity C p i.t a \ = 0.305 cm 2 /sec at 60°C Schmidt (Sc) kinetic viscosity molecular diffusivity Nusselt (Nu) Sherwood (Sh) total heat transfer conductive heat transfer mass diffusivity molecular diffusivity Kd The evaporation rate in terms of heat transfer can be expressed from equations (3.6) and (8.1) by substituting h, = 2K d /D dt ( h,D K) K gD ( D) where D = droplet diameter, p a = density of drying medium, pa = viscosity of drying medium, C, = heat capacity (constant pressure of drying medium), Kd = average thermal conductivity of gaseous film surrounding an evaporating droplet, h, = convection heat transfer coefficient, K g = mass transfer coefficient, D v = diffusion coefficient. 8.2.1. Evaporation of Single Droplets (a) Droplet Evaporation under Negligible Relative Velocity Conditions Experimental data (108) have shown that heat transfer to a spherical droplet in still air can be expressed as Nu = 2.0 27tDK, dW (8.1a) Likewise has it been established that the mass transfer from a spherical = (Ta T)s (8.3) where Ta = air temperature, TS = droplet surface temperature. Conclusions can be drawn from equations (8.2) and (8.3) as to the characteristics of pure liquid droplet evaporation. (a) The evaporation rate is proportional to diameter and not surface. (b) Absolute evaporation rates from large droplets are greater than from small droplets. (c) Evaporation is proportional to the square of initial diameter. The evaporation time can be deduced from a heat balance over a spray droplet. From equation (3.6) d14.7 2 — = h AAT dt =heAAT dt — (1147 Now itD 3 p i 284 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS 285 and for heat transfer Therefore (Nu) = 2 + K 2 (Rer'(Pr)Y' _hcnD2AT 41 dt 16 2 zp 1 3D 2 d(D) — h anD AT dt 6 A AP' dt = (8.4) d(D) 210 T The term —(2p 1 /2AT) remains constant during the majority of droplet residence time in the dryer, and integration of equation (8.4) yields the evaporation time (t) (D, .= initial droplet diameter). I D ° d(D) t = API 2AT JD 1 h c (8.5) AT is the mean temperature difference between the droplet surface and surrounding air. It is best to apply the logarithmic mean difference (LMTD) as defined by LMTD = AT. — AT. 2.303 log 10 (AM/AT' ) (8.6) AT, and AT, are the temperature differences between droplet and air at the beginning and end of the evaporation period. The arithmetic mean (AMTD) can be used with little error if AM/AT 1 is less than 2. AMTD AT, + AT, 2 (8.7) Equation (8.5) can further be simplified where for negligible relative velocity conditions h e = 2K d /D (equation (8.1)) t 19° API 4KAT T Dd(D) = API (D,1 8K d A T — D 2,) (8.8) . (b) Droplet Evaporation under Relative Velocity Conditions Evaporation rates increase with increase in relative velocity between droplet and air due to the additional evaporation caused by the convection in the boundary layer around the droplet. The total transfer coefficients for the transfer from a spherical droplet can be expressed in terms of the dimensionless groups where for mass transfer (Sh) = 2 + K i (ReNSc)Y (8.9) (8,10) Equations (8.9) and (8.10) reduce to equation (8.1) when the relative velocity is zero. There is much discussion over the power values of (x), (y), (ye), and constants K„ K2. Rowe, Claxton and Lewis (99) determined values of the above powers and constants for spherical droplets/particles, and by comparison of data from other investigations concluded x = x' = 0.5 (8.11) y = y' = 0.33 (8.12) Equation (8.11) represents an average value since the power of Reynolds number increases with Reynolds number from about 0.4 at Re = 1 to 0.6 at Re = 104. The value of x accepted generally for evaporation conditions in spray drying is 0.5. This is applicable to a Reynolds number range between 100 and 1000. Motion of small droplets in this range occurs only in the first fractions of a second of travel, and thus much of the evaporation occurs at droplet Reynolds number far below 100. According to Rowe (99) little importance should be attached to having an exact value for the power of Reynolds number. Various proposals of equations (8.9) and (8.10) are given in table 8.1. The form most widely applied is the Ranz and Marshall (100) equation. "3 Dvpa °•5 (17 D .= 2.0 + 06 CP'12 a (8.13a) Kd Kd lia „ 0.33 Dv Q.5 0.5 = gD 2-0 + 0-6 ' (8.13b) D, PaDv 11 a — When applying the above equations, certain limitations must be taken into consideration. Steady state drag coefficients apply. It is convenient to apply the drag equations at steady state to the case of accelerating or decelerating droplets. In reality the drag coefficients (C D ), for accelerated motion can be 20-60 higher than values at constant velocity. Heat transfer to evaporated moisture is neglected. For drying conditions at high temperatures, much heat is taken up in heating the vapour as it is transported outwards from the droplet surface. This effect is discussed later (see page 293). Droplet internal structure is stable. Any internal circulation, oscillation or surface distortion of the droplet will increase heat and mass transfer rates due to variations in the thickness of the boundary layer. DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING &La ss,,§8s.8 1;:4' cn on on on on on o? v? on o? o? on o? h o c Ch a o CD Table 8.1. Proposals for the E(iiation Nu (or Sh) = 2.0 + K(Re)x(Pr or Sc)'' 286 287 Droplets are stable in air flow. Droplets in a spray dryer are often subjected to a swirling air flow. This causes droplet rotation, and such rotation reduces the boundary layer, thus increasing evaporation rates. (0 Evaporation Rate. Droplets released from an atomizer decelerate rapidly to become completely influenced by the surrounding air flow. During droplet deceleration considerable evaporation occurs. Equations by Frossling (102) express evaporation during this period. The increase in evaporation rate due to droplet motion is represented by Frbssling as the second term on the right-hand side of equations (8.20). Mass transfer Ap (I. + 0.276Re"Sc' 33 ) (8.20a) 2701C dA T(1 + 0.276Re"Sc" 3 ) (8.20b) N = 2nDD u? ‘4 vn un ken 47 0 o 6 6 6 6 6 on rq rq c) 41 un c) rq cN t"? V7 yi vl o7 CD CD c) cb c5 c) o d die tu ms tes Sy RT Heat transfer dW dt where N = transfer rate, dp = driving force in terms of partial pressures. From equations (8.20) the Nusselt number for air system can be calculated Nu = coI a) &I ,f2r a) a) a) tA "t73 '7) g cti ri ariti#6 c)c 0 CD 000 a rrJ +al) a.) Kd = 2(1 + 0 , 25Re") = , ' 27rD13, R 0.276Sc t Ln r- 00 a\ -1 c6 06 06 06 D6 06 00 Re" dt (8.22) where NEx = transfer rate during deceleration. The fractional evaporation is a weight fraction, and is obtained by dividing NEX by the droplet weight (expressed in moles). The Sjenitzer equation to express the fractional evaporation (X w ) yields X, = 4.42AHSc'" m (8.21) Sjenitzer (107) developed equation (8,20a) to express the weight frar,tir,In (X,) of a pure liquid droplet that evaporates due to- droplet relative motion. The evaporation during droplet deceleration (from equation (8,20a)) equals NEx tn kD (Re ) CdRe1.5 (8.23) Where AH = humidity gradient (approx. ApM,IRTp„), = molecular weight of liquid droplet. Values of the integral are given in table 8.2. Inspection of equation (8.23) shows that subject to constant properties of the system, the fractional •aporation during deceleration depends only upon the droplet Reynolds number (at atomizer release) and the final velocity obtained at the completion of evaporation. The final velocity is 288 THE PROCESS STAGES OF SPRAY DRYING Table 8.2. Values of the Integral d(Re) C.Re 1.5 in Equation (8.23) Re 5 x 10 4 1 x 10 4 5 x 10 3 1 x 10 3 5 x 10 2 1 x 10 2 5 x 10 1 1 x 10 1 5 1 d(Re) CDR e " 0.030 0060 0.090 0.175 0.300 0.390 0.600 0.615 0.670 0.745 the terminal velocity of the droplet. This velocity, and hence the Reynolds number, is dependent upon the droplet diameter at the onset of terminal velocity conditions. For pure liquid droplets, the diameter changes during motion. Change of diameter produces change in deceleration rates and the extra evaporation produced by the droplet motion can only be calculated by a stepwise method. Values Of X will for the case of decreasing diameters become smaller than values calculated from equation (8.23), which assumes constant diameters during evaporation. For low values of the humidity gradient (OH) droplet diameter change during the short time interval of droplet deceleration can be considered negligible. Sjenitzer (107) illustrated the application of equation (8.23) for the aqueous droplet system using the assumption of negligible droplet diameter change during the deceleration period and employing the deduction that the fractional evaporation during the deceleration period is independent of the droplet release velocity when this is high. To comply with the assumption, a low humidity gradient was selected (OH = 0.06). Fractional evaporation due to droplet motion of water droplets ranging in diameter from 100-1000 micron is shown in table 8.3. Values were calculated for a drying air temperature of 379°F (193°C), droplet wet bulb temperature of 109°F (43°C), using equation (8.23) and table 8.2. Once droplet deceleration is completed and terminal velocity conditions prevail, the Frossling equation (8.20) can be rearranged to obtain the weight fraction of the droplet evaporated per unit length of travel (d W Id!). DRYING OF DROPLETS/SPRAYS 289 Table 8.3. Fractional Evaporation of Aqueous Droplets Undergoing Decelerated Motion in Dry Air 379°F (193°C) (Fractional increase due to motion of constant diameter droplet) Fractional Evaporation x,„,% (micron) 100 200 300 400 500 29.0 25.0 21.5 19.0 17.0 (micron) 600 700 800 900 1000 15.5 145 13.6 12.8 12.1 A pp dW = LLD (1 + 0.276Re"Sc') di ViD2 ART (8.24) where the terminal velocity Vi is calculated by equations in chapter 7 (7.25), (7.27). For aqueous droplet—air systems, equation (8.24) reduces to H W 4.6 x 10 (8.25) 2 (1 + 0.23Re') di fD where dW 'di = fractional evaporation per metre length of fall, V, = terminal velocity, OH = humidity difference. A plot of equation (8.25) shows dW I& decreases rapidly with increasing droplet diameter. In a spray distribution, the smaller droplet sizes will dry more rapidly than the larger. This results in the possibility of over-dried, small particles being present with larger particles of desired moisture content. Certain significant conclusions can be drawn from the Sjenitzer equations 1. A slight reduction in droplet size causes a marked increase in the fractional evaporation. Thus drying chamber dimensions based upon constant droplet size during evaporation will be conservative. The effect of droplet size reduction further acts to decrease the chance of wall impingement of semi-dried droplets. 2. If droplets remain a constant diameter the resulting evaporation will act to reduce droplet density and hollow dried particles will form. Hollow droplets fall at lower velocities. As the fractional evaporation is inversely proportional to the droplet velocity, and evaporation on a weight basis is equal, the fractional evaporation increases over that of a solid droplet at the same rate of fall by a factor equal to the ratio of droplet volume to its hollow air space volume. 290 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS 3. For small sized droplets under 100 micron, evaporation during deceleration Can be considered insignificant compared with the free-falling evaporation during the remaining residence time in the air. (ii) Evaporation Time. The evaporation time for a pure liquid droplet under relative velocity conditions is obtained from equation (8.5) by substituting values of h, from either the Ranz-Marshall equation (8.13a) or Ingebo equation (8.14). Using the Ranz-Marshall equation, the time of evaporation can be evaluated as follows t = DAD) 2K d AT JD (2 + 0.6Re"Pr' (8.26) 33 ) Equation (8.26) was integrated by Duffie and Marshall (22) for droplets falling at terminal velocity, within the semi-turbulent flow region (Reynolds number range 0.2-500). The terminal velocity was calculated for this region using equation (7.27) (chapter 7) D0 2# [(DI, - D?) t= 8KdAT D 2.° 7 On D i. " ± fDioo I where = [0153 ( gPa(P)122- .33 P ) (" 1 0.5 [ CP Pay a ) Kd (8.28) With D in equation (8.27) expressed in micron, equation (8.28) can be expressed for. aqueous droplet-air systems in corresponding metric units as 0.36 13 = 0.071 H 11 2 ram - i.o 7 Table 8.4. Evaporation Times for Pure Liquid Droplets (after Duffie and Marshall (22)) Droplet diameter D (micron) Evaporation times (sec) = 2.0 600 500 400 300 200 100 50 3.2 2.5 1.8 1.0 0.6 0.2 <0.1 p iA N [ 8K d A T (8.29) 3 = 3.0 13 = 3.5 6.0 4.8 3.1 2.0 1.1 0.3 0.1 11.0 8.2 5.9 3.8 2.0 0.6 0.2 19.0 14.0 10.0 7.0 3.3 1.1 0.3 1 2)3 0 D2.o7d(D) 2 D, r 1 + /3D 1 '" (8.30) Evaporation times for values of /3 are given in table 8.4 for droplet diameters between 50 and 600 micron. Values of /3 are obtained from the temperature driving force (AT) between air and droplet surface. Values of # are shown in table 8.5. The reference droplet temperature (Tr) for both tables is 130°F (54.5°C). For droplet temperatures that greatly differ from the reference temperature a correction factor can be applied to the predicted evaporation time. The correction factor is given -by L, - Ta where Prandlt number is taken as 0.73 and p i » Pa in g/cm . Ta is the absolute air temperature. Equations (8.28) and (8.29) result in a straight line graph on plotting 13 against Ta on log-log paper. The second term of the right-hand side of equation (8.27) is a velocity correction for droplets larger than 100 micron at terminal velocity in the semi-turbulent flow region. The necessary correction for droplets under 100 micron is considered negligible. To express the entire evaporation history of a pure liquid droplet, i.e. droplet evaporates away completely, equation (8.27) can be integrated for droplet evaporation time during the decrease in droplet size to 100 micron. The remainder of the evaporation time, i.e. droplet size decreases below 100 micron until evaporation completion is represented by equation (8.8). Total drying time on summation of = 2.5 equations (8.8) and (8.27) becomes t = (8.27) 291 T. droplet For evaporation of liquid droplets other than water, a correction factor Table 8.5. Values of fl for Different Temperature Driving Forces O T) AT /3(mm -1 ' 07) (°F) (°C) 2.0 2.5 3.0 3.5 800 480 290 200 426 249 143.5 93.5 292 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS can be applied following the use of table 8.4 and table 8.5. Values of /3, obtained from table 8.5 or equations (8.28) and (8.29), are multiplied by /3" 6 . The evaporation time corresponding to the modified /3 value, is finally corrected by the factor ro .Awaieri• Using the Ingebo equation (8.14) the time of evaporation can be evaluated as follows (for Nusselt numbers greater than 10 and constant relative velocity (101)) t = 4KdAT D1) . 4 X 1 0.6 Vreip agR T, X 0.213 K doir) Kd {vapour) P1MMDV (8.31) 0.5 ] where MM mean molecular weight of vapour and air, D v = vapour diffusivity. For droplets falling at terminal velocities in the Stokian region (Reynolds number < 0.2), evaporation times can be expressed by equation (8.32). The terminal velocity equation (7.25) (chapter 7) is applied. P [(D02 8K :iii:AT 2)6" D° D'd(D) Lop (8.32) PD1.5] where [ g ( pi = 0.276 p 18/4 o pa l 0.5 rc pita l 0.33 (8.33) Kd ° ° (3' varies from 80-200 over the temperature range 32-540 F (0-282 C). The second term of the right-hand side of equation (8.32) represents the decrease in evaporation time of a droplet falling at terminal velocity compared with the time required for evaporation in still air conditions. All the equations derived above to express droplet evaporation time are based upon two important assumptions (369). These are (i) areas of heat and mass transfer are equal for each droplet and (ii) all heat transfer to a droplet is consumed as latent heat of vaporization. Such assumptions are justified for evaporating conditions where drying temperatures are not excessively high. EXAMPLE 8.1 A spray dryer installation is applied to a titanium tetrachloride process whereby a TiC1 4 content in combustion gases is increased by spraying impure liquid TiC1 4 into the combustion gases. A purification takes place as the clean gases pass to condensers, while solid impurities are collected at the chamber base. If the atomizer produces a coarse spray, where the maximum droplet diameter is 500 micron, calculate the maximum evaporation time of the spray. 293 Data Dew point of TiCI 4 = 266°F p i = 1.65 g/cm 3 A„ = 72 BTU/lb Inlet temperature of combustion gases = 2000° F Outlet temperature of combustion gases = 302 ° F Feed temperature = 70°F Now droplets evaporate completely to vapour. Temperature driving force (equation (8.6)) A To = 2000 — 70 ° F = 1930°F A T, = 302 — 266 ° F = 36°F 1894 LMTD = 2. 303 log10 1894 36 1894 — 478°F 2.303 x 1.7211 Mean air temperature surrounding droplet = 478 + 266 = 744 ° F. From table 8.5 the corresponding value is taken as 2.5. Product correction factor /3 0 ' 36 = 1.39 therefore overall value = 1.39 x 2.5 =- 3.46. From table 8.4 take /3 as 3.5. Therefore at D = 500 micron, equivalent water evaporation time is 14.0 sec. Time correction for TiC1 4 droplet = , Pi Ai . ' wat r e Droplet temperature correction = [ 1.65 x 72 970 Ta — 130 1 Tdroplet 744 — 130 744 — 266 614 478 — 1.28 Maximum evaporation time 14.0 ( 1.65 x 72 ) 1.28 = 2.2 sec 970 The evaporation time of 2.2 seconds assumes the effects of the high gaseous temperature surroundings to be negligible. As discussed below, these effects can be significant. (c) Evaporation under High Air Temperature Conditions For droplet evaporation at high air temperatures heat transfer to the droplets no longer solely provides the latent heat of vaporization. Heat is also transferred to the vapours moving away from the droplet interface 294 into the air flow. This can lead to decisive errors when calculating evaporation times by the equations mentioned above. The evaporation time calculated in example 8.1 could well be invalid because the evaporation is conducted at high temperature, and here the assumptions for the computation are no longer relevant. The effect of high temperature on evaporation mechanism has been analysed mathematically by Marshall (108) and Godsave (367). For an evaporating droplet, the differential equation for conduction of heat through the surrounding vapour layer can be drawn up. Consider figure 8.2 where W' is the rate of evaporation (mass/unit time) and x the radial distance from the centre of the droplet. The differential equation for heat passing inwards through the gas film surrounding an evaporating droplet with simultaneous transfer of vapour outwards through the film can be shown to be x 2d2T2 + 2x dx 295 DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING W/C p \dT 0 4n1( d ) dx DROPLET SURFACE MASS FLOW OUT (W) I NEAT FLOW IN (8.34) where Kd = thermal conductivity of gas film surrounding droplet. Integration (108) (367) of equation (8.34) between the radial limits of droplet surface and bulk air flow enables the temperature to be expressed as a function of distance through the layer. E T — Ts Ta— Ts — exp ( exp ( exp ( E r E R Figure 8.2. Configuration of droplet evaporating in high temperature surroundings. (8.35) — exp ( — — r /) 2 where Ts = droplet surface temperature, Ta — bulk air temperature, t = any 1 temperature in the vapour layer, E = 14/ C p147rK„, r1 = droplet radius, R2 = bulk air flow radial limit: Values of E assume the thermal conductivity (K d ) to be constant over the entire layer. K d actually varies according to the vapour composition of the layer. An average value should be used. By defining the heat transfer coefficient (h e') as (108) QI AAT or Kd dTIdx r 1 ) ( hcD 2E1r, Nu — Kd 1 21 ) (7 1 (Nu)E= 0 = 1 1 (8.37) _ r1 - R The effect of vapour surrounding the droplet upon the Nusselt . number may be estimated from the ratio, 1 AT The Nusselt nuiriber Wu) can be expressed s Equation (8:36) forms the basis for expressing the actual and apparent evaporation conditions. Actual conditions are given by equation (8.36). Apparent conditions are obtained by expanding the exponential in equation (8.36) and substituting E = 0 into the equation to give the Nusselt number at negligible evaporation rate from the droplet. 1 [exp E(-1--1 r1 R2 (8.36) Nu Nu E _, E(— 1 'l exp E(-r/ (8.38) 296 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS where the Nusselt number ratio also represents the ratio of the actual and apparent heat coefficients (11,(actual) and h c (apparent)). Hence Correcting for mass transfer effects using the correction factor a' —1 ai h c (actual) = h c (apparent)( , ea — 1 (8.39) where a' is calculated from equation (8.43). Droplet relative velocity is assumed low, whereby Nu = 2. where (368) a , WiC p 1 47c1C d rt 1 R2 I (8.40) If the radial limit (R 2 ) of the boundary layer is of the order of the droplet diameter (D), (a') reduces to W'C P 1 X— a= • 47rKd D Nu(ATC11 2 A. LMTD = 478 ° F C p = 0.133 BTU/lb°F Calculation of correction factor : T = 478 ° F, ATC p ATCP = 0.88, a' = 0.61, (e' a 1+ = 1.88, l 1) = 0.72 Now t actua l = tapparent ( e a' 1 2.21 tactual = — = 5•1 sec 0 .72 Percentage increase in evaporation time due to mass transfer effects = 28 %. (8.42) The increase in droplet evaporation time due to heating of the surrounding vapours at high temperatures can be obtained by dividing the apparent evaporation time by the correction factor a' /(e" — 1). An expression for a' can be derived (108) a = In [1 + Data (8.41) Equation (8.39) shows the influence of mass transfer on observed heat transfer coefficients. Equation (8.39) indicates that at high evaporation rates (i.e. E is large) a' is large and the value of actual Nusselt number may be appreciably lower than apparent Nusselt number. At high temperatures, the value of a' can reach 4.0, when the corresponding value of a'/(e" — 1) becomes approximately 0.075. This indicates that values of h, (actual) can be as low as one-tenth the value of h, (apparent). The apparent Nusselt number (Nti) ED can be calculated directly from the McAdams (10) relation for heat transfer to spheres (Nu) apparent = 0.37 rvreiPay.6 297 (8.43) The relative velocity between droplets and air in the spray dryer is very low for a substantial part of the droplet evaporating time and the Nusselt value correspondingly approaches 2.0. The term (A TC p/A) determines the magnitude of a' and can be interpreted as the ratio (sensible heat transferred to vapour/latent heat). EXAMPLE 8.2 If the correction for high temperature operation is applied to the droplet evaporation in example 8.1, what difference does this make to the predicted evaporation time? Predicted evaporation time (example 8.1 = 2.2 sec). 8.2.2. Evaporation of Sprays of Pure Liquid Droplets The evaporation characteristics of droplets within a spray differ from evaporation characteristics of single droplets. Although basic theory applies in both cases, it is difficult to apply this theory to the case of a large number of droplets evaporating close to the atomizer. Any analysis of spray evaporation depends upon defining the spray in terms of a representative mean diameter and size distribution, the relative velocity between droplet and its surrounding air, droplet trajectory and the number of droplets present at any given time per given volume of drying air. Furthermore there are grave difficulties in determining these factors in the vicinity of the atomizer and spray evaporation data is subsequently limited. For sprays moving at low velocities in low velocity air (counter-current flow dryers) or at low relative velocities with high velocity air (co-current flow dryers), the following points can be made. 1. Spray evaporation causes reduction in air temperature and evaporation rate decrease. 2. Sprays of wide distribution evaporate initially more quickly than more homogeneous sprays of the same chosen mean diameter. The increased 298 THE PROCESS STAGES OF SPRAY DRYING evaporation is due to the smaller droplet sizes in the distribution. The larger droplets evaporate much slower, and thus the overall spray evaporation time is longer. 3. No mean diameter parameter can represent adequately the droplets during evaporation of a spray. 4. The size distribution gives the best representation of droplets during the evaporation of a spray. 5. Size distribution of droplets in a spray changes during evaporation. 6. For homogeneous sprays, the droplet diameter parameter decreases during evaporation. 7. For non-homogeneous sprays the droplet mean diameter will generally show an initial increase prior to decrease until completion of evaporation. Evaporation of sprays, whose droplets move at pronounced relative velocities (for example, coarse nozzle atomization in co-current flow or `fountain-type' dryers) shows additional features. 1. The droplets travel greater distances before a given fraction is evaporated. 2. Influence of relative velocity between droplet and air is more significant on evaporation rates at higher release velocities from the atomizer and at higher drying temperatures. 3. For droplet release from atomizers at high velocities, the relative error of neglecting droplet velocity is greatest for the smallest droplet sizes in the spray distribution. Small droplets evaporate virtually instantaneously, and a large proportion of the evaporation is accomplished in the period of droplet deceleration. Notable contributors to spray evaporation analysis have been Probert (110), Marshall (108), Shapiro and Erickson (111), Fledderman and Hanson (112), Manning and Gauvin (113), Bose and Pei (114), and Dickinson and Marshall (109). Probert (110) presented a - theoretical analysis based upon a spray size distribution following the Rosin—Rammler distribution. Spray droplets were considered to have no relative velocity and temperature driving force changes were assumed negligible during evaporation. The more homogeneous the spray the faster evaporation proceeds to completion, although Probert showed coarse spray distributions may well have higher initial evaporation rates. Work by Probert was extended by Fledderman and Hanson to cover spray evaporation under conditions of relative velocity, where the spray distribution was assumed to follow the NukiyamaTanasawa equation. The equations proposed by Fledderman and Hanson proved extremely complex, rendering the equations of little practical value. A practical method of spray evaporation evaluation has been proposed by Marshall (108). An increment method is involved. The size distribution is divided into small size groups. Each group is considered individually DRYING OF DROPLETS/SPRAYS 299 while evaporation proceeds and the average diameter of the spray decreases. The method was simplified to a spray following a logarithmic distribution, evaporating under zero relative velocity conditions. The method was set out for pure liquid droplets. The calculations, however, can prove useful illustrating the nature of changes that do take place when the spray drying operation does not involve pure droplets. The Marshall method involves the calculation of the change of the average droplet diameter in each selected size group over short time intervals. Short time increments are selected to enable the assumption of droplet evaporation under the same temperature driving force during the selected time interval. Evaporation for each size group in the distribution is considered, and a new distribution is drawn up on which the evaporation during the second time interval is calculated. Procedure continues until evaporation is complete. The procedure as stated by Marshall is as follows 1. Plot the cumulative distribution curve for the spray under investigation. This involves plotting the droplet size in the spray against the cumulative percentage of the spray less than the droplet size. 2. Size-increments are selected and the average diameter specified. Using the droplet size data, the frequency of droplet size occurrence is known and mass fractions (F) corresponding to the size increment are calculated. 3. The initial temperature driving force between droplets and air is determined. 4. The time for complete evaporation is determined and designated t o , The time is obtained from equation (8.5), substituting k for Kd. to p I 2.(D3 Df) 8KdAT (8.44) Value of AT, obtairidd from step 3, is assumed to hold during the entire droplet travel during the spray dryer. D, is zero for a pure liquid droplet. 5. On the basis of step 4, a suitable time increment (At,) is chosen for estimating the first increment of evaporation. Marshall proposes a suitable time increment which enables complete spray evaporation of the first two size groups. 6. The time increment At, is substituted from the calculated value t 0 . The resulting time t,, i.e. (t 0 — At,) is substituted back into equation- (8.44) and a value of D, the 'reduced' diameter of the droplet in each size group is calculated. The reduced diameter is assumed to exist after t 1 seconds of evaporation. The time increment must be selected so that constant temperature conditions (AT) over the time increment can justifiably be assumed. 7. The ratio (.13,1D 0 ) 3 is calculated. This ratio will give the numbers proportional to the fraction of the spray remaining in each size group. The mass fractions calculated in step 2 are multiplied by this ratio. 300 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS 8. The multiples of each size group are summed, i.e. EF❑ (D i lD ❑ ) 3 = Fl . (F,/F❑ ) equals the fraction of remaining spray and (1 — F,/F❑ ) is the fraction evaporated. If F❑ is normalized, F❑ = 1, and F 1 is the remaining fraction. 9. The incremental temperature drop over the first time interval is calculated from a heat balance. Heat transfer effects to the vapour surrounding the droplet are considered negligible. Hence M air C p AT (8.45) where M ai ,. = mass air flow rate through the dryer, M ug = liquid evaporation rate, AT = temperature drop through the dryer. The incremental temperature drop over the first time interval becomes (Ti — T2 )/(1 — F 1 ), where F1 is the fraction of spray remaining after the first time increment (At /). 10. The procedure (steps 1-9) are repeated for the new size distribution formed after At 1 seconds. 11. The calculation proceeds with each new size distribution being considered until evaporation is completed. The above procedure is time-consuming, but significant information becomes available. The variation of spray mass fractions and drying air temperature with time is computed. Marshall (108) illustrated the procedure for a spray of geometric mean diameter (120 micron). Maximum droplet size was 450 micron. The spray was contacted with 530°F (277°C). The outlet air temperature was 230°F (110°C). Table 8.6 illustrates the evaporation history of the given spray. Table 8.6. Spray Evaporation History Droplet size (micron) Droplet size below which stated % of spray occurs geoTime metric t max, mean (sec) Dina, DGM 10 % 90% °F 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 202 205 212 220 230 250 270 285 285 530 325 275 260 250 245 240 239 238 450 438 430 425 421 416 412 408 405 120 125 140 155 165 172 177 180 180 62 62 62 63 65 67 69 72 93 Drying air temperature 277 163 135 127 121 118 116 115 114.5 Temperature driving force T °F °C 400 180 150 130 120 115 111 108 106 204 82 66 54 49 46 44 42 41 Spray mass fraction remaining 1.0 0.30 0.15 0.10 0•07 0.06 0.05 0.04 0035 301 Conclusions applicable to spray dryer operation can be drawn from table 8.6. 1. The majority of spray evaporation is completed in a short time interval. For example, 90 % of the evaporation is completed during the first 1.5 seconds. 2. Rapid decrease in air temperature accompanies the evaporation. For example, air temperature drops to within 30°F (17°C) of the outlet air temperature during 1.5 seconds. 3. The mean size of the pure liquid spray increases with time due to the rapid completion of evaporation of the smaller droplet sizes in the spray. In actual spray drying operations, the variation of mean size with time will depend upon the solid content in the spray droplets and whether drying characteristics lead to particle expansion or retraction during evaporation. Shapiro and Erickson (111) studied the mathematics of spray evaporation for one-dimensional spray motion. General differential equations were proposed to express spray behaviour, but lack of a comparison between predicted and experimental results limits the usefulness of the work. Manning and Gauvin (113) determined heat and mass transfer rates for water sprays in co-current and counter-current air flows. Experimental data justified the use of the Ranz and Marshall (equation (8.13)) and Frossling equations (8.20) (8.21) for spray evaporation. Bose and Pei (114) studied evaporation of water sprays in a co-current flow nozzle dryer. The relative velocity between spray and air was concluded to be of great significance to the resulting heat and mass transfer rates. A substantial part of the evaporation takes place during spray deceleration. Large errors can occur if relative velocities are equated to the terminal velocity and used as the velocity term in the evaporation analysis. Dickinson and Marshall (109) drew up computer programmes to calculate the evaporation histories of water sprays. The conditions of both negligible and significant relative velocity between spray and air were studied. Principle parameters incorporated in the studies were a mean diameter, size distribudim of spray on release from atomizer, droplet population, drying air and droplet temperatures and air velocity. Mathematical equations for spray evaporation of non-uniform distributions were developed. Ideal conditions of constant droplet temperature, ideal co-current and counter-current air flow and droplets of pure liquid were assumed to prevail. It would appear that future procedures for evaluating evaporation histories will rely heavily on computer facilities, and the development of improved experimental techniques to study droplet and spray evaporation. Techniques for studying evaporation of sprays in three-dimensional movement would be of particular value to meet demands of accurate input data for full utilization of the computer resources. 302 THE PROCESS STAGES OF SPRAY DRYING Current manual step-wise methods will continue to be applied and provide useful data on the evaporation characteristics of any given system, once_ initial size distribution and vapour pressure data are known. It is well to recall that for spray dryer design, considering the evaporation of the largest droplet in the spray will generally suffice in sizing chambers. 8.3. Evaporation of Droplets Containing Dissolved Solids Droplets containing dissolved solids evaporate at lower rates than pure liquid droplets of equal size. The presence of dissolved solids decreases the vapour pressure of the liquid and the vapour pressure driving forces for mass transfer are reduced. The drying characteristics feature the formation of solid material at the droplet surface, and thus differ completely from pure droplet evaporation where the droplet evaporates away completely. 8.3.1. Evaporation of Single Droplets (a) Vapour Pressure Lowering Effect With the depression of the vapour pressure of liquid containing dissolved solids droplet temperatures will increase over the wet bulb temperatures that prevail when droplets consist of pure liquid. The vapour pressure lowering effect can be illustrated by plotting vapour pressure curves on the humidity-temperature (psychrometric) chart (curves A and B on figure 8.3). Curve A represents the saturation curve for pure liquid and B represents the saturation curve for the liquid containing dissolved solids. 7 4_ Hs Iw ,A 303 Figure 8.3 can be used to obtain the droplet surface temperature. (The humidity is represented by partial pressure of water which for air-water systems equals vapour pressure when air is saturated. Vapour pressure curve for pure liquid is the saturation curve for pure liquid on the chart.) The procedure is similar to that described in chapter 3. Drawing the adiabatic saturation curve through the drying air conditions of Ta , p a , (Ha ), the intersection of the vapour pressure curve of the saturated solution estimates the surface temperature of the droplet containing dissolved solids (Ts ). Continuation of the adiabatic line will intersect the vapour pressure curve for the pure liquid, and gives the droplet temperature (T w ). ( Ts Tw ) represents the increase in droplet temperature due to the presence of the dissolved solids. If the presence of dissolved solids has negligible effect on the vapour pressure relationship (this is the case for many spray dried salts), there is little difference in the vapour pressure curves for pure liquid and the solution. The surface temperature of the droplet can be taken as the temperature of adiabatic saturation in the case of water being the solvent, or the normal wet-bulb temperature if other liquid solvents are being evaporated. (b) Effect of Dried Solid Formation in Droplets The formation of dried solid at some stage in the evaporation of a droplet greatly alters the following evaporation history. Experimentation has shown that droplets of solutions when initially contacted with drying air in a spray dryer commence evaporation at rates that are more or less constant (first drying period). Ranz and Marshall (100) showed that surface temperature of the droplet during this period can be equated to that of the saturated solution, although the droplet surface concentration can be less -1 than saturated. The average drying rate (dW/dt) (dimensions MT ) during the first period of drying can be expressed from equation (8.3) as dW 27c1cD av AT dt A of cc H, j DRYING OF DROPLETS/SPRAYS (8.46) where Da, = average droplet diameter. The first period of drying ceases when the droplet moisture content falls to a critical value, characterized by the dnitial presence of a solid phase forming at the droplet surface. Then follows the falling rate period of -1 drying where the average rate of evaporation (dW'/dt) (dimensions 1 ) is expressed by equation (8.47). H) fra <° of •:E 0_ T DROPLET TEMPERATURE Figure 8.3. Estimation of temperatures of droplets containing dissolved solids. A. Vapour pressure curve for pure liquid. B. Vapour pressure curve for saturated solution. dW' -12K,4T dt ADC P s (i.e. dW/dt dirldt x wt of dry solid). (8.47) 304 DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING Movement of moisture from the interior to droplet surface becomes less and less, due to the increasing resistance to mass transfer caused by the solid phase becoming more extensive. The rate of heat transfer exceeds that of mass transfer. The droplet begins to heat up. Sub-surface evaporation occurs if the heat transfer is sufficiently high to cause vaporization within the droplet. In spray drying operations, where the air temperature is above the boiling point of the droplet solution, the liquid inside the droplet reaches its boiling point, and vapour is formed. When the solid phase formation forms a crust around each droplet, pressures can be set up within the droplet. The effect of pressure depends upon the nature of the crust. Vapours will be released if the crust is porous, but for non-porous, the droplet may rupture or even disintegrate. Droplet residence times in the hottest drying zones are short and -if droplet temperatures do not reach boiling point levels, moisture movement within the droplet is by diffusional and capillary mechanisms. Each material shows different drying characteristics in the falling rate period. If droplets form a film of dried product at its critical moisture content and this film is highly impervious to vapour flow, the drying rate will fall sharply, and the evaporation time for complete volatile removal is greatly extended. On the other hand, if a highly porous surface is first formed, vapour continues to easily migrate to the droplet—air interface, and the drying rates only gradually fall from the value established during the first period of drying. This is illustrated in figure 8.4. Droplets can form into a variety of shapes ; ruptured, expanded, collapsed, fragmented. For each shape, drying in the falling rate period undergoes different rates. I MPERVIOUS CRUST FORMATION POROUS CRUST FORMATION EVAPORATION H DROPLET EVAPORATION COMPLETED TO REQUIRED LEVEL EVAPORATION TIME Figure 8.4. Effect of crust properties on evaporation times. 305 Charlesworth and Marshall (115) have illustrated shape and composition changes that spray dried droplets can undergo. Shape and texture of the dried particles fall into two groups. Each group depends upon whether the drying air temperature is above or below the boiling point of the droplets. The characteristics of the two groups are shown in figures 8.5 and 8.6. (c) Droplet Evaporation Times Droplet drying times are equal to the sum of evaporation times in the constant and falling rate drying periods, and are calculated using equations (8.46) and (8.47). This requires data on the initial droplet diameter (D 0 ) and the droplet diameter at the critical moisture content (D o ). Four methods are available to determine the shape change factor, and hence (D o). (i) Experimentally determine the decrease in droplet size by observing evaporating droplet until the critical moisture point is reached. (ii) Determine the wet spray size characteristics (for convenience use a mean size parameter) and compare with the mean size parameter obtained from a dried powder sample. Manual sizing of individual particles will offset sizing errors due to non-spherical particles, but as this is time consuming sieve analysis of powder is often used. It is a convenient method but cannot differentiate between shape configurations. (iii) Estimate a value, as 60-80 % of initial droplet diameter. (iv) Use moisture content determination to calculate ratio of droplet to dried particle diameter (22). See also example 8.4. The critical moisture content is obtained from the moisture originally occupying the droplet volume lost during the first period of drying. Subtraction of this value from the initial moisture content realises the critical moisture content. One value can be used to define the critical moisture content of all droplets in the spray. This is justified as Charlesworth and Marshall (115) showed that for any solute the average critical moisture content of a droplet has approximately the same value for all droplets, and is independent of the initial droplet diameter, initial solute concentration and drying conditions. The droplet surface temperature (Ts ) is calculated from the humidity chart for the solution. If crystals are formed at the droplet surface, the temperature can be calculated according to Williams and Schmitt (116). Calculation of evaporation times based upon equations (8.46) and (8.47) is illustrated in example 8.3. EXAMPLE 8.3. A 45 % by weight aqueous solution of a dissolved salt is spray dried to a product of 4 % moisture. The inlet and outlet drying air temperatures are 350°F and 176°F. Calculate the drying time for a droplet of 196 micron. The droplet undergoes a 10 % shrinkage during evaporation and the critical moisture content occurs at 30 % moisture content. NO CHANGE BUBBLING MINOR FRACTURE LESS POROUS RIGID - z MAJOR FRACTURE -- LIQUID INITIAL RARTVAL COMPLETE DROPLET SOLID CRUST CRUST a - COLLAPSE SKIN REFORMS - f NFL A TII'JG NON POROUS PLASTIC --- 0 THE PROCESS STAGES OF SPRAY DRYING ...POROUS RIGID CON T/NUED INFLATION - BUBBLING - - COLLAPSE -- BLISTERING - 0 SPONGE-LIKE Figure 8.5. Characteristics of droplet undergoing drying (drying air above boiling point). Based on Charlesworth—Marshall (115). STRUCTURE OF CRUST R4G10 NO CHANGE NO CHANGE LESS POROUS RIGID INITIAL PARTIAL COMPLETE LIQUID CRUST DROPLET SOLID CRUST — NO CHANGE — FRACTURE _CRYSTAL FUR . GROWTH PLIABLE Am. —COLLAPSING --- —SHRIVELLING Figure 8.6. Characteristics of droplet undergoing drying (drying air below boiling point). Based on Charlesworth—Marshall (115). SAV/IcIS/SITIcIMIG 40 DNIAX ❑ r POROUS 308 THE. PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS Data 3 density of liquid droplet = 1.03 g/cm density of dried particle = 0.55 g/cm 3 latent heat of vaporization = 970 BTU/lb thermal conductivity of liquid droplet = 0.38 BTU/hr ft 2 F/ft thermal conductivity of drying medium = 0.0172 BTU/hr ft 2 ° F/ft droplet temperature from humidity chart = 103°F (a) Constant Rate Period (first period of drying) t ° , r , Average rate of evaporation is given by equation (8.46) (b) Falling Rate Period (tf.r. ) Average rate of evaporation is given by equation (8.47). Assume droplet temperature rises to 140°F. Air temperature falls 250°F 176°F. Logarithmic mean temperature difference = 78° F. Substitute in equation dW' dW dt 2n0.381186 x 101 192 970 30.5 Initial moisture content of droplet (grams) 4 196x10 3 2 -43 4)3 1-03 2.23 x 10' Solid content in droplet (grams) 41196 x 1013 0-45- 1.03= 1.82 x 10 -6 2 Moisture content at critical point (30 % by weight) (grains) 6 1.82 x 10 - 30=) 7.8 x 10' ( 70 Moisture removed (grams) (2.23 - 0.78)10 -6 = 1.45 x 10 -6 t„ 1.45 x 10 -6 = 1.1 x 10 -5 hr (0.04 sec) 131 x 10- = 106 x 103 dW dW' x (wt of dry solid) = 1.06 x 10 dt = dt = 4.25 x 10 lb moisture lb dry solid/hr -6 lb/hr(19.4 x 10 -4 3(1.82 x 10-6 454 ) g/hr) Moisture content at commencement of falling rate period (grams) 7.8 x 10 -7 Final moisture content (grams) (7.8 - 0.759) x 10' = 7.04 x 10 (where 1 ft = 30.5 cm) = 28.8 x 10 -5 lb/hr (1.31 x 10 -1 g/hr) 12 x 0-0172 x 78 -4 970( 177 x 10 ) 2 0-75 x 62.5 30 . 5 \ 3 The average density of droplet during this period is taken as 0.75 g/cm . Now evaporation rate Initial droplet diameter = 196 micron Critical droplet diameter = 177 micron Average droplet diameter = 186 micron Assume air temperature falls 100°F during this period, i.e. 350 250°F. Droplet temperature = 103°F, and the logarithmic mean temperature difference (by equation (8.6)) = 192 ° F. Substituting in equation 309 -7 Hence -7 7.04 x 10 = 362 x 10 -4 hr (1.3 sec) tfr = 194 x 10 -4 ' Total drying time = 0.04 + 1.3 = 1.34 sec. 8.3.2. Evaporation of Sprays Containing Dissolved Solids Theoretical considerations of heat and mass transfer of single droplets apply to sprays of droplets. The extent of vapour pressure lowering due to the presence of the dissolved salts will vary per droplet size. Resistances to moisture transfer will also vary, as the solid phase will not appear simultaneously throughout the size distribution. Methods of spray evaporation analysis are highly complex, and investigations in this field are limited. Dloughy and Gauvin (117) are among the few investigators to study specifically evaporation of sprays containing dissolved solids. They showed that the total spray evaporation time could be predicted with a fair degree of accuracy by employing a step-wise method of calculation. Baltas and Gauvin (118) have shown that application of computer programming to stepwise techniques offers the most promising method of evaluating evaporation histories. Baltas and Gauvin studied evaporating sprays of sodium nitrate. Many of the difficulties of the spray dryer system that require simplifying assumptions (often unrealistic) were overcome by 310 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS the selection of a simple system of spray movement at terminal velocity in the free fall zone of a single nozzle dryer. The computations were nevertheless complex, and they indicated that the difficulties in accurate prediction of spray evaporation was not in the ability to programme the complicated features of spray dryer operation (e.g. swirling air flow, temperature gradients, multiple atomizers, chamber shape) but in the inability to obtain representative data of these parameters for including in the programming, 8.4. Evaporation of Droplets Containing Insoluble Solids Feeds of insoluble solids form slurries and pastes (hereafter referred to as suspensions). There are negligible vapour pressure lowering effects in droplets containing insoluble solids and the temperature can be put equal to the wet bulb temperature of pure liquid droplet during the first period of drying. Total drying times of droplets containing insoluble solids can be evaluated by dealing separately with the two drying periods. Drying times for the first period of drying are short compared with the following second period, but in calculations where the first period is not considered negligible, Ranz and Marshall (100) have reported equation (8.8) applicable, where K d is the thermal conductivity of the evaporating liquid. The drying time for the falling rate drying period cannot be reliably expressed in equation form. It depends upon the nature of the solid phase. Ranz and Marshall (100), however, have proposed a relationship in terms of the critical moisture content (140, where tf, ADePs(We — W2) 2,1) Ps(We 6/0 Tay — W2) 12.K,A Tav (8.48) where W2 = final moisture content of the dried particle, Kd = thermal conductivity of drying medium. For drying of droplets at low Reynolds number, and negligible vapour pressure effects, the total time according to Marshall (108) can be expresSed by adding equations (8.8) and (8.48). ttotal APIM 81Cd (Ta — Ts ) + AD!Ps(Wc — 1412) 12.K,ATa , (8.49) Equation (8.49) represents the evaporation history in its most simplified case. However, calculated values give close agreement with actual evaporation times in many instances and thus the equation is useful for obtaining data for spray dryer chamber design. For a known flow pattern within the chamber, the minimum residence time for spray evaporation can be cal- 311 culated, i.e. the time to evaporate the droplets to a state of dryness for prevention of semi-wet product build-up on the dryer walls. In applying equation (8.49) the thermal conductivity is calculated at the mean film temperature surrounding the evaporating droplet. The film temperature can conveniently be taken as the average between the exhaust drying air temperature and the droplet surface temperature. The droplet surface temperature is the adiabatic saturation temperature of the suspension spray. The surrounding air temperature at the end of the first period of drying is usually unknown. The driving force (AT) over the entire period is most conveniently taken as the logarithmic mean temperature difference between the inlet air temperature and the slurry feed temperature, and the exhaust air temperature and the droplet surface temperature at the critical point. The driving force (AT) for the falling rate period can be taken as the difference between the exhaust air temperature and the droplet surface temperature at the critical point although the surface temperature will rise during the falling rate period. Alternatively air temperature at the droplet critical point and droplet temperature rise during the falling rate period can be assumed. The logarithmic mean temperature difference is applied to both periods of drying. The droplet diameter at the critical point (D c ) is usually an unknown value. Ideally this value requires data on the evaporation characteristics of the suspension droplet to enable determination of droplet size change before solids form at the surface. In the absence of such data, the methods described under evaporation times for droplets containing dissolved solids (page 305) can be applied. The factor is taken to express the percentage decrease in droplet diameter during the first period of drying. Droplet size change is then considered negligible during the second period of drying. Example 8.4 illustrates a method for calculating evaporating times of suspension droplets. The shape change factor and critical-moisture contents are calculated from initial and final droplet/particle moisture contents. EXAMPLE 8.4 A slurry containing 40 % by weight of insoluble solids is spray dried to a moisture content of 1.5 %. Inlet and outlet dryer temperatures are 860°F and 200°F. The saturated droplet surface temperature estimated from the psychrometric chart is 148°F. Calculate the evaporation time for a 300 micron droplet in the spray. Data Density of slurry (p w ) = 76 lb/ft' Density of dried product p d = 50.2 lb/ft' Feed temperature of slurry = 80°F Mean thermal conductivity 2 of gaseous film around droplet = 1.375 x 10' BTU/hr ft /ft °F 312 DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING The temperature profile of air and droplet through the dryer is established. Air temperature falls rapidly on contact with the spray, but the rate of decrease becomes less and less as the outlet temperature is approached. The droplet temperature initially rises from the slurry feed temperature to the saturated surface temperature, fixed by the humidity conditions of drying air on contact with the spray. The droplet temperature is considered constant during the first period of drying (t c. ,..). The droplet temperature increases slowly during the second period of drying (t f „..). A likely profile for the given example is given below in figure 8.7. 313 AT = (air) 860°F 350°F 148° F (droplet) 80°F LMTD = 426°F 2 1 t 970 x 62.3[(9.8 2 - 8.35 ) '13600 8 x 0.01375 x 426 ,, = 1.2 sec (b) Second period of drying (t Er. ) Substituting values in equation (8.48). Moisture content at critical point (W c). 3 Decrease in value due to 15 % shrinkage = *7[D' (0.85D) ] CRITICAL POINT(c) 1000 860-F- Ta TEMPER ATU RE i 800 600 350 • F = Tac n 3) = 0.386( — 6 70 Moisture removed = 0 386 ( - )th . 6 70 400 3 Moisture remaining = —6 -(0 6p w 0.386th) AIR 148.F Tel 86F= TI C 3 200 = 200 - F DROPLET = 175- F d Critical moisture content = (70 3 /6)(0-6p, - 0.386th) o 3 (P i = 62.3 lb/ft ) DRYER INLETii) DRYER OUTLEToi Figure 8.7. Temperature profile in example 8.4, T. = air temperature, Td = droplet temperature. Droplet Size Change During Drying Moisture content of slurry = 1.5 lb/lb dry solid Moisture content of dried product = 0.0152 lb/lb dry solid Substitute values in equation (8.51) DD 76 (1 + 0.0152)1 1 / 3 = 0.85 x D w - 50.2 (1 + 1.5) Droplet size shrinkage = 15 %. (a) First period of drying (t° , r• ) Substituting value in equation (8.8) D i = 9.8 x 10 -4 ft D c = 8.35 x 10 -4 ft OrD 3 16)0.4p, 0.386pi = 1.5 - 04, p = 0.7 lb/lb dry solid AT = (air) 350°F -* 200°F 175°F (droplet) 148°F LMTD = 94°F 970(0.7 - 0.0152) x 50.2(8-35 x 10 t fr 12 x 0.01375 x 94 -4 2 ) 3600 = 5.4 sec Total evaporation time = 1.2 + 5.4 = 6.6 sec 8.5. Drying in Media Other Than Air Air is the drying media most widely used in spray drying operations, but operations are becoming more frequent where drying is carried out in an inert atmosphere. Nitrogen or superheated steam are used in cases of extreme explosion hazard promoted by presence of solvents in the feed. DRYING OF DROPLETS/SPRAYS THE PROCESS STAGES OF SPRAY DRYING Use of inert atmospheres will demand performing the spray drying in a closed-cycle system to limit gas usage and recover feed solvents, The effect of gaseous media on evaporation rates and the comparison between air and inert atmospheres on drying rates can be observed by inspection of equations (8.20a, b) where the mass and heat transfer around a sphere is given. For any gas having a higher diffusivity and thermal conductivity than air, there will be an increase in the rate of droplet evaporation. For low viscosity gases, the Prandlt number increases accordingly. 8.5.1. Drying in Gases When evaporating in light gases (for example, hydrogen), the rate of evaporation is much higher than in air due to the higher rates of diffusion and thermal conductivity. This advantage of light atmospheres is counteracted by droplet trajectory being more extensive than in air. Evaporation times may be considerably faster, but terminal velocities are correspondingly higher, resulting in little change in overall dryer dimensions for a given evaporative capacity. S.5.2. Drying in Superheated Vapours The mechanism of droplet evaporation in drying media of superheated vapours is one of negligible mass transfer resistance and the droplet temperature approximating to the saturated vapour temperature, equivalent to the dryer operating pressure. The mechanism differs from evaporation into gases, where droplet temperatures are not so high, only equivalent to wet bulb temperature levels. Proposals for use of superheated vapours instead of gases or air in spray drying arise from (a) marked improvement in the thermal efficiency of the drying operation, and (b) the provision of inert atmospheres, where product oxidation and likely explosion hazards are prevented. Use of superheated vapours enables the volume of drying media leaving the dryer to be smaller than when using gases. For materials of poor heat conductivity superheated vapours prove effective drying media. However, heat degradation of product will occur if the product is sensitive to temperatures above the boiling point of the liquid phase at the pressure of the drying operation. This is shown in figure 8.8 where droplet temperature during droplet evaporation in superheated vapour is compared with that in air. Problems of condensation at the dryer outlet and within the product separation equipment arise when superheated vapours are used as drying media. Correlations (equation (8.13)) for predicting heat transfer coefficients of evaporating droplets in gases also apply to droplet evaporation in the presence of superheated vapours (374). Evaporation and drying of droplets in superheated vapours has been studied by Trommelen and Crosby (374). 315 BOILING PONT OF SOLVENT AT DRYER PRESSURE TEMPERATU RE 314 WET BULB TEMPERATURE FEED TEMPERATURE EVAPORATION TIME Figure 8.8. Temperature of droplet undergoing evaporation in air and superheated vapour. A. Evaporation in superheated vapours. B. Evaporation in air. 8.5.3. Drying in Superheated Steam Evaporation of aqueous droplets into superheated steam is only determined by heat transfer to the droplets. There is no diffusional mass transfer in the gas phase (107). Heat transfer rate is the limiting factor to volatiles removal. Droplet surfaces are much higher than when evaporation takes place in air. Actual temperature values depend upon steam pressure. The heat transfer rate into steam is somewhat lower than into air. The Prandlt numbers are almost identical (Pr air = 0.74, Prsteam = 0.78). The heat transfer coefficients are given by equation (8.50) 2 ---5_,= _-(8.50) h e (s [ eam) = hc(air) x 3 Re m , 0 ' 5_ It follows from equation (8.50) that the heat transfer coefficient in steam is approximately 15 % less than the coefficient in air. Overall evaporation rates are lower with superheated steam than with air at 212° F (100° C). At ° temperatures of 752°F (400 C) rates in air and steam become virtually equal. Dried products of high bulk density often result from evaporation in superheated steam. The main problem with applying superheated steam concerns condensation, especially at the dryer outlet and product handling equipment. Operational difficulties often outweigh any improvements in the dried product properties obtained by employing drying atmospheres of superheated steam. Moreau and Passey (472) report successful application. A comparison of evaporation rates for aqueous droplets in air and superheated steam are given in table 8.7. • 316 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS 0.8 Table 8.7. Evaporation of Aqueous Droplets in Atmospheres of Air and Superheated Steam (after Trommelen—Crosby (374)) Air Superheated steam 1250 395.6 118.4 6.1 0.54 5.26 x 10 -2 1260 392.0 208.4 6.25 0.405 416 x 10 - 2 317 U 8.6. Dried Product Properties on Completion Of Drying 8.6.1. Effect of Operating Variables on Product Properties (Particle Size and Bulk Density) Each operational variable of the spray drying process influences dried product properties. The extent of each influence depends upon the product. However, general conclusions can be drawn. (a) Effect of Feed Rate Increase of feed rate at constant atomizing and drying conditions increases particle size (see figure 6.7) and bulk density of the dried product. There need not be any change in the deviation of the particle size distribution. (b) Effect of Feed Solids Increase in feed solids increases the particle size of the dried product. As feed solids are increased at constant drying temperatures and feed rates, the reduced evaporation load will result in products of lower moisture content. There will be greater tendency for such rapid moisture evaporation that hollow dried particles result and overall bulk densities are lower. However, this does not always occur because this effect is counteracted to a certain extent by individual spray droplets being larger and the weight of moisture per given droplet remaining approximately the same. The variation of bulk density of spray dried coffee extract with increased solids is reported by Duffle and Marshall (22), and Crosby and Marshall (119). The effect of feed solids on bulk density of various spray dried products is shown in figure 8.9. (c) Effect of Feed Temperature Increase in feed temperature has an effect on dried product properties if lower feed viscosities are required for adequate feed pumping and atomization. For low viscosity liquids at room temperature levels, increases in feed temperature have negligible effect. Increase in temperature will tend to decrease the total heat requirement for spray evaporation, but the subsequent increase in feed heat content remains small compared with the heat requirement for vaporization. , 0.6 BULKDENSITY OF SPRAY DRIED PRODUCT Droplet diameter (micron) Air temperature (°F) Droplet temperature (°F) Relative velocity (ft/sec) Rate of heat transfer (BTU/hr) Rate of evaporation (lb/hr) 0.4 0.2 0 10 20 33 40 50 60 70 SOLIDS CONTENT IN FEED %. Figure 8.9. Effect of feed concentration on bulk density of spray dried products (results of 95°C, 116°C (Duffle, various investigators). a, b, Water dispersible dye, t i = 493°C, t r = 20°C (Wallman, Blyth, 40); d, Sodium Marshall, 22); c, Sodium silicate, t ; = 260°C, silicate (Lamont, 370); e, Sodium silicate (Reavell, 371); f, gelatin (Lamont, 370); g, Soap (Jones, 372); h, Coffee, t i --- 212-215°C (Crosby, Marshall, 120). Duffle and Marshall (22) report a trend of decrease in bulk density with feed temperature increase for products forming spherical hollow particles, but they present literature data that show an inconclusive effect. (d) Effect of Surface Tension Surface tension effects vary widely for each product. However they are rarely pronounced. Surface tension values of most feeds for spray drying fall within a range too narrow to have much influence on dried product properties. Surface tension effects dried product properties by influencing the mechanisms of atomization and drying. Low surface tension feeds produce smaller spray droplets. Sprays contain an increasing proportion of very fine droplets and spray distributions tend to become wider. Larger droplets will dry, with the likelihood of hollow particle formation and low bulk density. The fines fractions are dried to lower moisture levels. Their blending in with the remaining product maintains bulk densities as high as possible. High values of surface tension produce larger droplet sizes, 318 THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS and size distributions tend towards being narrower. There is little difference between the bulk density of products, having their natural surface tension and products obtained from feed material of lower surface tension through addition of surface wetting agents (at identical feed solids composition and drying conditions). (e) Effect of Inlet Drying Temperature The effects of drying temperatures depend upon the drying characteristics of the products. For droplets that tend to expand on drying, larger particles of decreased bulk density result from increased drying temperatures. This has been substantiated by Duffle and Marshall (22) and is shown in figure 8.10. If however, the temperature increases to the extent that evaporation becomes so rapid that the droplets puff, fracture or disintegrate, the resulting fragments CD 0 a. 0.8 0 w TY OF SPRAY cc 0.6 319 compact to form higher bulk density powders. The effect of inlet drying temperature on the bulk density of coffee extract has been reported by Crosby and Marshall (119). (f) Effect of Spray Air Contact Velocity Increase in contact velocity between spray and air will create increased mixing that will increase heat and mass transfer rates. At very high velocities, droplet shape distortion may occur, droplets may fracture and even disintegrate or coalesce through impact with other droplets in turbulent flow motion. With increased velocity, evaporation times become shorter, dried product particles exhibit irregular shapes. Any bulk density change will vary according to the product. There is no general trend. 8.6.2. Formation of Hollow Particles The tendency of expansion and formation of hollow particles plays an important role in the final bulk density of dried product. Hollow particles can be formed from four mechanisms. (a) A surface layer, semi-impervious to vapour flow forms at the droplet surface. The droplet puffs out as vapour is formed within the droplet and expands with the increase in droplet temperature. (b) Moisture evaporates at a rate, faster than the diffusion of solids back into the droplet interior. On completion of evaporation, air voids are present, especially in the case of crystalline products. (c) Liquid flows with accompanying solids to the droplet surface by capillary action. This leaves the centre of the droplet as a void. This mechanism is applicable to clay slip feeds. (d) Air entrained in the feed contributes to air spaces within the droplet. — 0.4 8.7. Size Differences hilti'ieen Product before and after Drying tfr Lu 0.2 -J CD CO 0 100 200 30D 400 500 INLET DRYING AIR TEMPERATURE 600 PC Figure 8.10. Effect of inlet drying air temperature on bulk density of spray dried products (results of various investigators). a, Sodium silicate, 25 % 60°C (Duffle, Marshall, 22); b, Sodium silicate, 25 % 20°C (Wallman, Blyth, 40); c, Sodium silicate (Lamont, 370); d, Water dispersible dye, 19.5% 95°C (Duffle, Marshall, 22); e, Dispersing agent, 36% 80°C (Duffle, Marshal], 22); f, Soap (Lamont, 370); g, Gelatin (Lamont, 370); h, j, Santomerse, 20 % (Chu, Stout, Busche, 373); k, Coffee extract, 22 % (Crosby, Marshall, 120); m, Sodium sulphate, 20 % 80°C (Crosby, Marshal], 120), Evaporation calculations use the estimation of dried particle diameters at the end of the first period of drying to represent the dried product diameter. This assumption is valid for products whose surfaces are completely porous to moisture flow. Inorganic salts come into this category. However, there are many spray dried products whose dried product shape characteristics have not been finalized until well into the second period of drying. Final particle size and density for these materials are often difficult to predict and the exact relation between wet spray and the resulting dried powder requires experimental determination over a range of drying temperatures and feed solids concentration. The droplet size on atomization depends upon the mode of atomization, physical properties of the feed, feed solids concentration and applied drying temperatures. The particle size on completion of evaporation depends upon the dried product properties. Shape and size changes will differ THE PROCESS STAGES OF SPRAY DRYING DRYING OF DROPLETS/SPRAYS according to whether the droplet has an amorphous, granular or colloidal form. The size changes that occur during evaporation can be expressed in a mass balance over the droplet on dry solids basis. Thus : Initial solid content per spherical droplet (subscript w) = p 6 (1 +1- W, Final solid content per dried droplet (subscript D) 1 = — 6 7ED D- p 11)( 1 1 w2 ) WEIGHT DISTRIBUTION OF SPRAY 60 40 20 180 D, 1(1 + W2) 1 P o (1 + WI ) x 1] 113 - x 160 DROPLE DIAMETER (8.51) 80 0 (microns) 160 PARTICLE DIAMETER 240 For the majority of spray dried products, W2 is low, so that 1/(1 + W2 ) tends to unity. Denoting 1/(1 + W) as C, the weight fraction of solids per unit weight of product in dried particle equation (8.51) becomes I3 D,= [PD x CD TD i, p, C, WEIGHT DISTRIBUTION OF PRODUCT 80 The ratio of diameters can thus be expressed DD 321 100 CUMULATIVE PERCENT LESS THAN 320 (8.52) All droplets are taken to contain the same proportion of solids. 8.7.1. Procedures to Predict Dried Particle Size Distribution (a) Graphical Method The weight distribution of a spray dried product can be conveniently predicted from the wet spray data using the graphical method of Crosby and Marshall (120). This is shown in figure 8.11 for the case of sprays that undergo size decrease during evaporation. The relationship between wet spray droplets and dried particles is given by equation (8.52). The wet spray size distribution is determined by micro scope size analysis or represented directly as a distribution function if the atomization characteristics of the given atomizer follows a known distribution law (chapter 6). Conversely the initial spray can be predicted from a size distribution of dry product by sieve analysis. (b) Mathematical Prediction It follows from equation (6.32) that for every product, the wet spray size equals the dried particle size times a factor 13 that depends upon the product's physical characteristics, drying temperature and the initial and final moisture contents. D W = AD D (6.32) C _ 45° Z X160 if 80 w 0 cc 0 0 80 160 PARTICLE DIAMETER (microns) RELATIONSHIP BETWEEN DROPLETS AND DRIED PARTICLES Figure 8.11. Graphical determination of size distribution of dried product from that of wet spray. Equation (6.32) has been discussed in relation to atomization in chapter 6. f can be estimated for an individual product, and can be used when predicting plant performance. Prediction of plant performance by experimental determination of such a factor has been reported by Moore et al. (121) for non-soapy detergents. From work in a nozzle tower (6 ft diameter, 30 ft high, 1.8 m dia x 9 m) the size of the dried product was found larger than the droplet in wet form. The shape factor was expressed as a volumetric expansion factor. Experimental data established a relation between the volumetric expansion factor, the outlet dryer temperature and wet spray droplet size. The relation led to an interpretation of the evaporation events leading to the droplet shape 322 THE PROCESS STAGES OF SPRAY DRYING change during drying. These events were listed as (a) rate of heat transfer to droplet, (b) rate of heat loss by evaporation, (c) effect of droplet size on the amount of expansion caused by the generation of a given amount of vapour within the droplet, (d) modification of film properties and rate of formation of the surface film due to changes in drying temperature and (e) reduction in volume during the early stages of drying due to loss of moisture. The work (121) serves as an example of how mathematical predictions of product characteristics from large dryers can be carried out from data obtained experimentally on a pilot plant unit. EXAMPLE 8.5 A product is being spray dried as a slurry of 35 % solids. If the feed concentration is to be raised to 50 % solids, what changes to the atomization stage must be made to maintain the same dried particle size? The relation (f) between the wet and dried product size can be taken as established in terms of initial moisture content, where # = 1.5 — 0.015 100/(1 + 0.01 W). (W is percentage moisture, dry basis.) At 35 % solids W.H= 185% At 50 % solids W.H= mo% Hence #35 = 1.5 — 0.015 100 2 .85/ = 1.5 — 0.53 = 0.97 100 )51 50 = 1.5 — 0.015( —) 2.00 = 1.5 — 0.75 = 0.75 From equation (6.32) D w , = /3 2 /fl 1 x D w 1 (D, is constant). For dried particle size to be the same, atomization conditions must be changed to obtain a reduction in wet spray size. Wet spray size must be reduced by 0.75/0.97 to 0.774D w . 8.8. Size Distributions of Wet Sprays wad Resulting Dritd -Particles Size distributions of dried particles are mostly narrower than the size distribution of the atomized wet spray. This has been established over a range of feed temperatures and feed concentrations by Crosby and Marshall (119) (120) for materials whose drying characteristics exhibit crystalline, surface film forming and capillary mechanisms. In cases where the distribu- DRYING OF DROPLETS/SPRAYS 323 tion of the wet spray more. or less follows a well-established distribution function, the distribution of the dried particles shows marked deviation from the function. If the wet spray is represented by the square root normal function, the dried particles more clearly become represented by the lognormal distribution. Wet spray and dried particles follow the same distribution function only for low drying temperature and low feed solid conditions. Experimenting with (a) sodium sulphate (drying characteristics representative of a crystalline product), (b) coffee extract (drying characteristics representative of a film forming mechanism) and (c) clay slips (drying characteristics representative of a capillary mechanism), Crosby and Marshall (120) found the dried particle size did not exceed the wet spray size. The difference between the mean sizes of wet spray and dried particles show different trends when feed solids concentration is changed at constant inlet temperature. For crystalline products, the difference between the mean sizes decreases as feed concentration increases towards saturation. The effect becomes less pronounced at low drying air temperatures and high feed temperatures. For products characterized by their film forming properties, there is little difference between the mean sizes at 'high feed concentration. At low concentrations, however, the difference is significant. Decrease in feed concentrate acts to increase the difference between the mean sizes. When feed temperature is varied, any change to the difference between the mean sizes appears to be of lesser significance. Only at high drying air temperatures does feed temperature exhibit any degree of influence. SEPARATION AND RECOVERY OF DRIED PRODUCT FROM AIR 9 Separation and Recovery of Dried Product from Air 325 a. 9.1. Introduction The fourth and last stage of the spray drying operation is the separation of dried product from the air. Separation is followed by the removal of product from the dryer. The stage shall meet two important requirements of spray dryers ; (a) an economic dry solids recovery and (b) an exhaust free of airborne particles. Economic recovery requires recovery of product in its most useable and/or most saleable form. A clean exhaust in open-cycle dryers is the requirement for prevention of discharge of airborne powder to atmosphere in quantities that exceed local or national pollution standards. A clean exhaust in closed-cycle dryers is the requirement for drying air/gas return through the air heater without chance of scorching airborne powder. Such scorching can lead to a source of ignition or passage of dark particles into the drying chamber. Separation of dried product can be carried out firstly at the chamber base (primary product separation (discharge)) followed by separation of fines in collecting equipment (secondary product separation (discharge)). Alternatively, all product can be conveyed to collecting equipment (total product separation (discharge)) (figure 9.1). The amount of primary product separation depends upon the chamber design, atomization of product and drying air flow. ProcilIct is either seban; red out of the air by the cyclonic air flow set up at a conical chamber base, or by the ability of particles to fall out of the air flow to a flat chamber base. Whatever method of separation is used, some form of collection equipment is required after the drying chamber. Collection equipment can be dry or wet types, e.g. cyclones, bag filters, scrubbers, electrostatic precipitators. Choice of equipment (see later, 9.2) is based primarily on cost, collection efficiency and product treatment undergoing separation (comminution). Equipment was introduced in chapter 5. Equipment performance is discussed in section IV. b. Figure 9.1. Product discharge from conical and flat chamber bases. (a) Primary product dis-.barge from chamber, secondary product discharge from collecting unit. (b) Total product charge from collecting unit, 1. Spray drying chamber. 2. Product—air separation in collecting unit. 3. Product discharge. 4. Clean air. Recovery of dried product involves powder removal valves to discharge powder into silos, packing machines or conveying systems. Valve selection depends upon whether intermittent or continuous discharge is required. Manual, flap or rotary valves can be used. Further details are given in section IV. For dryers with primary product discharge, the degree of separation in the drying chamber is closely connected with the location and design of duct leaving the chamber. This is especially so for chambers with a conical base. Eight such exhaust arrangements are shown in figure 9.2. The arrangement selected depends upon the product form and collection equipment installed. The arrangement giving a very low powder loading need not necessarily be the most suitable. With cyclones, for instance, a very low loading of 'fines' results in low collection efficiencies and appreciable loss of fines. Using higher loadings of powder including slightly large particle sizes would recover some of these fines due to the ability of large particles 326 THE PROCESS STAGES OF SPRAY DRYING to entrain or agglomerate fines that would otherwise be lost. Of the arrangements shown in figure 9.2, those in which air is made to turn 180° (types A, F, 0, H) to enter the duct give higher powder carry-over (hence lower chamber separation) than those requiring only a 90° or less turn. This is. particularly the case with type A as this arrangement has the duct inlet in an area of high powder loading. Types F, G and H are not so prone to higher powder carry-over as they are incorporated with nozzle atomizers producing coarser sprays. Figure 9.2. Exhaust duct layouts with primary product discharge from conical chamber base. Type A features a downward facing outlet projecting deep into the conical base. With the close proximity of the wall, and the air velocity increase on approaching the duct entrance, the arrangement is susceptible to re-entraining powder that has already separated out at the walls or base. Re-entrainment effects can be severe where air leakage in at the chamber base (chamber operating under atmospheric pressure) fluidizes powder reaching the base discharge point. This fluidizing effect becomes of less significance to type B, where air turns through 90° and the entrance is further removed from the walls and chamber base. However, types A and B do feature favourable points. They utilize the chamber volume fully for evaporation, as the air must flow throughout the entire volume. This SEPARATION AND RECOVERY OF DRIED PRODUCT FROM AIR 327 gives maximum residence time, and enables the air flow pattern created by the air disperser to be maintained substantially throughout the chamber. The downward facing exhaust duct has a minimum interference on this air pattern, and in fact, acts to maintain the pattern down into the chamber cone. Type C, on the contrary, draws air to the side of the chamber, greatly interfering with the flow by creating a lopsided air flow pattern. Again suction is in the neighbourhood of powder present at the walls. Type C is only used when handling products that are sticky or heat sensitive or in cases where any deposits forming on the exterior surface of the projected duct is likely to create product quality deterioration and frequent dryer shut down. Type D, the upward facing duct can achieve lower levels of powder carry-over than type B, since air is drawn from an area of low airborne powder concentration. However, the chamber volume is more poorly utilized. Type E requires no air turn into the duct and the location of the duct entrance ensures even lower powder carry-over, but again utilization of the chamber volume is poor. This aspect can be improved by adding a cap to the duct (type F). The cap maintains the rotary air flow into the lower half of the chamber. The presence of the cap requires air to turn 90°. Powder carry-over increases, but the cap discourages product falling into the duct entrance. The cap attachment is only feasible for non-sticky powders. The duct arrangement causes accessibility problems for cleaning. Types G and H differ from the above as separation is achieved by educting the air from the dryer at the wall area located at the base of the chamber cylindrical section. The exhaust duct can be tangential to the wall or leave from an annular ring (plenum). With these two arrangements, air is exhausted where separated powder -congregates at the wall. Powder is continuously scrubbed by the air, and re-entrainment is inevitable. However, these arrangements are used with coarse powders, and if lower wall or plenum air velocities are maintained, primary separation of product can be very high. 9.2. Selection of Equipment for Separating Powder from Exhaust Drying Air Many spray drying applications are so established nowadays that certain types of separating equipment are connected with certain products. This has arisen from operational practice which has shown equipment to meet demands in separation performance and operational costs. While the majority of equipment selection is based upon experience, there are certain rules of selection, although these rules may at times be rather general. The desired separation efficiency depends upon the value of the product, cost of recovery, and environmental pollution codes. If the product is 328 THE PROCESS STAGES OF SPRAY DRYING SEPARATION AND RECOVERY OF DRIED PRODUCT FROM AIR expensive and/or the dryer is in an area of strict pollution control, separation (as close to 100 % as technically possible) is essential. If the product is cheap and/or the degree of recovery less critical, the efficiency is fixed at the point where cost of further recovery per unit of recovered product exceeds the value of the extra product recovered. Even though many types of separation equipment cannot approach efficiency levels of 100 %, they are nevertheless often acceptable on the grounds of suitability in the other aspects of operational convenience, costs, and degree of maintenance required. These aspects are just as important. Any limitation in collection efficiency can always be rectified by installing secondary separating equipment, whereas limitations in these other aspects are not so readily rectified. Whatever the performance, selected equipment must be able to handle the product with a minimum of attention. To justify installation of any separation equipment, (a) the separation efficiency must be acceptable, (b) the product characteristics be such to enable successful handling, (c) all operational features must fit in with those of the drying chamber operation, (d) the product itself must render the separation equipment investment and operational cost realistic, (e) the necessary space requirements must fit in with the available area designated to the separation equipment in the spray dryer plant layout. Selection based on Collection Efficiency The vast majority of spray drying installations produce particle sizes in the range 1-400 micron. If the total production is conveyed to the separation equipment, this is the range of particle sizes selected equipment must handle. If some product recovery is achieved from the drying chamber, this will remove the larger particle sizes. The selected separation equipment handles Table 9.1. Collection Efficiency of Primary Separators on Low and High Powder/Air Loadings Type Cyclones Bag filters Electrostatic precipitators Operating on Operating on low powder—air loadings high powder—air loadings 90-96% 95-99.5 % 90-99 95-99%* 97-99.9% 95-99% *This value can range over 99% in many transport cyclones (see figure 1.3, item 19) where very high powder—air loadings exist. For example, tests with a 1250 mm diameter (D) transport cyclone (wrap around inlet, cone height 2 x D) operating with an air throughput of 5700 Nm 3 /hr at 30°C has established separation efficiencies exceeding 99% when handling 1000 kg/hr dusty powder Inlet powder loading: 175 g/Nm 3 Outlet powder loading: 191 mg/Nm 3 Collection efficiency : 99.89 % 329 low powder—air loadings, where the particle sizes involved range from 1-80 micron. For this range of particle sizes, equipment available for use as primary separators (mounted directly after the drying chamber) have efficiency levels exceeding 90 % as illustrated in table 9.1. The efficiency of equipment used as secondary separators falls within the ranges : for bag filters : 98-99.99 %, for scrubber (wet) : 80-96 %. Inlet powder loadings to secondary equipment are low (under 250 mg/Nm 3 ). Inspection of the above data shows that where collection efficiency is critical (as in the case of products that cause environmental pollution even in very small quantities), bag filters must be selected and installed in the exhaust drying air either as a primary or a secondary collector. When efficiency levels are not so critical, cyclones will prove the best selection. Selection based on Product Handling Suitability The suitability of equipment to handle a given product can be assessed by noting the conditions under which the unit must operate. The unit must cope with the exhaust drying air temperature and powder properties and operate over long periods continuously. Cyclones can handle most products and operate at high temperatures. Wet scrubbers can operate with sticky products, and at high temperatures too, but have not the advantage of dry recovery of the collected powder. Bag filters are severely restricted in the operating conditions they can successfully withstand, but the handling of the finest of powders is a great advantage. The suitability of equipment types to spray drying conditions is summarized in table 9.2. It can be seen that no one type is ideal for all conditions. Selection must be made on the basis of what type best fulfils the intended application. Selection based upon Operational Features A small yet important point to bear in mind is that the operational procedure of the separation equipment must fit in with the operational procedure of the drying chamber. The equipment must operate continuously as long as the drying process proceeds. For cyclones there are no problems, as long as blockaging of the cyclone base does not take place. For bag filters, proprietary equipment must have a cleaning arrangement to enable continuous operation of the drying chamber without wide fluctuations in air throughput. For scrubbers, there are no operational problems as long as sufficient, water supplies are available, and plugging of any jets or nozzles is prevented through liquid filtering or straining. Electrostatic precipitators create few problems, as designs are developed for continuous operation over long time periods. Selection based upon Costs Costs are an important factor in all industrial operations, and this is certainly so with spray dryers where the collection of airborne powder can constitute SEPARATION AND RECOVERY OF DRIED PRODUCT FROM MR THE PROCESS STAGES OF SPRAY DRYING -0 2.3 g. j * 1 • . m .... I . • I • I I .• • 1 1 C Design used in spray drying plant 330 • • • 1• • * 1 1 1 1. * 4 * OF * • II 1 ** * • ** • 11 1 g r" v o. 1 C t, a sizeable proportion of total operating costs. The main purpose of the selected unit is to recover as much product as possible, but the level for the most economic recovery is seldom the highest, especially where product worth is relatively low per unit weight. It is obtaining the final! 04 of recovery that causes costs to soar, and thus equipment selected must strike the happy medium of operating at an optimum efficiency. To go above this efficiency level, the extra costs of recovery involved exceeds the value of the product collected. If pollution of the environment is the criteria in fixing a recovery efficiency, the optimum efficiency is that which meets the standards set up to safeguard health and local surroundings. It is very difficult to generalize on equipment cost suitability. Product handled, and plant location changes proprietary equipment suitability from place to place. Many types can have relatively low cost price, but high operational costs, or low operational costs, but low collection efficiency. A general guide to costs is given in table 9.3. As prices quickly change, costs are presented on a relative basis. Table 9.3. Relative Costs of Separation Equipment in Spray Drying (122) (Dry cyclone cost used as reference level) 2 U 2 g bf Type Cyclones Bag filters Spray chamber scrubber Venturi scrubber Impingement scrubber Electrostatic precipitator -0 u t ›. 2 * * 3 • ** • * * 11 1 if * •••* ► * 0 zt,'E .. 0OO ** 331 • • Capital costs Operating costs (including maintenance) 1 4-5 1.5-2 2 4-5 5-6 1 5-6 4-4.5 7-8 2.5-3 1 Selection based upon Space Area Requirement All types of separation equipment have differing space requirements. However, it is seldom that space limitations are such to reject a unit type if it is suitable on all other aspects of selection. With selection of equipment for new spray drying plant, the overall plant layout can be adjusted to accept any dimensions of separation equipment. There may be difficulties if a new plant has to be erected in an existing building or an old dryer modified for increased capacity or change of product, but such problems can be overcome by using two smaller units in parallel if a single unit requires too much height. It is not always limited building height that decides multiple small units. One large cyclone, for example, may handle the total air flow and achieve acceptable collection efficiency, but its sheer size can mean an extensive duct length between the drying chamber and cyclone inlet. 332 THE PROCESS STAGES OF SPRAY DRYING Two cyclones in parallel give a better layout and cyclone supporting structures can be simplified, an added advantage. The relative dimensions of collection equipment are illustrated in table 9.4 based upon design sizes to handle 70 000 m 3 /hr air at 80 ° C. Table 9.4. Dimensions of Separation Equipment to Handle 70 000 m 3 /hr air at 80° C Type Cyclones Bag filter Spray chamber scrubber Venturi scrubber Impingement scrubber Number of Dimensions (1 x b x h) or (dia x h) 2 1 1 1 1 2.8 dia x 10.5 m 4 x 1.5 x 2.5 m 3 dia x 6 m 1 dia x 12 m 1.5 dia x 6 m For further guidance on the selection of powder—air separation equipment, reference should be made to Stairmand (122) (507). Review of recent equipment is available (123) (124) and modern trends in separation is described elsewhere (125) (508) (516). 10 Control Systems Operational practice involves (a) dryer operational procedures, (b) dryer control, and (c) measurements to assess dryer performance. Operational procedures include start-up, operation, shut down, cleaning and maintenance. It is common to start up spray dryers on water (where moisture is to be evaporated from the feed solution), but this is not essential. The required inlet and outlet temperatures are established on water, after which the system is switched over to feed under either manual or automatic control. Operational procedure requires maintenance of the desired product moisture content, usually by maintenance of a set outlet air temperature. Ensuring availability of feed, and handling the discharge of powder leads to continuity of operation. Shut-down procedure often involves the change-over from feed to water for the running down of the plant without affecting the quality of product remaining in the dryer system. Cleaning procedure involves a washing cycle that achieves plant cleanliness within a minimum of time. Maintenance procedure is based upon scheduling to prevent overlooking any equipment that can cause plant shut-down through failure. Instructions for spray drying plants differ from product to product and from design to design. Instruction manuals for a given dryer application are available from dryer manufacturers. • Methods of dryer control depend upon dryer design and product. Control systems are discussed in chapter 10. Measurements to assess dryer performance are described in chapter 11. The aim of a spray dryer control system is the maintenance of desired dried product quality, irrespective of what disturbances occur within the drying operation and variations in feed supply. The most effective product parameter to control is the moisture content. Equipment for continuous measurement of moisture content is in an advanced state of development but as yet is not widely used. Outlet air temperature (exhaust air from drying chamber) is the parameter controlled. This temperature represents product quality, i.e. bulk density, colour, flavour, activity as well as moisture content. Spray dryers can be controlled either manually or automatically. Manual control is applied to small plant (laboratory, pilot-plant or small industrial sizes) which are operated batchwise, often on a range of products. The products must be easy to dry. Manual control can be applied to large industrial units operating on such products, but the demands of continuous operation on operating personnel, the maintenance of constant product quality over lengthy durations of production makes automatic control (semi or full) a virtual necessity. As shown in figure 10.1 outlet temperature with smaller deviations from the control setting (+0.5 to 1.0°C) are maintained over longer periods by automatic control than by manual control. If products are difficult to dry, automatic controls are utilized irrespective of dryer size. Control is accomplished by maintaining a set outlet temperature through varying (a) the feed rate to the dryer, hereafter denoted control system A, or (b) inlet drying air temperature, hereafter denoted control system B. Control system A is the more widely used of the two systems. By applying automatic control to the outlet air temperature, product moisture can be held within very narrow limits. 336 OPERATIONAL PRACTICE CONTROL SYSTEMS 4 P.M, 337 The control system is illustrated in figure 10.2. The system consists of two control loops of quick response. Quick response loops are the desired control characteristics to prevent adverse drying conditions. AIR FLUE GASES FEED wu rx,„.0.12& umv..4"- As To VARIABLE SPEED DEAR PUMP 4 INDIRECT OILFIRED AIR HEATER %A. OIL COMBUSTION MR Figure 10.2. Control system A. Outlet temperature control by regulation of feed rate. Inlet temperature control by regulation of fuel combustion rate. Figure 10,1. Outlet air temperature chart for dryer operation under manual and automatic control. Theory of automatic control is considered outside the scope of this book. For details, the reader is referred to available textbooks (126) (127). Automatic controlling and regulating systems are covered in British Standard 1523 part I (1967). Rasmussen (128) describes the design of instrumentation for spray dryer control systems. Aikman (129) reports frequency-response analysis of spray dryers. Hatfield (130) describes available control systems. Patent coverage includes (473) (474) (475). 10.1. Control System A (a) Outlet temperature control by feed rate regulation. (b) Inlet temperature control by air heater regulation. The air temperature in the exhaust duct is measured and transmitted to the temperature indicating controller (TIC), which counteracts any temperature deviations from the desired set point by varying the feed rate. The temperature of air to the dryer air disperser is measured and transmitted to a temperature indicating controller. Any deviation from the desired inlet air temperature is corrected by control of fuel and combustion air to the burner (oil and gas fired air heaters), steam pressure in a steam—air heater, or power input to an electric—air heater. In the event of failure in the feed system (pipe or atomizer blockage, pump damage, pump control failure) where feed supply to the atomizer is drastically reduced or ceases, a safety system can be installed to prevent the outlet air temperature rising above a known safety level, since the system can be potentially dangerous for many products inasmuch that feed failure can lead to rapid rise in outlet air temperature as the air heater continues to function. A built-in safety system can shut down the air heater once a certain outlet air temperature is reached, or water can be passed to nozzles positioned as safety measure, for example in the dryer roof. These nozzles 338 OPERATIONAL PRACTICE can be sized to act either as atomizer nozzles (and therefore restore the normal outlet temperature on water feed while the feed system failure is rectified), or as quenching nozzles to flood the chamber if the product under high temperature conditions can cause a fire hazard through spontaneous combustion or explosion hazard through an extremely dry dusty product swirling in the chamber. Some safety systems switch feed over to water at the feed pump and operate on a two temperature level safety system. For a partial blockage of the feed system the outlet air temperature will rise more slowly, and on reaching the first level (say 300°F (150°C)), feed supply is stopped and switched over to water. If the blockage is minor, the water flow may dislodge the blockage and after a short time when the normal outlet temperature has been restored, so can the feed supply. If the blockage cannot be removed by water, or water cannot pass to the atomizer (in cases of pump failure) the outlet air temperature will continue to rise to the secondary safety level after which the chamber is flooded by quench nozzles or the air heater is shut down or a combination of both. To draw attention to rise in outlet air temperatures, alarms can sound 20-40°F (10-20°C), before any unsafe temperature level is reached. The use of two level safety systems gives the opportunity of restoring dryer conditions on water by using water to flush out a blocked feed or enable feed system failures to be rectified. If feed system difficulties can be overcome by a short operation on water feed, time will be saved by not having to shut down and restart the dryer. 10.2. Control System B (a) Outlet temperature control by air heater regulation. (b) Feed rate held constant. The control system is shown in figure 10.3 and is used particularly for dryers with nozzle atomization where wide variations in feed rate cannot be handled. The outlet air temperature is measured and transmitted to a temperature indicating controller. To compensate for any deviation from the desired outlet air temperature, the heat input to the dryer is adjusted by the controller through regulation to the combustion rate in the gas or oil air heater (if fitted), or steam pressure at the steam—air heater (if fitted). From a theoretical viewpoint this is an inherently safe and acceptable system as any increase in outlet temperature brings about a decrease in heat input to the dryer. From a practical viewpoint, however, the system has operational disadvantages of lengthy control lags due to time lags in the heater control circuit. These time lags can increase outlet air temperature fluctuations. The system has the inability to handle effectively variations CONTROL SYSTEMS 339 AIR FLUE GASES FEED 0 PUMP INDIRECT OILFIRED HEATER VARIABLE SPEED GEAR OIL COMBUSTION AIR Figure 10.3. Control system B. Outlet temperature control by regulation of fuel combustion rate. Manual regulation of feed rate. in feed solids, but it can be improved by outlet temperature cascaded on the inlet temperature controller which controls the heater. Safety systems similar to those used in control systenLA are-used. When using a two level safety system, the rise of outlet air temperature to the first level will switch feed over to water flow to the atomizer. If water flow cannot regain and maintain the desired outlet temperature, the heater is automatically shut down. 10.3. Feed System Controls 1. Systems for Rotary Atomizers. Control system A is adopted with direct feeding from a suitable positive displacement pump with variable speed control, a centrifugal pump throttled by a control valve, or a gravity feed constant head tank with a control valve in the outlet pipe. Control system B is rarely considered. 2. Systems for Nozzle Atomizers. Both control systems are applicable, but control system B is preferred. Control system B can be applied in two ways with the feed pump on a fixed manual control setting. The outlet temperature controller can be cascaded on to the inlet temperature controller as 340 OPERATIONAL PRACTICE CONTROL SYSTEMS • r- AIR FEED FLUE GASES -------- OIL J INDIRECT OIL- FIRED AIR HEATER 341 alone for shut down and cleaning purposes. For example; for an 'air-sweep' chamber cleaning operation. An alternative system for prevention involves a vacuum switch mounted at the chamber ceiling in a powder-free area. The switch is normally set to shut down the exhaust fan if chamber pressures reach —4 in W.G. ( — 100 mm W.G.). For prevention of heater damage. An interlock ensures that the burner cannot be ignited unless the storage pump, burner fuel pump, combustion fan and dryer fans are in operation. For indirect heaters a differential pressure switch can be installed to check the correct air flow, and linked to the combustion and supply fans. Prevention of wet chamber wall. An interlock ensures that feed cannot be passed to the rotary atomizer when not running. Furthermore the interlock will cause the feed to cease on atomizer failure. Precaution against burnt product. An interlock ensures that the main dryer fans cannot be started unless the necessary cooling fans are in operation. The fans cool potential hot areas in the chamber where build-up and scorching of product can take place. 10.5. Fully Automatic Spray Dryers COMBUSTION AIR Figure 10.4. Control system for pressure nozzles (control system A). shown in figure 10,4 or linked directly to the heater. Pressure safety systems are incorporated to shut down the dryer if excessive pressures build up in the feed system due to blocked nozzle(s). Control system A can be applied in two ways. The outlet temperature controller sets the pressure control loop in the feed system or is linked directly to the feed pump. It is usual for each nozzle in a multi-nozzle assembly to be brought in manually during start-up as the inlet temperature rises. 10.4. Interlocks Interlocks are closely connected with the control and operation of the dryer. Interlocks are installed to ensure safe start-up, operation and shut down of the dryer. Some examples of typical interlocks are as follows : For prevention of drying chamber damage. An interlock ensures that an exhaust fan cannot be started before the supply fan. This is installed if there is a chance of chamber collapse under the low negative pressure conditions caused by an exhaust fan operating alone, The interlock is usually overridden when a chamber door is open. This allows the exhaust fan to operate 10.5.1. Programmed Start-up Analysis of spray dryer control systems has reached the stage when it is possible for the complete spray dryer installation to be started up from the pressing of a single push button. The swing to full spray dryer automation is motivated by the need to meet stricter product quality specifications, and hold quality levels during extended periods of dryer operation, and achieve lower running costs. The combined block and schematic diagram for a fully automated spray dryer operated on the control system A principle is shown in figure 10.5. The dryer installation features a rotary atomizer, indirect oil fired air heater, cyclone collectors and pneumatic conveying of the powder to automatic weighing equipment at the powder discharge. Control programming is through timing equipment. A sequence timer starts up the dryer in the correct order. A typical start-up sequence for a dryer with an oil-fired air heater is as follows : (a) atomizer start-up, (b) cooling fans, (c) supply fan—exhaust fan, (d) transport fan, (e) rotary valves, (f) vibratory conveyor (if fitted), (g) oil burner pumps, (h) combustion air fan, (i) flue gas exhaust fan, (j) oil burner—and at the start of product drying, electric hammers or similar devices (if fitted) on the chamber wall. With the initiation of the heat source to the dryer, a series of process control follow automatically. Dryer feed is usually initially water, which continues until (1) a temperature equilibrium has been reached in the dryer 342 OPERATIONAL PRACTICE CONTROL SYSTEMS _J 343 (inlet and outlet temperatures at desired level), and (2) there is sufficient product in the feed tank to ensure continuity of operation. Once these two conditions have been fulfilled, an air operated three-way valve changes the feed automatically from water to feed product. The changeover is smooth and little deviation occurs to the outlet temperature apart from the effect of initial feed dilution in the feed line. The outlet temperature is controlled by the feed rate and the inlet air temperature by the oil combustion rate. Any fall in inlet temperature is counteracted by the servomotor introducing greater quantities of oil and combustion air for an increased combustion rate, and vice-versa for any rise in air temperature. Temperature deviations are within 1-2°F (0.5-1.0°C). Such control contributes greatly to product quality. The success of any fully automated system is reliability in operation, and the ability of the control system to deal with failure on the dryer installation. Reliability is met by the use of established robust equipment whether pneumatic, electrical or mechanical in operation. Where fault in equipment does occur, interlocking and alarm systems limit operational dangers by shutting down appropriate plant items and indicating the type of failure. In the case of the layout depicted in figure 10.5, for example, a feed-back system will prevent an operation from starting if the previous step is faulty. If a motor fails during the start-up sequence, after the motor has received the start-up impulse from the sequence timer, a control lamp will light up to give visual indication of the fault. However, as the sequence timer proceeds with the programme and submits the start-up impulse to the next step, a feed back interlocking system is brought into operation. This means the following step will not be started. Further protection against continued start-up in a manner dangerous to the drying equipment is afforded by interlocking the different start-up steps. Although the start-up steps proceed automatically, the plant operator can follow the switching-in sequence as a light comes on for each equipment item in operation. This light is extinguished in cases of faulty equipment operation, and a red lamp comes on to indicate the type of failure. Faults in the system are also made known to the operator through siren alarms. Faults covered by siren alarms can be faulty lubrication in a rotary atomizer, excessive outlet temperature level, or low feed tank levels. It is common for the alarm to sound after a short delay (5 sec) following a failure lamp signal, since in many cases the failure lamp signal is due to a temporary condition, e.g. a valve change-over at the feed tanks. In such cases there is no need for the alarm signal to sound. If a fault does occur in the control equipment itself, it is possible to switch over to manual control and continue the production. Shut down and cleaning programmes operate in a similar way via the sequence timer. 344 CONTROL SYSTEMS OPERATIONAL PRACTICE The adoption of the above system to the spray drying of milk has been reported (131). 10.5.2. Full Automation of Spray Dryer and Feed Pretreatment The full automation of the spray dryer as described above will maintain a uniform product quality as long as input feed compositions do not vary widely during operation. To reduce variations in feed solid concentration, attention must be paid to the pretreatment section that supplies the spray dryer. The maintenance of constant feed solids to the spray dryer is best achieved by coupling the pretreatment section to the spray dryer and applying control system analysis to the two parts as one unit. The coupling of an evaporator (pretreatment section) to the spray dryer has been achieved within the dairy industry. Notable advantages achieved, apart from control of feed conditions to the dryer include the elimination of intermediate feed tanks and great precision in the dosing of additives. Feed concentrate does not come into contact with ambient air. C d b Figure 10.6. Automatic feed solids content measuring equipment used in fully automatic spray drying plant in the dairy industry. (By courtesy of Niro Atomizer.) 345 The control parameter is the total solids in the feed concentrate leaving the evaporator and is based upon the continuous measurement of density, or continuous weighing. Systems are based upon hydrometer measurement, refractometers or electronic sensors but all have disadvantages to various degrees in accuracy, reliability or unsuitability to certain products. Continuous weighing techniques of a given volume, however, have been successfully applied. Such measuring equipment is shown in figure 10.6. Concentrate from the evaporator flows via the intake pipe (a) through a U-tube loop (b) pivoted on flexures (c) and connected by flexible connectors (d). Any change in density results in a proportional change of force in the weigh beam (h), which is measured by a pneumatic force balance system nozzle and flapper (e) and relay (f). (The diaphragm actuator (g) is for the concentrate feed control valve.) The milk or steam supply at the evaporator is controlled by signals from the U-tube transmitter. Four possible control arrangements are shown in figure 10.7. System A has the evaporator as the dominating unit. (The evaporator is termed the master, spray dryer is termed the slave.) Systems B — D are in reverse with the spray dryer playing the dominant role in the control. In system A, signals from the total solids detector (i.e. U-tube equipment described above) control the input of raw feed to the evaporator. The steam pressure is held at a fixed setting. The variations in the amount of concentrate due to deposit formation in the evaporator are compensated by moderate alterations to the spray dryer inlet temperature. In system B the spray dryer inlet and outlet temperatures are fixed. The total solids in the concentrate is kept at the required value through alteration of feed input. The evaporative capacity of the evaporator is changed through alteration to the steam pressure supplied to the thermo-compression stage, which itself is controlled by a level controller in the last effect of the evaporator. In system C steam pressure regulation is governed by the solid content in the feed passing to the spray dryer. The raw feed input to the evaporator is governed by level control on the last effect of the evaporator. In system D steam is added to the finisher stage and is independent of steam supply to the main evaporator stages. The total solids control the steam pressure to the finishers, and the level controller regulates raw feed input to the evaporator. This system has faster response characteristics. Cleaning-in-place (C.I.P.) can be built into the control system to operate automatically on evaporator shut down. There are considerable advantages in establishing a fully programmed system for the spray dryer too. Full benefit of evaporator and spray dryer automation is achieved only when other sections of the factory are under automatic control, but the 346 CONTROL SYSTEMS OPERATIONAL PRACTICE 0 control of complete plants that include a spray drying stage. Balls (132) has compared electronic and pneumatic control systems of the future. Level Steam Spray dryer Milk Powder 10.6. Precaution against Fire and Explosion To condenser Evaporator stage I L --------------- -8 Steam Total solids Level Drying air • > 1 Stage Milk . II Stage Spray dryer Finisher Ut Stage L_ To condenser I Outlet air Total solids Drying air nSteam C Powder -I—I/ Evaporator stage L ) Milk I Stage 1 1 .11 Stage Finisher Sigge Powder 32z) I To condenser I-72 Evaporator stage L 8— Outlet air —Total solids Level ■ Drying air Steam Mil k? I Stage r21 Stage Stage *:> L I— 7y Evaporator stage Evaporator: .Masier" A: Spray dryer: • Slave' 4 Finisher (1 ) 347 4 Spray dryer -8 —Total solids Powder Outlet air Evaporator: „Slave' 13 — D: Spray dryer: „Mosier' Figure 10.7. Block diagrams for automatic control of combined evaporator and spray dryer systems. time is fast approaching when instrumentation for a whole factory incorporating spray drying plant is centralized, and the control room likened to those already established and publicized in the modern oil refining industry. Electronic instrumentation is now being applied more widely to spray dryers. More extensive usage appears inevitable with computors for process Potential hazardous conditions can exist during spray drying operations when (a) handling products that form flammable mixtures at certain powder— air (or powder—drying medium) loadings (363), (b) handling solids associated with flammable solvents, or (c) permitting ignition sources (spark generation) to occur through faulty component performance. Rose (133) in a recent paper (1970) has discussed dust explosion hazards, dealing with the subjects of initiation and maintenance of explosion, minimizing hazards and eliminating explosion sources. In dryer design, therefore, even the remotest possibility of fire and explosion must be considered and counteracted through allowance in dryer construction design, proper explosion detection equipment, means to discover danger signs that can lead to mishap, and of course, adequate extinguishing equipment. The outbreak of fire (364) is the resultant of the prior events of ignition, and maybe explosion (in that order). Spontaneous flare-up can be the `explosion'. If ignition sources are removed, the fire hazard no longer exists. For any spray dryer operation, conditions that could cause ignition must be fully appreciated by operating personnel. The operators' responsibility is always one of discovering potential ignition sources and nullifying them. Causes of Ignition The causes of ignition are as follows : 1. Spontaneous combustion in certain product deposits. 2. Hot solid particles entering the dryer with the drying air. 3. Spark generation through friction between metallic surfaces or between hard product deposits. 4. Electrical failure leading to electrical discharge. 5. Static electricity discharge. Re. 1. Spontaneous combustion is associated with the burning of organic matter by an oxidation process (exothermic) which proceeds at increasing reaction rates due to its own heat generation. Spontaneous combustion occurs in deposit masses. The process leading to flame break-out is often slow as in the initial stages heat generated by the reaction is dissipated to the surrounding product drying medium or metallic surfaces. Ignition will only occur if the intensity of heat generation for a certain critical surroundings temperature is higher than the ability of the product to dissipate the heat. The critical temperature can -vary with product layer thickness. Ignition propagation time increases with decrease in critical temperature 348 OPERATIONAL PRACTICE levels. The composition and critical temperature of the product together with its location play a leading role in the mechanism toward flame generation through spontaneous combustion. For combustible products, there is always the chance for spontaneous combustion to occur in any place where product deposits out and remains in contact with the drying air. As dry product contacts the hottest drying air in counter-current flow dryer designs, these designs are more prone to spontaneous combustion explosion than co-current designs. Potentially combustible products are not dried in counter-current flow systems. The hotter the region in which product deposits, the greater the risk of spontaneous combustion occurrence. Critical deposit areas are at the chamber walls (although not near the humid drying zone) and the exhaust duct (especially in horizontal bends where product can readily deposit), Such deposits can form product layers of several millimetres thickness and remain over considerable time periods. The self-ignition process can be accelerated at any time by a complimentary heat source. This could be a chamber illuminating light. Under normal operating conditions, the extent of product build-up on the drying . chamber wall is normally well below layer thickness levels for self ignition. Nevertheless, thick isolated layers of product can be created from non-operational conditions. These include : (a) Wet washing. Poor chamber and duct cleaning can lead to wet patches of product remaining on surfaces. These patches will dry out on heating up the dryer, providing a good basis for further deposit formation. (b) Incorrect start-up/operation procedure. If incorrect start-up or operation causes wet product to be trajected against the chamber walls, these wet deposits on drying out can create a basis for further deposits of dry product. Re. 2. Not Particles. A great danger resulting from badly filtered drying air is the possibility of red-hot particles entering the drying chamber. The particles of foreign matter become red-hot on passage through the heater. The danger is real for both direct and indirect heaters. If these particles are large enough to penetrate the humid zone around the atomizer, they will enter the less humid zones of the chamber while still relatively hot. Their presence can spark off an explosion with resulting fire. The danger is greatest in spray dryers operating at high inlet air temperatures, but products liable to ignite or form mixtures with air within the limits of flammability are rarely subjected to very high drying temperatures in spite of high drying efficiencies that can be obtained. Red-hot particles can also be formed from the return of powder fines to the drying chamber (e,g. for agglomerating purposes) if there is a likelihood of powder entering or remaining in the chamber air disperser. This is prevented by the introduction of fines into the chamber via the atomizer, under the atomizer or through the dryer roof (away from the air disperser). CONTROL SYSTEMS 349 Re. 3. Friction between Surfaces. The contacting of metallic surfaces or layers of hard deposits can generate high temperatures through friction. Ignition temperatures can be reached. Fans or rotary valves are areas where such conditions can occur. Where rotary atomizers are used, incorrect assembly or a badly cleaned atomizer wheel and liquid distributor can constitute danger areas. Sticky deposits consisting of high solids content form and eventually dry during the spray drying prOcess giving a friction surface with the rotating wheel. Re. 4. Electrical Failure and Electrical Discharge. Sparks readily create explosions within powder—air mixtures having combustible properties. The source of spark is commonly from damaged rotating equipment striking casings (e.g. fans). Such conditions must always be avoided through preventive maintenance. Faulty electrical equipment is always a potential source of sparks, but rarely causes an explosion as electrical equipment is located away from the powder—air environment. Re. 5. Static Electricity. Spark discharge through build-up of static electricity could under certain circumstances create explosions (e.g. powder transport). The spray dryer is normally a completely metallic structure, and when earthed static electricity is rarely a problem. Earthing eliminates the build-up of static electricity to levels that create spark discharge. Static electricity is discussed in detail by Haase (134). 10.7. Control Systems for Preventing Fire/Explosion Conditions in Deposit Formations Prevention through Pressure Detection The use of sensors that react to variations in pressure can be used in explosion prevention control. The sensors mounted within the drying chamber are extremely sensitive to pressure variations that are produced during the first phases of explosion. These variations are sufficient to activate fire extinguishing equipment. The success of the system is based upon explosions not being an instantaneous occurrence but requiring a definite time period to develop a destructive pressure. Only milliseconds are required but this is sufficient to activate the explosion/fire suppressant. The sensor, on detecting imminent explosion, activates through an electrical power unit the dispersion of a suppressant. (Dispersion is often triggered by controlled explosion.) From the instigation of ignition to explosion/fire suppression, as little as 60 milliseconds may elapse. Further details are reported by Isaacs (135). Prevention through Air Analysis Prior to ignition due to spontaneous combustion, many products smoulder for lengths of time. The smouldering can release gas as a result of combustion. 350 CONTROL SYSTEMS OPERATIONAL PRACTICE Released gas can be detected through analysis of the exhaust drying air. Continuous gas analysis can record the presence of any gas that characterizes burning deposits. However, such analysis equipment is expensive. As ignition follows some time after commencement of smouldering, steps can be taken to shut down the plant for thorough inspection of the smouldering deposit areas. If the product is characterized by rapid outbreak or flame on smouldering, continuous gas analysis can activate automatic dryer shut-down or chamber/duct dousing. Often with organic products the evolved gases are pungent, and operating personnel may often be able to detect the smell. This is certainly possible if dried milk smoulders where pungent acrolein is evolved (375). Prevention through Limiting Explosion Possibility Although instruments are available to detect conditions constituting an explosion hazard, these should never be required to operate since ways of dryer operation are available to reduce to a minimum the possibility for spontaneous combustion and explosion. There are precautions special to each dryer application, but in general the following apply : (a) The operating instructions supplied for correct dryer operation are closely followed. Special attention is paid to maintenance of temperature control during operation, and correct start-up and shut down procedure. (b) Cleaning of equipment is thorough. Areas of likely deposit formation are inspected for cleanliness before start-up. There is full control of parts re-assembly. (c) Regular cleaning of supply air filters. This includes washing of filters, daily control of filter cleanliness and exchange of filter media when demanded. (d) Regular inspection of all electrical installations, mechanical equipment, bearings, packings, etc., within the dryer vicinity. (e) Regular inspection during operation of areas that are known to be prone to deposit formation. (f) Close control of the operation : (i) Control of temperatures and atomizer loadings. (ii) Product quality—control of product cleanliness. Burnt or discoloured product may originate from a smouldering deposit. (iii) Control of product discharge rate to establish no accumulation of product in the chamber. (g) Odour in exhaust drying air. Personnel should have experience in associating pungent smell with smouldering deposits. Prevention through Temperature Detection The use of thermostats placed at a wall or duct surface where deposit formation is likely is a known method for minimizing fire damage. It will not prevent fire however. - 351 Precaution to limit Explosion Fire Damage Extra precautions to limit damage are required for plant handling product that tends to form deposits within the system and is prone to spontaneous combustion. This is to limit damage in the event of explosion, where prevention was not possible. The following precautions can be made : (i) Installation of bursting discs in drying chamber wall. (ii) Installation of chamber doors that burst open under sudden pressure rise. (iii) Modern fire fighting equipment on hand and in operating order. Extinguishing media can be water, steam, carbon dioxide or other special chemicals. Chlorinated hydrocarbons have the disadvantage of producing phosgene gas when contacting a heated metallic surface. Carbon dioxide does present some limitations in personnel breathing in the working area, especially in the air space under the spray dryer chamber. Procedure in case of Explosion or Fire On the break-out of fire, the following actions must be carried out as quickly as possible : (i) Shut down fans and heater. (ii) Switch off the feed of concentrate, and pass water to the atomizer as soon as possible at maximum rate. (iii) After plant has cooled down, continue feeding water. Product in the chamber will inevitably be spoilt. The causes of explosions in dried milk has been reviewed by Pisecky (375). OPERATIONAL MEASUREMENTS 11 Operational Measurements 353 (a) Air heater characteristics (steam, fuel/gas, electricity). (b) Evaporation rate. (c) Supply fan characteristics. (d) Pitot tube measurements in the inlet duct. (e) Anemometer measurements in the inlet duct. (f) Orifice/venturi (built into inlet duct) characteristics. (g) Air dilution methods. Re (a). Air Heater Characteristics (1) Steam Heater. Reliable _air flow measurements can be obtained from measuring the condensate from the steam—air heater : From a heat balance over the heater tubes, the air flow rate (L a ) can be expressed as _ M e(H s— H )c IA (11.1) CAut — Tin) x where M, = condensate rate, H s = enthalpy of - steam entering heater, H = enthalpy of condensate, I/ = heater efficiency (95 %), Cp = specific heat of air (0.24), Tout = air temperature leaving heater, 1;„ = air temperature entering heater. N.B. The flow of condensate from the heater is always fluctuating. When measuring condensate, a sufficient volume must be collected to compensate this fluctuating flow. Calculations based upon insufficient condensate can lead to marked inaccuracy in the calculated air rate. 3-4 condensate volumes are collected to determine the mean flow rate. Prior to measuring condensate, the heater must be operating under steady state conditions (at least z hour after dryer start-up). The condensate temperature is measured as near to the heater steam traps as possible. When measuring air temperatures leaving the heater, readings are taken from all sides of the duct leading from the heater. Temperatures often vary across the duct due to uneven heat transfer throughout the heater. The thermometer bulb should be protected against any radiation effects from the heater coils. (ii) Oil or Gas—Air Heater. Air rates can be calculated from the heat generated during fuel combustion. The air rate (L a ) is expressed as : a The ability to asses dryer performance requires measurement of operational variables and product properties. In this chapter measurement of operational variables, e.g. air flow, powder—air loading, conducted on the dryer by operating personnel is discussed in greater detail than measurement of product properties, e.g. moisture content, bulk density, particle form, conducted under laboratory control procedures. This is due to the difficulty in relating laboratory measurement techniques to given products. Moisture content, for instance, is one of the most important dried product properties, yet for a given product, determination can be carried out in various ways. Every operator of a spray dryer standardizes his own procedures. Laboratory techniques are merely touched upon and for further details, the reader is referred to publications on laboratory practice. 11.1. Determination of Air Flow Methods are available to measure air flow either continuously or manually. For continuous measurement, the pressure difference over an item of equipment, or built-in restriction (orifice, venturi) is calibrated in terms of air flow. Manual measurements involve use of equipment performance characteristics or special measuring equipment. The choice of technique depends upon whether clean or powder laden air is involved, the type of equipment installed, and air temperatures and humidities in the measurement area. There are three areas of measurement : (a) supply of air to the air disperser, (b) air flow leaving the drying chamber, and (c) air flow in pneumatic conveying systems (if fitted). Measurement of air flow has been discussed in detail by Ower (136). 11.1.1. Supply Air to Dryer The supply air rate can be determined from measurements based upon : MQ Hf L= (11.2) Cp(T.3.1 — where M = combustion rate (weight of oil/unit time of Volume of gas/unit time), Q H = calorific value of oil or gas used. Efficiendy values for direct and indirect heaters are listed under heaters in chapter. 12. The accuracy of the air flow- calculation depends upon accurate measurement of fuel and gas combustion rates, and reliable data on the fuel calorific values. a 354 OPERATIONAL PRACTICE (iii) Electric Air Heater. Air rates can be calculated from the heat generated by the elements of the heater, as given by the heater kilowatt rating, and the increase in air temperature over the heater (1 KWH = 3413 BTU/hr (860 Kcal/hr)). Heater efficiencies are of the order 95 %. Re (b). Evaporation Rate The air flow to the dryer can be determined from measurements of evaporation rate. The measurements can be based on water or feed product evaporation. If a fixed feed rate of water is evaporated under steady state conditions, the measured temperature drop in the drying chamber will be caused by the water evaporation, plus heat loss through the chamber walls. The air rate can be calculated from the measured inlet and outlet drying temperatures by conducting a heat balance over the chamber (see chapter 4). The heat input (drying air and water feed heat content) is equated to the heat content in the exhaust air leaving the dryer, the heat loss through the chamber walls and the heat used in moisture evaporation. If secondary air enters the chamber, this also contributes to the temperature drop over the chamber. The heat content of this air flow must be included in the heat balance as a further heat input. Secondary air can be (a) the return of transport air to the chamber via ducting or atomizer, (b) any cooling air that enters the chamber, or (c) false air from leakage through door or window. The heat loss (Q L ) from the chamber walls is determined using the basic heat transfer equation (Q = UAAT). The heat transfer or transmission coefficient ( U) depends upon the insulation material used at the outer 2 chamber wall surface. This can vary from 0.2 BTU/ft /hr °F (1 Kcal/m' hr °C) 2 2 for well-insulated chambers to 2.0 BTU/ft /hr °F (10 Kcal/m hr °C) for chamber walls having forced air cooling. Thermal conductivity of some insulation materials is given in appendix 9. Re (c). Supply Fan Characteristics The air flow is obtainable from fan performance curves. Data on fan speed, operating pressure and air temperature are required. Air rates are then read directly from the curves. The reference temperature and atmospheric pressure levels on which the curves are based rarely coincide with the operating conditions. The operating data must be adjusted accordingly when using the curves. This method can give inaccuracies, and should not be used as the only measuring technique. Re (d). Pitot Tube Measurements If a suitable duct length exists within the supply air system, pitot tube measurements can be conducted to determine the velocity profile over the duct. The average velocity can be calculated and using the cross sectional OPERATIONAL MEASUREMENTS 355 area of the duct the volume flow is readily deduced. The mass flow is calculated using the air density, which is dependent upon the duct air temperature. Further details on pitot tube measurements are given under air velocity measurement (11.2.1). Re (e). Anemometer Measurements The anemometer is suitable_ as the supply air is clean. The inlet air duct normally_has sufficient straight lengths for anemometer access and accurate air measurement. Many types of instruments are available commercially and are robust enough to cope with plant site conditions. A useful portable instrument is the electronic anemometer, which measures velocity directly (137). The anemometer is used in conjunction with a transistorized indicator unit. Use of anemometers for measurement of air flow is illustrated later in this chapter. Re (f). Orifice/Venturi Characteristics If a suitable duct length exists within the supply air system, an orifice or venturi meter can be installed to give a continuous pressure drop reading that is related to air flow. Figure 11.6 shows typical positioning of the meters. Further details of measurement are given under air velocity measurements (11.2.2). Re (g). Air Dilution Methods Air flow rate can be measured by methods involving air dilution with gas analysis. It is especially suitable for flow measurement in irregular shaped ducts or in duct systems having a complexity of bends. The air flowing through the duct is diluted with a known quantity of diluent gas, and the diluent gas concentration is determined by gas analysis following thorough mixing in the duct. This method is applicable to measuring air flow rate from a direct heater. The method is illustrated in example 11.1. Of the manual methods mentioned above, measurements based upon heater characteristics, evaporation and pitot tube are usually the most dependable. Pitot tubes (with manometer) can generally be made available, which cannot be said for anemometers, Dilution methods are for special duct layouts which prevent _ use of alternative techniques. Results from fan characteristics should be treated with caution unless other techniques can be carried out as a check. EXAMPLE 11.1 In a pilot plant spray dryer, the supply air contains 0.24 % CO 2 by volume. To measure the air rate, carbon dioxide is introduced into the duct from a cylinder at constant rate before the heater. The dilution rate was measured at 1.6 lb/min, After mixing, the air contains a 1.4 % CO 2 by volume. If the air temperature after dilution is 76°F, what is the air flow into the drying chamber at 300° F? 356 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE Basis : 1 ft 3 of CO 2 free air. Supply air contains 0.24 \ 100 0.241 -- — 0.24 parts CO2 99.76 parts CO, free — 0 0024 ft 3 CO2 ft' CO, free Air after dilution contains 1.4 100 — 1.41 3 1.4 parts CO, — 0.0142 ft CO, 3 ft CO, free 98.6 parts CO 2 free Increase = 0.0142 — 0.0024 = 0.0118 ft 3 ft normally available in the exhaust ducting. Further details on pitot tube measurements are given under air velocity measurement (11.2). Re (d). Anemometer Measurements This method can only be used in duct work after a high efficiency dry powder separator since clean air conditions are required. It is not recommended if the exhaust air is saturated or corrosive. Details given for measurements in the supply air duct apply here. Re (e). Air Dilution Methods Details given for measurements in the supply air duct apply here. .6 CO, added = 11.2. Measurement of Air Velocity in Ducts L x 359 ft /min at N.T.P. 44 3 536 Volume at 76°F = 16 x 359 x 492 44 142.5 ft 3 /min 142.5 x 100 — 1210 ft 3 /min Air rate before heater = 357 0.0118 99.76 760 3 Air rate into drying chamber (1210 x —) = 1715 ft fmin 536 11.1.2. Exhaust Air Leaving Dryer The exhaust air flow rate can be determined from measurements based upon: (a) Pressure drop characteristics of the powder—air separator in the exhaust system. (b) Exhaust fan characteristics. (c) Pitot tube measurements in the exhaust duct. (d) Anemometer measurements in duct after the powder—air separator. (e) Air dilution methods. Re (a). Pressure Drop Characteristics of Powder Air Separator, e.g. Cyclones Approximate air flow rates can be obtained from pressure drop characteristics of the powder—air separator, especially cyclones. Correlations relating pressure drop and air flow depend upon equipment design, and are available from equipment suppliers. Re (b). Exhaust Fan Characteristics The use of fan characteristics to determine air flow has been mentioned under the supply fan characteristics (11.1.1). The same procedure applies here. Re (c). Pitot Tube Measurements The pitot tube technique is commonly adopted as suitable duct lengths are 11.2.1. Pitot Tube Measurement The velocity of air in dryer ducts is conveniently measured by a pitot tube and inclined manometer where air velocities exceed 10 ft/sec (3 m/sec). A pitot tube and accompanying inclined manometer (single limb) are shown in figure 11.1. The pitot tube consists of two concentric tubes formed into a 90° bend so that the nose points directly upstream when the tube body is inserted through the duct wall. The small hole at the nose of the tube faces directly into the air stream and measures impact (total) pressure . (head) (Pt). TOTAL PRESSURE HOLES ,g// WA ',Kir wr■ STATIC PRESSURE ( HOLES PITOT TUBE ELLI PSOI PAL NOSE — Figure 11.1. Pitot tube with inclined manometer. 358 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS The ring of small holes drilled into the side of the outer tube measures the static pressure (P s ). The positioning of these holes in relation to the tube nose is critical and is carefully chosen to eliminate unwanted pressure effects set up between the impact and static pressure holes. It is thus important that pitot tubes conforming to recognized standards are always used. Tubes made from 18/8 stainless steel will cover virtually all temperature conditions likely to be met on spray dryers (i.e. 18 % chromium, 8 % nickel, 0.6 % titanium steel welded points—can be exposed to 700°C). For a pitot tube facing into the air stream the impact pressure will exceed the static pressure. Thus the plastic hose fitted to the central tube is connected to the stud at the zero end of the manometer scale. The plastic hose fitted to the outer tube is connected to the top end of the single-limb manometer. The pressure read on the manometer scale is thus the difference between impact and static pressure, namely the dynamic pressure (P d ). To conduct a velocity measurement the pitot tube is inserted in the duct with the nose facing directly into the air stream. Care should be taken when inserting the pitot tube to prevent blowing the fluid out of the manometer by ensuring the impact and static holes enter the duct simultaneously. The most practical method to prevent loosing manometer fluid is the pinching of the plastic hoses while inserting the pitot tube. Alternatively, manometer balancing valves are obtainable commercially. The pitot tube is clamped so that the nose is at a fixed position within the duct. The differential pressure is read off the manometer. Slight fluctuations always occur to the meniscus in the manometer and the mean value is taken. This is the dynamic pressure for the position in the duct only where the tube nose is placed. 20 seconds should always be allowed to elapse before taking the mean value. This allows the meniscus fluctuations to settle down. The air velocity (K) is given by the general equation va = 2Pd g where Va is m/sec, Patin°, is mm Hg, Tabs is '1K, Pc,Ps is mm WG, K = 2 (a) For Circular Ducts For duct diameters less than 2 ft (600 mm) 4 equal area zones are used. Pitot tube readings are taken at distances from the duct access holes at 0.062D, 0.25D, 0.75D, 0.938D, where D is the duct diameter (see figure 11.2(a)). ACCESS HOLE FOR PITOT TUBE (11.3) Pa 30 Patmas x Tra, 528 d ) 408 K1— 408 + Ps i 0.706 0 0.062 0 , 25 0.75 (11.4) where va is ft/min, Pat ., is in Hg, Tab , is °R, P,P, is in WG. The correction factor 0.044 0047 0.294 0 1/2 xP 10 350 10 350 + P, but is equated to K2 1, = if Ps is less than 250 mm WG. Values of I/a in equations (11.4) and (11.5) are local velocities, A series of measurements is taken over duct area to form a velocity profile for determination of the average duct velocity. A profile is necessary as velocities are rarely uniform over the duct. The positions at which pitot tube readings are taken in the series of measurements depend upon duct size. Positions are selected from dividing the duct into zones of equal area. Equation (11.3) can be written correcting for variations in temperature and pressure. In British units = 4 x 103 ( K x 359 K, is a correction to the barometric pressure to allow for static pressure in the duct. If. P, is less than 10 in WG K can be taken as 1. In metric units 1/2 va = 4.05 ( 1(2 760 as (11.5) P X 293 0.853 D 0.9360 0•956 D D A DUCTS UNDER 2 ft DIAMETER 600 mm) B. DUCTS EXCEEDING 2 ft DIAMETER 600 mm Figure 11.2. Positions for velocity measurement by pitot tube in circular duct (equal duct areas. ▪ 360 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS For duct diameters greater than 2 ft (600 mm) 6 equal area zones are used. Pitot tube readings are taken at distances from the duct access hole at 0.044D, 0.147D, 0.294D, 0.706D, 0.853D, 0.956D, where D is the duct diameter (see figure 11.2(b)). Measurements should preferably be made along two traverses 90° apart. _1.a [ I2 ACCESS-• HOLES FOR PITOT TUBE --. -1- 1- - - Pitot Tube Misalignment The ratio of pressure difference measured in a uniform air stream with the pitot tube deviated at an angle 0 degrees from the air stream to the pressure difference when the pitot tube is facing directly into the air stream is given in table 11.1. As the pitot tube is turned, there is an initial increase followed by decrease in Pd recorded values until eventual negative response. At 90° to the air stream there is a sharp negative response and this effect offers an approximate method of detecting and measuring swirling air flows. + 4 H 4 H f PI TOT TUBE PRESSURE DIFFERENCE + in WG mmWG e-100 4A AREA LESS THAW 2 ft ' or 0 , 2 r00 B. 4- 4- + •C (b) For Rectangular Ducts Pitot tube measurements should be taken at points shown in figure 11.3. The minimum number of points for fairly uniform flow is 17 1 00 2 4 positions duct areas less than 2 ft (0.2 m ) 2 duct areas between 2-24 ft 2 (0.2-2.25 m ) 12 positions 20 positions duct areas exceeding 24 ft 2 (2.25 m 2 ) - 5•0 1 40 - 60 - -7o 1 80 2. -- qa 0 25.5 2 4. 30 37. 0 10 20 40 60 80 (PA 130 1 42 - 1 4 1r 1 4. 13.2 rz,r - ISO - 12.0 Angle of deviation from air stream 0 53.331•1" AIR TEMPERATURE AREAS 2-24 ft . or 02-2.25 rri Table 11.1. Effect on P d Reading of Pitot Tube Misalignment in the Air Stream AIR VELOCITY nysec. Io Figure 11.3. Positions for velocity measurement by pitot tube in rectangular ducts (equal duct areas). 2 Iry 11.17 11-2. 10■6 - 110 VIC 400 200 • ( cl)0=0 210 470 1.0 1.05 0.9 0.6 0.0 - 0.6 361 Sao G, 6•. Figure 11.4. Pitot tube pressure difference (P LO-air velocity nomograph. 362 OPERATIONAL PRACTICE Pitot Tube Calculations Air velocities from measured P d values are calculated from equations (11_4) and (11.5) or read directly from the nomograph (figure 11.4). When calculating the average velocity, the square roots of the velocity heads are often recommended to give a 'root mean square' value, but in practice this is not necessary. No appreciable error is involved if an arithmetic average of the velocity heads is taken where the majority of readings making up the velocity profile does not vary by more than +25 % from the mean figure. The average velocity is multiplied by the cross-sectional area of the duct to give the volume air flow. Mass air flows are obtained from the air density at the point of measurement. Although pitot tube instructions require the tube to point directly into the air stream, an air velocity measurement of sufficient accuracy for spray dryer applications can be obtained as long as the tube head alignment is within 15° of the air. Limitations in the Pitot Tube Methods 1. Presence of Airborne Powders. The pitot tube measurements are affected by powder entrained in the air stream. A pitot tube should not be used in powder conveying ducts, where powder—air loadings are high. Powder loadings in air leaving powder separator units (e.g. cyclones, bag filters) are normally low enough to enable pitot tube methods to be successfully applied. 2. Low Air Velocities. The accuracy of the measurement depends upon a measurable dynamic pressure difference recorded on the inclined manometer. Duct velocity must exceed 10 ft/sec (3 m/sec). Good accuracy demands at least a Pd of 0.4 in WG (10 mm) equivalent to 40 ft/sec (12 m/sec). Use of lighter manometer fluids will assist the recording of low Pd values. 3. Non Ideal Duct Layout. Ideal flow conditions for accurate pitot tube measurements require six duct diameters of straight duct before the measurement point. This is to obtain uniform flow conditions at the point of measurement. However, it is uncommon in spray dryer layouts to have inlet and exhaust duct systems with such unrestricted straight lengths of duct. This is due to the presence of dampers and sharp bends. To conduct a velocity measurement with a pitot tube, therefore, the duct layout must be studied so as to select the most favourable measuring position. If the best position available is still not ideal, determination of the velocity profiles along two or four perpendicular planes across the duct is essential. Permissible sampling positions, as shown in figure 11.5, are subject to every care taken with the pitot tube measurements. Otherwise velocity profile data obtained is of questionable value. There are limitations, however, to how much careful velocity profile determinations can compensate for non-ideal duct arrangements. The use of a pitot tube should not be attempted at (a) positions OPERATIONAL MEASUREMENTS 363 S.P NOT LESS THAN ONE DUC T DIAMETER (D) A. NOT LESS THAN 4 D NOT LESS THAN 20 - B. C. Figure 11.5. Permissible positions in ducts for pitot tube measurements of air sampling. (S.P, sampling (measurement) plane.) A, Sharp bend (upwards). B, After fan. C, After damper. closer than one duct diameter to any upstream bend or damper, or (b) at a point where air flow is in swirling motion. 4. Liable to Damage. Any damage to the pitot tube holes will affect the value of the dynamic pressure measured. Always before use, inspect the holes for damage (e.g. dents or burrs). 5. Small Holes Tend to Block. The pitot tube will not function if the holes are blocked. Before use, the tubes should be blown through via the connection nipples to ensure that the impact and static pressure holes are open. 364 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS 11.2,2. OrificelVenturi Measurements Orifice or venturi meters are for continuous measurement of air velocity. Both types can be installed permanently in supply air ducting, figure 11.6. Venturi meters are seldom considered in the exhaust duct system due to the required run-in and run-out duct lengths for mounting. Orifice meters should not be mounted in the exhaust system, as air is never 100 % powder AIR DISPERSER VEN TURI 365 free. This leads to deposit and cleaning problems at the orifice. Both types of meters are based upon the acceleration of air through a constriction. The kinetic energy increases with pressure energy decrease. The air rate is measured from the resulting pressure drop, where the rate is approximately proportional to the square root of the pressure drop. The pressure tappings are located at the inlet of the meter and at the point of lowest pressure. For the orifice meter, the upstream pressure tappings is approximately one duct diameter and the downstream tapping approximately one half duct diameter from the orifice. For the venturi the upstream tapping is approximately one duct diameter from the entrance, with the downstream tapping at the throat. Minimum run-in and run-out duct lengths are 4 x diameter run-in and 9 x diameter run-out. The venturi is generally preferred over the orifice. The venturi has a higher discharge coefficient and is more efficient in operation due to a greater proportion of the pressure drop being recoverable. It does constitute a larger equipment item, but the duct to the dryer air disperser can normally accommodate this. Air flow through an orifice/venturi is represented by the basic equation ) 1/2 (20 p) 1/2 1 (11.6) Vm = CD( 1 — (a/A? Pa , MR HEATER A . VENTURE ME TER AIR DISPERSER 41110 where Vm = mean velocity at the orifice plate or venturi throat, a = area of orifice or venturi throat, A = duct area. Compressibility of the air must be allowed for if the pressure difference is an appreciable fraction of the absolute pressure. Compressibility can be taken into account by multiplying the discharge coefficient C, by an expansion factor (Ye ). For air flows in spray dryer ducts, values of Ye approach unity. For pressure ratios (downstream divided by upstream) exceeding 0.8. For an orifice : • > 0.934 where a/A = 0.3 ORIFICE PLATE 11111 AIR HEATER DRYING CHAMBER ROOF B > 0.91 where a/A = 0.7 Ye = > 0.876 where a/A --- 0 , 3 Ye = >0.836 where a/A = 0.6 • For a venturi : ORIFICE METER Figure 11.6. Location of venturi and orifice meters in inlet drying air duct. 11.2.3. Anemometer Measurements An anemometer is used in duct flow conditions under 10 ft/sec (3 m/sec). It is an instrument for low air velocity and applicable to cases where dynamic pressures registered by pitot tubes are too small to allow accurate measurement. Anemometers are usually calibrated in feet of gas flow. To conduct 366 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS 367 l000 mm a measurement, the anemometer is placed in the air stream and is held in a set position for a definite time. A stop watch is best used. Hence, if the instrument is held for one minute the anemometer velocity reading will be in feet/min (m/min). The limitation of the instrument concerns the difficulty in keeping adjustment. It should be calibrated every time used. It is not suitable for hot, powder-laden air flow or ducts handling corrosive air—gas mixtures. 1 +w a +- E 1 12 + 13 ±. + 1— 19 ± + - H + -1— H- -- + 18 + 21. 4 + -F 4- —I- + 30 25 Figure 11.8. Inlet duct zoning for anemometer measurements in example 12.2. Figure 11.7. Positions selected in spray dryer layout for various air flow measurements illustrated in example 11.2• 11.2.4. The Application of the Various Techniques of Air Flow Measurement to Determine Air Rates in Spray Dryers, An Example EXAMPLE 11.2 It is required during commissioning of a spray dryer to determine the air flows. The dryer layout is shown in figure 11.7. A gas fired indirect heater is used. The inlet temperature is 210°C and the outlet temperature 88°C. The feed temperature is 48°C. Ambient air temperature = 5°C. It is proposed to use the various techniques: A. Air to dryer (1) Anemometer (2) Gas—air heater combustion rate (3) Fan characteristics (4) Evaporation B. Air leaving dryer (5) Pitot tube measurement (6) Pressure drop over cyclone (7) Fan characteristics The measurements are discussed below. The exhaust air composition after the cyclone is not suitable for the anemometer. A. Supply Air to Dryer Method (1) Anemometer Measurement A rectangular duct 1000 mm x 1300 mm before the supply fan was used for the anemometer measurement. The measurement point in the duct was considered not ideal and thus the duct was divided into 30 zones of equal area (figure 11.8). Each zone measured 167 x 260 mm. Each zone area was 0.0433 m 2 . The anemometer was held in each zone and the following results obtained. Zone Anemometer reading after 1 min 1 2 3 4 5 6 7 8 9 10 175 152 188 154 207 173 208 229 200 243 Zone Anemometer reading after 1 min Zone Anemometer reading after 1 min 11 12 13 14 15 16 17 18 19 20 178 188 220 242 191 244 235 191 224 228 21 22 23 24 25 26 27 28 29 30 246 239 225 238 226 246 250 259 246 250 368 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS Summation of zone velocities EV = 6495 m/min Total air flow L = EV .p air . A x 60 kg/hr Pair at 5°C = 1.252 kg/m 3 L = 6495 x 1.252 x 0.0433 x 60 = 21 200 kg/hr Method (2) Gas Fired Indirect Air Heater Characteristics The air flow rate is calculated using equation (11.2). Calorific value of gas = 8400 Kcal/Nm 3 Heater efficiency = 80 % Gas consumption rate (average of five readings) = 165 Nm 3 /hr L 165 x 8400 x 0.80 — 22 500 kg/hr a — 0.24(210 — 5) Method (3) Fan Characteristics The fan speed is calculated from the electric motor drive and diameter ratio of the fan and motor pulleys. A tachometer measures the motor speed. In this example, the fan speed is 1980 rev/min. To calculate the air rate from the fan characteristics curves the total pressure (Ps ) developed by the fan is required where P, = P s + Pd. The static pressure (Ps ) over the fan (use static pressure hole of pitot tube and a U-tube manometer) = 120 mm WG. The dynamic pressure (P d ) can be obtained using pitot tube, but flow in the inlet and outlet of the fan does not give conditions for accurate measurement. Calculation of P d by equation (11.7) was used. p APd = (11.7) 2 g For example 2 Fan inlet area at measurement point = 0.738 m 2 Fan outlet area at measurement point = 0.193 m Air temperature = 5°C Air density = 1.252 kg/m' Let air rate be assumed = 23 000 kg/hr From equation (11.7) ( 1 23 000 2 Pa = 1 1.252 1 2 2 2 9.81 1.252 x 3600 0.1932 AV = vou, — To calculate velocity values, the air flow is first estimated from which values of V° „, and V,„ are obtained from the outlet and inlet fan areas. The calculated value of P c, is added to the measured value Ps to obtain the total pressure (Pr ). With the value of P, and fan speed for ambient conditions, the air flow rate is read off the fan characteristic curve. If the air flow rate estimated initially to calculate P d does not agree with the value read of the characteristic curve, further values of air rate are taken until a value is obtained for complete agreement with the fan curve value. 1 0,7382 ) 42 mm WG = 42 + 120 mm WG -= 162 mm WG For the fan in question, an air flow rate indicated on the fan curve 23 200 kg/hr. Estimated value 23 000 23 200 kg/hr. Values are close enough to consider estimation correct. Method (4) Evaporation Measurement Air flow rate based upon evaporation of water feed is calculated from a heat balance from which (with given metric units) La M L (595 + 0.46 Tu ) — Cp(Ti (11.8) The accuracy of using equation (11.8) depends upon the correct data or estimation of (TL ), i.e. how many degrees of the measured chamber temperature drop are due to heat transmission losses through the dryer structure and introduction of secondary or false air. For given measurement, water feed rate (M L ) = 940 kg/hr, and for an insulated drying chamber, TL is estimated 7°C. Substituting in above equation L aa = where 369 940(595 + 0.46 x 88) — 21 700 kg/hr 0.24(210 — 88 — 7) B. Exhaust Air from Dryer Method (5) Pitot Tube Measurements The duct diameter at point of measurement is 800 mm, 6 zones were used (see figure 11.2). Measurements were conducted through traverses in the horizontal and vertical planes. Data are tabulated below T = 85 ° C D = 800 mm A = 0.504 m 2 370 OPERATIONAL PRACTICE 1 2 3 4 5 6 OPERATIONAL MEASUREMENTS Pitot tube measurement (Pd ) Horizontal Vertical (mm WG) Zone Distance from duct access hole (mm) 0.044D 0.147D 0.294D 0.706D 0.853D 0.956D - 35 120 235 565 680 765 7.0 9.6 11.9 11.8 10.6 8.4 Average Pd measurement (mm WG) Air velocity (m/sec) 7.1 9.7 11.9 11.5 10.0 8.2 118 14.0 15.8 15.4 14.1 12.6 7.2 9.8 11.9 11.2 9.4 7.8 Using figure 11.4 Zone 1 2 3 4 5 6 Av = 13.9 m/sec. Volume air rate = 13.9 x 0.504 x 3600 = 25 200 m 3 hr p a (85°C) = 0.988 kg/m 3 . Therefore L a = 24 900 kg/hr Method (6) Pressure Drop over Cyclones This measurement requires the cyclone suppliers' correlation for air rate in terms of cyclone diameter (d), static pressure drop, and air temperature. The given single cyclone has a volute (wrap around inlet), and air rate (L a ) is given by (n = number of cyclone0 L a = 6700nd ( AP, p X T, + 273 760 kg/hr where = 87°C, AP, = 180 mm WG d = 2.24 m Pa s s = 760 mm Hg 760 1/2 the air rate = 6700 x 1 x 2.242 180 23 700 kg/hr x ( 360 760 Method (7) Exhaust Fan Characteristics Similar procedure adopted as for the air rate determination at the supply fan (item 3). = 1230 rev/min Fan speed Fan inlet duct area at measurement point = 0.436 m 2 2 Fan outlet duct area at measurement point = 0.490 m = 85°C Air temperature = 250 mm WG Measured static pressure (P,) = - 3 mm WG (where Calculated dynamic pressure (.1%) estimated air rate corresponds with value from the fan curve) = 247 mm WG Total pressure -= 23 500 kg/hr From fan curve Conducting an Air Balance over the Dryer Method (1) 21 200 kg/hr Method (2) 22 500 kg/hr Method (3) 23 000 kg/hr Method (4) 21 700 kg/hr 22 100 kg/hr Average 940 kg/hr Evaporation Air leaving dryer Method (5) 24 900 kg/hr Method (6) 23 700 kg/hr Method (7) 23 500 kg/hr 24 033 kg/hr Average Thus false air (by difference) = 24 033 - (22 100 - 940) = 993 kg/hr Air to dryer N.B. The fan characteristic method is often considered too inaccurate to be of use. If this method is used, and the air flow value does not agree with data from other methods, the value should be disregarded. 11.3. Determination of Powder Loading in Air Flows 1 2 / 371 Data on powder loading in air flowing through the dryer exhaust ducting provide insight into the important operational aspects of 1. efficiency of powder separating and recovery equipment, 2. powder losses from powder separating and recovery equipment. Powder loadings in air can be determined by manual sampling or by continuous in-line measurement (510) (511). Manual determination involves the sampling of air at a duct access point where air flow is conducive to isokinetic sampling techniques. Air is sampled for its powder content at positions selected across the duct cross-sectional area for representative sampling. Sampling is conducted 372 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE x wz cc 1-(r) by drawing air plus entrained powder into a sampling nozzle of known size and through a probe tube which is inserted into the duct. The sampling rate is adjusted so that the air velocity entering the nozzle equals the air stream velocity just outside the nozzle (figure 11.9). This is the requirement for isokinetic sampling. The effect of incorrect sampling rate on observed powder loading is shown in figure 11.10. Air passing out of the probe tube is separated of its powder content. Knowledge of the air sampling rate and the weight of entrained powder separated per unit time enables calculation of the powder loading. The basic layout for sampling is shown in figure 11.11. In principle the method is simple enough, but in practice it 10 micron 1 micron 1.0 cc LI] 0 cc LLk 0 0 LU cc LU tr) POWDER AIR 100 micron z DUCT IN lg /cc . 2 0 . C,.. 1 oto BASIS : PARTICLE DENSITY 2.0 373 -J 0 1.5 1 0 05 0 SAMPLER NOZZ LE AIR VELOCITY I N SAMPLER NOZZLE LOCAL AIR VELOCITY IN DUCT STREAM Figure 11.10. Effect of incorrect sampling rate on observed powder loading in air stream A. (after Stairmand (188)). is complicated by the need of extreme sampling care to ensure that the powder loading of the sampled air is representative of duct conditions. Sampling must represent the average of powder particles passing through the sampling plane. This presents no difficulty when the distribution of particles is uniform throughout the duct cross-sectional area. However, this is rarely so due to the duct-work layout. It is necessary to collect B. PROBE TUBE SOLI DS COLLECTING DEVICE SAMPLED AIR SAMPLING PLANE ACCESS HOLE SAMPLING NOZZLE 1 C. Figure 11.9. Flow conditions at sampling nozzle. Flow profiles indicating isokinetic and non- isokinetic sampling conditions. A. Conditions for isokinetic sampling. B. Non-isokinetic conditions. Insufficient sampling rate (excess of large particles). C. Non-isokinetic conditions. Excess sampling rate (insufficient large particles). POWDER LADEN AIR SOL DS RECOVERY Figure 11.11. Basic layout for sampling powder laden air. TO SUCTION FAN 374 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE samples from a sufficient number of positions across the sampling plane to account for variations in particle population (mass flow) over the sampling plane. Flow of air and airborne powder are similar though not identical. The extent of the difference depends upon the size distribution and particle density of the powder, the air velocity and duct layout. In bends, the particles tend to be centrifuged to the outside of the bend although the uniformity is gradually restored by turbulent mixing. Uniformity is obtained 2-6 duct diameters from a 90° bend. 3-5 diameters is sufficient to establish a uniformity suitable for sampling. If the air velocity is high and the bend sharp, the air flow may separate from the inner wall of the bend and not begin to be corrected until 2 diameters downstream. The air in the dead space will tend to recirculate in one large eddy. The eddy rotation is forwards near the main stream and backwards near the wall. The rotation velocity is not high but may be sufficient for reverse flow to be detected by a pitot tube. When selecting a duct position to measure air velocities the selected position must be free of eddy flow effects. Typical velocity and likely powder loading over the cross-sectional area of duct arrangements are illustrated in figure 11.12. Duct arrangements considered are (1) straight duct, (2) following a sharp bend in a circular duct, (3) following a fan, (4) following a damper. The need to consider a number of sampling positions to obtain the overall powder loading leads to a time-consuming and often tedious sampling practice. However, failure to recognize variations in air velocity and powder loadings over the duct area can lead to high sampling errors. If powder sampling is merely conducted at the duct centre, under conditions of marked non-uniform flow profile, sampling can be considered in error in excess of ± 75 %. With correct attention paid to non-uniform flow profiles, sampling of airborne powder can be in error less than + 20 %. Continuous determination involves an in-place mounting of a powder detector or collector unit. With detector units, the presence of solids in air flowing across the path of unit sensors is registered on indicating equipment, calibrated for the product in question. Presence of solids are commonly detected by light intensity methods. With in-place collector units, the air is continuously sampled for powder. The equipment design enables the sampling rate to vary with fluctuations in air flow. A sampling nozzle is often incorporated, fixed in a position selected as representative of the air flow through the duct sampling plane. The quantity of powder collected per unit time indicates the extent of powder loading in the air flow. A sharp increase in collected powder signifies a marked increase in powder loading. Such monitoring of powder levels can provide useful information in assessing 0 > 375 376 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE day-to=day dryer performance. Once the equipment is installed it can always be calibrated against a method giving an absolute powder loading value. A useful in-place collector unit is the Vegrit' equipment (137), which is applicable to many spray dryer exhaust systems. Selection of Equipment for Determination of Powder Loadings in Air Flow The selection of equipment for either manual or continuous sampling depends upon the powder loading range likely to be met at the sampling location. Measurements to determine efficiencies of powder separator units involve both high loading conditions on the inlet side and low loading conditions on the outlet side. Measurements of powder loadings that constitute powder losses from spray dryer exhausts involve only very low loading conditions. For measurements in high powder loading conditions, equipment units must be capable of handling large quantities of powder if any degree of measurement accuracy is to be achieved. In manual sampling procedures, there must be effective separation of powder from the sampled air. In continuous detector systems, the sensors must be able to handle high powder populations. For measurements in low powder loading conditions, equipment must handle very small amounts of entrained powder. In manual sampling procedures this calls for near perfect separation efficiency of the separator incorporated within the equipment. In continuous detector systems, the sensors must be able to detect often minute particle sizes in air containing low levels of powder entrainment. Equipment Available Equipment offered for manual sampling of airborne powder comprises a sampling nozzle of known diameter, a probe on which the nozzle is attached, a means of extracting powder from the sampled air, a means of regulating and measuring the sampling rate and an air velocity determination set. Equipment offered for continuous measurement is characterized by the type of detecting systems. Most include sensors, amplifiers, converters and recording equipment. Equipment offered for continuous monitoring not based upon electronic units, are characterized by the sampling technique system adopted. Equipment suitable for determination of powder loadings in spray drying exhaust air flows is listed in table 11.2. Low powder—air loadings exist after main or secondary powder separator units, e.g. cyclones, bag filters, electrostatic precipitators. High powder—air loadings exist before main separator units or in powder conveying systems. Choice of Equipment The cyclone probe equipment is recommended as an all-purpose manual sampler. It can be used with the vast majority of spray dried products. It operates in both high temperature and high humidity air, is easy to operate, 377 Table 11.2. Equipment for Determination of Powder Loading in Ducted Air Flows Powder—Air loading Low High Manual sampling Continuous measurement Cyclone probe* (B.C.U.R.A. method) Internal filter* External filter* Light intensity methods Cyclone probe* (B.C.U.R.A. method) with (Large hopper attachment) Light intensity methods Electrostatic methods CEGRIT sampler (137) * B.S. 3405, 1961. and high degrees of accuracy can be obtained by plant operator personnel. The alternative filter methods demand. greater finesse of measurement. Without great care, experimental errors can be high. Only where the bulk of airborne particles have a size less than 3 micron does the filter method become essential. The Cegrit equipment is recommended as an all-purpose continuous (semi) sampler, for use with non-sticky particles in non-saturated air conditions. Light intensity and electrostatic techniques are much more expensive and their installation is only justified if powder loadings require monitoring due to (a) slightest powder emissions to atmosphere cause prohibited pollution levels, or (b) the product is of high value and 100% recovery is economically essential. Installation of equipment stated in table 11.2 involves careful and important preparation. Firstly, an initial inspection of the spray dryer duct-work is required to decide the most suitable sampling point. Arrangements must be made for making the necessary holes in the duct for equipment mounting, erect a working platform (if none is already available) and provide a power source to operate the equipment. When selecting the most suitable sampling position the ideal is a duct location where a uniform air flow profile is likely to exist (i.e. at the end of an extended straight duct section containing no flow interference such as dampers). Where there are no such duct sections, a position must be chosen where the powder population can be expected to be predictable and reasonably uniform. If this position is in a vertical duct position so much the better. The air velocity at the sampling point must exceed 10 ft/sec (3 m/sec) if a pitot tube is to be used for air velocity determination. Access hole requirements will depend upon the chosen equipment. For continuous methods, the equipment design will fix the type and size of access holes required in the duct wall. For manual sampling, access holes 378 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS for circular ducts should be such that one sampling line lies on a diameter in the plane of the duct and the other lies on the diameter at right angles to it. Access holes for rectangular ducts should be at different levels in the side of the duct. The number of required levels will depend upon the duct size. Access hole locations are shown in figures 11.2 and 11.3. 11,3.1. Manual Sampling (a) Measurement of Powder Loadings in Ducted Air Flows using the Cyclone Probe (B.C.U.R.A,) Method (138) Principle of Operation. A sample of air from the spray dryer exhaust system is drawn into a sampling nozzle, attached directly to the inlet of a small cyclone inserted completely within the duct (figure 11.13). The cyclone is mounted at the end of the probe. Powder particles are centrifuged out of the air sample and enter a detachable hopper. The air is drawn by a suction fan through the cyclone, the probe tube, a flexible hose and a control valve. The quantity of powder sampled is determined by weighing the hopper (dry) before and after the measurement. The cyclone is of special design having a high efficiency (see table 11.3), but particles smaller than one micron are not collected but pass down the probe and through the fan. A filter attachment can be used to collect such sizes, but for general sampling on spray dryers, the attachment is not required. No appreciable error is involved. If there is strong evidence of powder passing through the probe tube to the fan, and the filter attachment is not available, a correction factor can be applied to sampled powder, by stipulating that powder actually collected represents 80-90 % of powder entering cyclone. (This would only be considered when sampling very fine powders, where over 80 % of powder collected is less than 10 micron.) HOPPER CYCLONE ■ SAM PL] N G NOZZLE E PROBE TUBE PRESSURE TAPPI NG -HOSE LANE 0 F DUCT WALL PROBE HANDLE - Af R PLOW VALVE MANOMETER ` Figure 11.13. Layout of B.C.U.R.A. cyclone probe for sampling powder laden air. - SUCTION FAN 379 Table 11.3. Efficiency of B.C.U.R.A. Cyclone Particle size (micron) Efficiency of collection 2 3 4 5 6 8 10 15 20 72 86 91 94 95 96 97 98 99 >99.2 Sampling is based upon the isokinetic principle. Air is drawn into cyclone nozzle at such a rate that the nozzle air velocity is the same as the local duct velocity. Maintenance of isokinetic sampling conditions is - very simple. The cyclone itself is used as a flowmeter, and the pressure drop over the cyclone (registered on a manometer) indicates the air flow through the cyclone. Calibration of the cyclone enables the required manometer reading for isokinetic sampling to be read directly from a chart, which is based upon the pitot-tube dynamic pressure difference corresponding to the duct velocity. The location of the cyclone in the duct is selected and sampling procedure conducted so that the powder content in the sampled volume is representative of the total powder content in the duct air flow. The features of the method include : 1. The cyclone can be used at any temperature likely to be met in a spray dryer exhaust system. 2. The cyclone can be used over long sampling times, as the collection of powder does not increase the resistance to air flow through the cyclone. 3. Sampling control is straightforward as the cyclone acts as its own flowmeter. 4. A simple calibration chart relates duct velocity to required cyclone pressure drop for correct sampling. 5. At least 5 grams of powder can be collected. Such measurable amounts reduce experimental errors. 6. The cyclone can be used in humid air conditions so long as no entrained wet droplets are present in the air flow. 7. Cyclone operation is not always reliable with sticky airborne powders. For full details on the equipment, sampling procedure, and theory, the reader is referred to Hawksley et al. (138), British Standard 3405, 1961, Appendix 1, or instruction manuals (137). 380 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE (b) Measurement of Powder Loadings in Ducted Air Flows using the Internal Filter Thimble Method Principle of Operation. A sample of air from the spray dryer exhaust system is drawn into a nozzle attached to a filter thimble housing. The filter housing is mounted within the duct. Powder particles entrained in the sampled air are separated out in the filter thimble. Air is drawn through the filter housing by a suction fan. Air sampling rates are measured by (a) an orifice plate assembly, or (b) a gas meter assembly. Air flow is adjusted to give isokinetic conditions at the nozzle. Sampling procedure is such that the powder content in the sampled air volume is representative of the average powder content in the ducted air flow. The theory of measurement is described by Soo et al. (139). The advantage of using a filter to remove entrained powder (as compared with the cyclone method above) concerns the ability of the thimble to remove all airborne particles down to 1 micron. There are, however, notable disadvantages, namely (a) sampling times are generally short as powder collection steadily increases the resistance to air flow through the filter to a point where isokinetic sampling conditions can no longer be maintained, (b) constant readjustment to sampling rates is required due to increasing resistance to air flow, (c) common paper thimbles are unsuitable for use in high humidity conditions, (d) fractions of a gram are normally only collected, leading to high possible experimental errors, (e) variations in paper thimble weight due to atmospheric humidity can be significant. Sampling with the internal filter method requires constant personal attention paid to the equipment. However, due to the 100 % collection efficiency the method is often selected for sampling air flows containing a large proportion of particle sizes less than 10 micron, and/or where powder— air loadings are very low, e.g. after a bag-filter. Sampling by the internal filter method involves (a) selection of the most suitable sampling position, (b) access into the duct to mount the probe tube and conduct velocity measurements (usually by pitot-tube), (c) determination of the air velocity profile in the duct and (d) careful weighing of the thimbles. Paper extraction thimbles, used in the sampler, readily absorb moisture, and since the weight of powder collected is small, any variation in thimble weight due to moisture alone causes considerable error. It is therefore essential to use a control thimble. The control thimble is subjected to the same humidity variations as the test thimbles, and thus any weight change in the control can be referred to the test thimbles. This procedure is based upon the assumption that changes in humidity will affect the weight of all the thimbles equally. While not absolutely true, the method is sufficiently accurate if the thimbles are of the same material and approximately the same weight. 381 An alternative method is the complete drying out of the thimbles in a constant temperature oven. In this case, there is a chance of destroying the paper thimbles should the oven be too hot. Experience has shown that no improvement in accuracy is obtained with this method, except for hygroscopic materials. With hygroscopic materials, the test thimble is dried in the oven 230°F (110°C) with a standard thimble. Both are weighed in weighing bottles, or sealed test-tubes before and after the sampling. The control thimble is placed in the oven for 10 minutes. If the standard thimble loses more weight from the second heating, the oven is too hot and is destroying the paper. The accuracy of the test thimble weight is thus doubtful. It is necessary to resample and dry in a cooler oven or under vacuum. EQUIPMENT DESCRIPTION (i) The Internal Filter Thimble Equipment containing the Orifice Plate Assembly for Air Sampling Rate Control The equipment layout is shown in figure 11.14. Principle of Operation. The sampling probe tube is mounted in the duct (C) with the nozzle (A) facing directly into the air stream. Air is drawn through the nozzle by a fan (H). The quantity of air is controlled by valve (E) so that the air velocity into the nozzle is equal to that of local air velocity around the nozzle. The powder entrained in the air passing through the nozzle (A) is filtered out in a paper filter thimble (B). From the difference in the thimble weight before and after sampling, powder—air loading in the duct is calculated. The air sampling rate is read by the pressure drop reading (K) over the orifice plate (F). The sampling air temperature at the orifice is measured by the thermometer (I). A typical sampling probe tube, containing the filter housing and detachable sampling nozzle, is shown in figure 11.15. Various designs of isokinetic probe tubes are discussed by Denis (140). The correct air sampling rate is determined from the local duct velocity at the position of sampling, following a pitot-tube velocity measurement. The pressure drop over the orifice that corresponds to the pressure difference reading of the picot-tube is obtained from the orifice calibration chart supplied with the orifice plate assembly. Values of orifice pressure drop for isokinetic sampling conditions depend upon the operating variables of orifice suction pressure and sampling air temperature. The suction pressure is regulated by the bleed valve (0). The catchpot (L) is only included when condensation occurs in the probe tube (D). The placing of the filter thimble within the duct reduces the possibility of condensation fouling the filter. Sampling times should not be less than 30 minutes per filter thimble. A clean thimble is used at the same time as a control to determine changes in thimble weight due to humidity variations. 382 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS 0 FOCAL 111Fe 383 WALL 0 0 C 1:. SUCTION FAH cd O) DO E 1=4 k rt ti t■—■ E -c C ta t.= 3,T2 . ❑ (.) C 0 E tu tu tr (‘' N Uy ,13 5 ▪ E 6 2 E. D. C. B. . CA AM FLOW `) Figure 11.15. Filter thimble sampler for measuring powder loadings in air flow, 0 "CI H.Suction fan 0 1=1, tx) 171 Probe tube Suction control valve Duct wall CA w 6.r Filter thimble rn 57_ E 03 +a) (ii) The Internal Filter Thimble Equipment containing a Gas Meter for Air Sampling Rate Control The equipment layout is shown in figure 11.16. Principle of Operation. The sampler is mounted in the duct (C) with the nozzle (A) facing directly into the air stream. Air is drawn through the nozzle by a fan (F). The quantity of air is controlled by diaphragm valve (G) so that the air velocity into the nozzle is equal to that of air around the nozzle. The powder entrained in the air passing through the nozzle (A) is filtered out in a paper extraction thimble (B). From the difference in the thimble weight before and after sampling, powder loss rate is calculated. The total air volume sampled is calculated from the gas meter (H) reading, the air temperature at the meter being measured at thermometer (T). The venturi (D) and manometer (E) are used as a visual indication to any variation in air sampling rate. 30 minutes sampling is sufficient for each measurement. A clean thimble is used as the control to changes in thimble weight due to humidity variations. When condensation occurs in the probe tube and flexible tubing, the water is collected and measured in a catchpot. This is to prevent water entering 384 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE 385 8 7 it Figure 11.16. Layout for measuring powder loadings in air flows using the filter thimble sampler with gas meter for sampling rate control. the gas meter. Since the gas meter thus records a 'dry' air rate, a correction to the sampling rate is required. The equivalent volume of water vapour is determined and the sampling air rate (to be measured at the gas meter to correspond with the required wet sampling air rate at the sampling nozzle) is calculated. (c) Measurement of Powder Loadings in Ducted Air Flows using the External Filter Thimble Method The external filter thimble method of sampling is identical to that described for the internal filter thimble. Orifice plate or gas meter air sampling controls can be used. The difference in the two methods concerns the location of the filter thimble, which for the external filter thimble method is outside the duct. The arrangement allows easier access to the thimble for mounting or removal as the probe need not be removed from the duct. It also allows the nozzle to remain fixed in the duct, although sampling at a fixed nozzle position in the duct requires a uniform velocity profile over the duct for maintenance of good sampling accuracy. The equipment layout is shown in figure 11.17. Principle of Operation. Air is drawn through the nozzle (1) and through the probe tube (2) into a filter housing (3), mounted outside the duct. Condensation is prevented in the probe tube and housing by a heating mantle (9) wrapped around the sampler. Air flow is metered and controlled by an orifice or gas meter (5). A pitot tube (7) measures duct velocity. Air sampling rate is adjusted to give isokinetic conditions at the nozzle. The weight of powder collected in the filter per unit time is determined and the total powder loading in the duct is calculated using the ratio of nozzle-duct areas. 11 1. sampling nozzle 2. probe tube 3. filter thimble housing 4. filter thimble 5. instrument case containing air sampling rate controls 6. suction fan 7. Pitot-tube 8, inclined manometer 9. heating mantle 10. heating mantle control 11. duct wall Figure 11.17. Layout for external filter thimble equipment. The external filter thimble is not widely used unless the duct diameter is small, and duct air humidity low. Duct diameter (d) should be less than 18 in (450 mm) and sampling conducted in a length of straight duct of at least 10 x d, so that sampling in one position is justified due to uniform velocity profile across the duct. Air humidity in the duct should be low to minimize likely condensation problems in the filter housing, which can occur even with the heating mantle in operation. The powder should be non-sticky to prevent deposits forming in the probe-tube bend after the nozzle mounting. Deposits lead to clogging and powder collected in the filter will no longer be representative of actual duct conditions. 11.3.2. Continuous Sampling (a) Continuous Monitoring of Airborne Powder by Light Intensity Methods Continuous measurement of powder—air loadings using light intensity methods have been successfully applied to the spray dryer field. Equipment (141) (142) has been reported to measure loadings down to 0.005 grains/ft 3 (approx. 11 mg/NW). Equipment is usually mounted on the suction side of the fan, or in ductwork having a negative pressure. 386 OPERATIONAL MEASUREMENTS OPERATIONAL PRACTICE OPTICS LIGHT SOURCE DETECTOR FRESH AIR BLEAD RECORDER Figure 11.18. Measuring powder—air loadings by light intensity methods. Principle of Operation. The instruments are based upon the absorption of light by airborne powder. A light source emits a strong beam across the duct (see figure 11.18). A detector on the opposite side of the duct responds to the light beam, and produces an electrical field signal that is proportional to the energy it detects. The detector can consist of a filament whose electrical resistance varies according to the energy it receives. The light source is fixed in intensity and the electrical signal from the detector will depend upon the amount of powder passing through the light beam. Powder particles will reflect or absorb a proportion of the light energy. Fluctuations in detected light energy are measured and transmitted to a recorder. The recorder is calibrated for the powder type and powder-loading range likely to be met in the given duct system. The accuracy of the instrument depends upon maintenance of a constant light source, and detecting sensitivity. All optical parts in the equipment must remain clean during operation. By installing the equipment before the exhaust fan, clean atmospheric air can be drawn into the layout to prevent dust and dirt settling on the lens system and the light source. Light intensity equipment is available both in Europe and U.S.A. (143) (144) (145). (b) Continuous Monitoring of Airborne Powder by Electrostatic Methods Continuous measurement of powder—air loadings using electrostatic techniques is a new development in sampling equipment. Two main techniques are used (i) separating powder from air by charging by ion bombardment, (ii) detecting powder in air by charging by contact electrification (146). Technique (i) is more commonly known as electrostatic precipitation. In equipment using this technique, air is sampled via a probe tube and 387 nozzle located at a fixed position in the duct. The sampling rate is adjusted to maintain isokinetic conditions at the sampling nozzle. Sampled air is drawn through a small electrostatic precipitator, where the air velocity is reduced substantially to allow complete powder separation from the air. The separated powder falls to a graduated container where rate of collection can be monitored. Accuracy of measurement depends upon selection of a sampling nozzle position fully representative of the powder—air loading of the duct. For this reason, it is not recommended for sampling in large ducts, or in duct systems having sharp bends and flow obstacles (i.e. dampers) in the neighbourhood of the sampling point. Technique (ii) features the sampling of air via a probe tube and nozzle located within the duct. The sampling rate- is adjusted to meet isokinetic conditions. However, instead of separating the powder from the air, as in (i), the air is made to rapidly rotate so that the powder is centrifuged out to touch an electrically insulated excitor tube. The excitor tube has carefully selected electrostatic properties. An electrostatic charge is generated on the tube by the particle contact. The charge is measured and transmitted as an electrical signal to a recorder. The equipment layout is illustrated in figure 11.19. Once the sampled powder laden air has passed through the nozzle, probe tube, and excitor tube, it is exhausted back into the duct. The magnitude of the charge depends upon the quantity of powder in contact with the 10 8 it 0 0 AIR FLOW 1. sampling nozzle 2. probe tube 3, detector housing 4. excitor tube 5. insulation material 6. suction fan 7. manometer 8. recorder 9. exhaust tube 10. duct wall Figure 11.19. Layout for sampling equipment based upon contact electrification. 388 OPERATIONAL PRACTICE excitor tube per unit time. For the monitoring of absolute powder—air loadings, the system is calibrated for the product in question. This calibration is carried out by introducing known amounts of powder fines into clean air prior to passage through the excitor tube. The detection of powder by the excitor tube is very accurate. The probe tube and sampling nozzle , must be carefully located in the duct so that flow into the nozzle is representative of overall duct conditions. This technique is developed commercially (147). It is not suitable for sticky powders, or those that form deposits in the probe or excitor tubes. (c) Continuous Monitoring of Airborne Powder by the CEGRIT Sampler The CEGRIT automatic sampling equipment is an easy-to-use monitoring unit for airborne powders. It requires little personnel attention and provides data on the fluctuations of powder—air loadings in exhaust ducts throughout a plant operating day. Sampling through a probe tube and collection of powder in a cyclone over long time periods is involved. Instantaneous values of powder loadings cannot be obtained as in other automatic equipment (e.g. based upon light density measurements). The sampler operates on a wide range of powders, but it is restricted to non-sticky powders, where there is no likelihood of build-up in the probe tube and cyclone inlet. The sampler is highly flexible, being operated at most temperatures likely to be found in spray dryer exhaust systems. The sampler can be mounted in either horizontal or vertical ducts. The sampler consists of a sampling tube with nozzle, a highly efficient small-scale cyclone (2 in diameter) with - collecting jars, and an ejector at the cyclone outlet. The cyclone can be heated to prevent condensation problems within the powder collection system. The sampler contains no moving parts, and can be mounted either indoors or outdoors. It is suitable for sampling in ducts having an underpressure of 1 in (25 mm) WG or more, air velocities up to 70 ft/sec (21 m/sec) and air temperatures up to 700°F (370°C). The sampler conforms to British Patent 872 904 and is manufactured under licence (137). Sampling procedure is based upon isokinetic. measuring techniques. Powder loadings in the duct are determined by the rate at which the collected powder builds up in the cyclone jar. The cyclone efficiency exceeds 99 % for most powder sizes likely to be met. Both the ejector and sampling probe tube can be fixed in any direction to meet the air flow. Principle of Operation. Powder laden air is drawn through a sampling nozzle and probe tube into a cyclone by an ejector device operated by the suction of the duct itself. Air flow through the cyclone is continuous and uniform, as resistance to flow remains constant in the absence of product build-up. The air rate is controlled to give isokinetic sampling conditions. Once set, isokinetic conditions are maintained irrespective of fluctuations in air flow along the duct. OPERATIONAL MEASUREMENTS 389 The sampler is shown in figure 11.20. Various nozzle sizes are available to cover the range of duct air velocities likely. More than one collecting jar is required to enable rapid changeover during operation. The pressure drop over the cyclone is measured by a manometer (0-8 in WG). The equipment samples at one position in the duct. The equipment is best located in a straight section where a single central sampling point represents flow conditions within the duct. For less ideal duct sections a velocity profile over the duct is determined by a pitot-tube traverse to select the position representative of the average powder air loading. The probe tube length is sized so that when the sampler is mounted at the duct, the sampling nozzle is located at the selected position. From the local air velocity at the selected position the sampling nozzle is selected using the calibration chart supplied with the equipment. The air velocity into the nozzle must equal the air velocity past it, and yet the air flow rate through the cyclone must be sufficient for efficient powder separation while not exceeding 8 in WG. The sampling rate is read off calibration curves that relate cyclone pressure drop to pitot tube readings. A temperature correction is usually involved. 1. sampling nozzle 2. probe tube 3. cyclone 4. powder hopper 5. heating mantle 6. heating control 7. manometer 8. pressure tappings 9. sampling flow control 10. ejector for air flow through cyclone 11. duct wall Figure 11.20. The CEGRIT sampler for measuring powder loading in air flows. 390 OPERATIONAL. MEASUREMENTS OPERATIONAL PRACTICE 11.3.3. Determination of Dried Product Losses from Mass Balance Techniques The use of mass balance techniques to determine the product losses from the recovery system of a spray dryer is often cited as a method for use where sampling equipment is not available. Although the required weighing and tank dipping operations seemingly offer a simple method, this technique should not be used. Experimental errors involved in the measurement of tank volumes, feed solid content, sack weighing and product moisture content, when additive, can be very significant in a calculated loss value. The source of errors can be in the measurement itself, e.g. the physical li mitations of reading a scale exactly, or be one of precision, due to inaccuracies of the measuring equipment, e.g. inaccurate weighing balance or thermometer. The procedure for relating errors in measured quantities to the error in the calculated quantity involves the general law for propagation of errors (148). This law is expressed in the form of a partial differential equation. For a variable (z) being a function of several directly measured quantities x n ) is expressed as (x 1 x 2 ...x n ) the error in z due to errors in (x i x, Az = az ax , Ax, + ez ax, Ax, + + az x ax (11.9) where Ax ,Ax 2 ... A; may be considered as errors in the measured quantities x 1 x 2 x n (67). Equation (11.9) holds for any types of errors provided they are small. The possible errors in using mass balance techniques to determine losses, where data are obtained by general methods of measurement under dryer operation, are illustrated in the following example. EXAMPLE 11.3 A spray 'dryer layout with cyclone separators has a reported excessive powder loss following visual observation of the exhaust duct. In the absence of sampling equipment, a mass balance was attempted over the spray dryer to calculate the powder loss. A tank of stated volume (5000 litres) was set aside and during the drying of this volume, every care was taken to account for all the powder produced. The feed contained a solids content of 12.4 %, 45 sacks containing 15 kg powder were collected. 2 kg powder was swept from the floor around the packing area. The powder moisture content was 7.7 %. What is the maximum percentage error possible in the powder loss calculated by the mass balance technique? Now powder accounted for following drying = (15 x 45) + 2 = 677 kg. The loss is the difference between accounted powder and solids equivalent fed to dryer. 391 Now equivalent solids is a function of measurable variables, feed volume, solids contents and density where ST = F pFX F 5000 x 1.033 x 0.124 = 694 kg Xp 0.923 (I ) The accuracy in solids feed to the dryer depends on the accuracy of each variable. The error can be calculated by estimating the accuracy of the measured variables and using equation (11,9). Variable Approximate value Estimated maximum error 5000 litres 1.033 g/cm 3 12.4 92.3 % 15 kg 2 kg ±20 litres +0002 g/cm 3 ±0.1 % +0-1 ±0.1 kg ±01 kg Feed (F) Feed specific gravity (p,) Feed solid content (X F) Product solid content (Xp) Bagged powder (P) Spilt powder (L a ) Error (AS T ) in feed solids is given by applying equation (11.9) to equation (I) AS T = OST aST DS T AF + apF. Ap F + = p,X FAF FX F Xp ax AXp Fp F IKE FpFX F Xp 1.033 x 0.124 0.923 DS Xp + 5000 x 1.033 AXF 0.923 X?) 5000 x 0.124 5000 AP s 0.923 ' 5000 x 1.033 x 0-124 AX, (0.923) 2 = 0.136AF + 673Ap F + 55AX F 7.4AXp In order to obtain the maximum error, individual errors are summed. S T(m „) = 0.136(20) + 673(0.002) + 55(0.1) + 7.4(0.1) =10.3 kg Now powder loss (L c ) is given by Lc = P — Lc 392 OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS Applying equation (11.9) the maximum error is the sum of individual errors &L omax) = 1AS T + 45AP + 1AL, = 10.3 + 4.5 + 0.1 14.9 kg Powder loss calculated from mass balance L = 5000 x 1.033 x 0.124 0.923 2 — (45 x 15) = 17 kg 17 Percentage loss = 6 Maximum percentage error = 94 = 2.45 %. 14.9 = 87.5 %. 17 Powder loss calculated by the mass balance technique can be in error by as much as + 87.5 %. 11.3.4. Reducing Powder Losses from Spray Dryer Exhaust Systems The efficiency of a powder—air separator is virtually constant under ideal operational conditions. However, efficiency levels can drop substantially if dryer operation causes conditions to deviate from normal. Reduction in efficiency is registered as high powder losses from the spray dryer exhaust ducts. Dryers are designed for a given recovery of solids. For products that can cause damage to surroundings recovery must be 100 % and multiple separator units in series are used. For non-toxic products that sell cheaply, 99.5 % recovery often suffices as the cost of equipment operation to recover the final 0.5 % is more than the value of the powder recovered. Cyclones are generally used for these products. For plant layouts where powder loss measurements establish a.loss value higher than normal, it is unusual if the reason cannot be traced to plant maloperation or poor equipment maintenance. Excessive losses from cyclones are due to (a) overloading, (b) finer particle size of powder entering the cyclone, (c) malfunction of the cyclone powder discharge equipment. Re (a). This can be caused by : (1) Partial or total blockage of one or more of a battery of cyclones, thereby overloading the cyclone(s) with clean inlets. (2) Incorrect drying chamber operating pressure, leading to (for dryers with primary powder discharge at the chamber base) a larger cycloneborne powder fraction. (3) Sharp reduction in air flow through the cyclone 393 handling a fixed powder quantity. (4) Sharp increase in air flow through the cyclone leading to excessive turbulence and high re-entrainment losses. Re (b). This can be caused by: (1) Too fine an atomization. (2) Too low a feed viscosity. (3) Too low feed solids. (4) Reduced feed rate at constant atomization conditions. (5) Excessive comminution of powder in pneumatic conveying systems (transport cyclones with air return to main cyclones inlet). Re (c). This can be caused by : (1) Blocked or partial blockage of cyclone base. (2) Leakage of air into cyclone base via powder discharge equipment. (3) Incorrectly adjusted Vortex air locks (see chapter 12). For conditions of excessive powder loss, the feed, atomization, chamber and cyclone conditions must be investigated. Order of investigation could be as follows : (a) Visually inspect cyclone for cleanliness. If deposits exist in inlet or outlet ducts or cyclone sides, the cyclone must be coMpletely cleaned. (b) Measure air flow through the cyclone by AP or other suitable methods. If air flow is not as specified adjust air dampers to achieve correct flow. (c) Measure ratio of powder leaving chamber and cyclone and determine whether cyclone is overloaded. If overloaded, check (1) chamber pressure (if low, re-establish correct pressure by adjustment of inlet/outlet dampers) and (2) particle size distribution, bulk density, and moisture content of powder at the point of bagging-off. If powder is finer, control feed solids, feed rate, atomization conditions. If bulk density or moisture content is lower, check for any increase in inlet and outlet drying temperatures. If no real deviations are found during the above investigation, the fault must lie at the cyclone base with excessive air leakage into the cyclone. Check the clearance of rotors, rotor rotation in rotary valves or the pressure drop over Vortex air locks, or correct seating of flap valves (i.e. according to applicable equipment). Excessive losses from bag filters are invariably due to broken or ill-fitting bags, and for scrubbers insufficient water supply. 11.4. Assessing Acoustic Environment (Noise Levels) A spray dryer being industrial processing equipment invariably produces noise which, depending upon the sensitivity of the recipient can be distracting and annoying through interference with speech or wanted sounds. Individual equipment items (fans, atomizers, pumps, pretreater, product handling equipment) can produce noise above acceptable levels, but due to flexibility in equipment layout, overall levels in operator working areas need not be above safe working levels. Equipment items rarely emit noise levels to cause temporary or permanent hearing damage to personnel in OPERATIONAL PRACTICE OPERATIONAL MEASUREMENTS close vicinity for short periods. Noise levels around spray drying plants can be contained to comfortable limits by good building and equipment layout, correct equipment operation and regular equipment maintenance. In the past few years, the subject of noise, and noise control has been receiving increasing publicity (504). The resulting public interest has turned to concern, with pressure now being applied to authorities for legislation to limit noise. From the operators viewpoint, it is becoming necessary for owners of spray drying equipment to measure and limit noise levels. Two categories of noise must be dealt with : (a) External noise, radiated from a dryer installation to nearby residential areas giving rise to complaints from local property owners, and possibly infringing on local regulations, particularly at night. Particular care must be taken in locating open or semiopen plant. (b) Internal noise within plant working areas. Such noise levels can affect plant personnel, and exceed permitted limits. With noise consciousness becoming more recognised, acoustic engineering (149) (150) is now being applied in the design of spray drying installations.. 11.4.1. Basic Nomenclature in Acoustics Decibel (dB). The decibel (dB) is a logarithmic unit, and is defined in terms of a pressure ratio. Strictly speaking the decibel is ten times the logarithm of the ratio of two sound powers. Sound power is proportional to the square of sound pressure (P) and hence 2 PI = 20 log , ( -1 ) dB = 10 log in ( —) ic Po Po (11.10) where P0 is a reference sound level, P 1 is the actual pressure. The reference level (P0 ) corresponding to 0 dB is taken as the pressure for the threshold of hearing (0.0002 dynes/cm 2 or 0.0002 //bar (microbar). Sound Pressure Level (SPL). A noise meter responds to sound pressure variations giving an SPL reading normally in decibels. An SPL reading does not completely represent the noise characteristics that are causing the noise nuisance, since the human ear has a different response to different frequencies. Noises of a given SPL value will sound quite different to a human observer if they are at different frequencies. Noise Rating Number (N or NR). This is a number to denote acoustic environment. Each N or NR number represents a curve of sound pressure levels (dB) plotted against frequency in cps (Hz) (figure 11.21). From the slope of the curve, it can be seen that for a given N number a greater SPL is acceptable at lower frequencies than at the higher ranges of frequencies for the permitted acoustic environment not to be exceeded. 11.4.2. Assessing the Acoustic Environment for Safe Working For the given working area, a noise level meter and frequency analyser is used to measure noise and frequency. The measured data are plotted on the 395 110 SOUND PRESSURE LEVEL ( SPL } ( d B I 394 100 90 80 EQUIPMENT CREATING 70 AN ACOUSTIC ENVIRONMENT FOR SAFE WORKING 60 250 500 FREQUENCY 1000 cps 2000 4000 8000 REF 0.0002 MICROBAR Figure 11.21, Sound pressure level against frequency plot for assessing acoustic environment of equipment, N-curve for permissible environmental conditions (figure 11.21). If the curve plotted from measured data breaks the N-curve at any point, the permissible conditions are exceeded. The permissible N-curve depends upon the location area and plant items. For internal noise in working areas, an N 85 level is generally agreed by medical specialists and health authorities to be acceptable for personnel working in the environment for eight hours per day. The N 85 level also means that working near machinery exceeding this level has to be regulated, and personnel be advised to wear ear protection. Alternatively, acoustic attenuation can be applied to the machinery to bring the noise level below N 85 when measured in working areas. The distance between machine and point of measurement depends upon local codes of practice. During measurement of noise from a single item of machinery, the effect of background noise must be considered. During noise testing it is often difficult or impossible to take tests with just the one noisy machine in operation. It is usual to take a reading with the machine first on, and then off to obtain a background noise measurement. If the background noise is 10 dB lower in all frequencies than the figures in the first reading, then the effect of the background can be .ignored. Should the background levels be within less than 10 dB, then to obtain the effect of the noise source alone, the two readings must be combined. Special tables and graphs must be used for combining levels, since due to the logarithmic nature of dB figures, direct addition and subtraction is not valid. (Consult Handbook on Acoustic Engineering for tables and graphs) (151). 396 OPERATIONAL PRACTICE 11.4.3. Likely Areas having Noise Problems (a) Small Rooms (Especially small rooms with hard floors and tiled walls) It is common for hygienic reasons to place specialized equipment in individual small rooms with hard floors and tiled walls. Such arrangements lead to rooms being acoustically live. Multiple reflections occur leading to high reverberant sound fields. In this situation, use of acoustic tile on wall and floors is of little value where only marginal noise reduction is gained (2-3 dB at some frequencies). In such circumstances the necessity of equipment isolation in a small room for hygienic reasons must be judged against the working environment caused by the equipment, if noisy. (b) Vicinity of Fans Fan noise is a function of pressure development, and with the tendency to increase working pressure there is consequently higher noise output. For a given pressure requirement, there is not a significant difference between different types or makes. When the effect of fan noise on the environment is crucial, three approaches can be taken. (a) Use two fans working in series instead of one, thus halving the pressure development load, and operating at lower speed (multi-stage fans are not suitable where high powder loadings are expected). (b) Arranging duct layout so that the fan can be mounted in a separate room isolated from general working area. (c) Providing an acoustic enclosure around the fan and motor, and ensuring fan support is stiff and anti-vibration pads are used. Provision for heat disposal must be provided in any enclosure. (c) Buildings For a spray drying plant housed in a well-made building having closefitting doors and windows, the external noise levels created by plant operation will be very low. The building will act as a large acoustic enclosure, and stops effectively high frequency noise. Internal noise levels will depend upon the noise generated from each equipment item, and the degree of noise reflection at the building walls. A lightweight building is subject to greater noise levels through transmittance of equipment vibration through the structure. If structural panels are subjected to transferred machinery vibration, the panels in turn will vibrate at their own natural frequency. Large vibrating surfaces produce low frequency noise, which adds to the general noise level in the plant. To prevent equipment vibrations being transferred to the building structure, anti-vibration dampers and flexible pipe and duct connections become standard fittings. (d) Exhaust Ducts Acoustic energy as exhaust fan noise leaks through the building shell and passes to atmosphere via the exhaust duct. This leakage can cause a nuisance as fan noise is beamed over areas adjacent to the plant. Such sound emission covers a wide band of frequencies, and contains discreet low frequency OPERATIONAL MEASUREMENTS 397 tones that are specially annoying to noise sensitive people. For exhaust fans (centrifugal type) there is usually a strong low frequency component of noise caused by the passage of each impeller blade passing the fan cut-off or throat plate. This low frequency disturbing note is often at about 250Hz. The actual value depends upon fan speed and the number of blades on the impeller. In theory, noise problems associated with exhaust duct operations can be overcome by attenuation. However, in practice low frequency components of noise are difficult to attenuate as the majority of barrier and absorbent materials have a better noise reduction performance at higher frequencies than they do at frequencies in the range 250 Hz. The choice of materials is also limited due to the air conditions in the exhaust duct. Materials must withstand high temperatures (up to 250°F (120°C)), high humidity (even dew point conditions), often powder-laden air and corrosion (particularly if mounted outdoors). The presence of powder-laden air leads to eventual build-up on attenuation materials. Many acoustic materials are cellular and prone to powder penetration. Cleaning becomes difficult. A most effective noise barrier that is readily' washable is merely a concrete mass, but excessive weight is non-compatible with lightweight building structures used to house spray dryers nowadays. Attenuators for exhaust fans are generally mounted on the building roof although they can be mounted within the building subject to good access. The construction materials are comprised of those having good noise Table 11.4. Measurement of Available methods Droplet size distribution of sprays General (35) (152) I mpaction coated slides (153) (154) (155) (156) Sampling cells (26) (57) (63) (157) (158) (159) (160) (161) (162) Spray solidification (56) (163) Spray freezing (8) (164) (165) Photographic (166) Light scattering (4) Particle size distribution of dried product General (167) Preparing samples (168) Sieving (4) (169) (170) BS 1796 (1952) Microscopy (4) (171) Air elutriation (172) BS 3406 (1962), part 3 Sedimentation (4) BS 3406 (1963), part 2 Coulter counter (173) 398 OPERATIONAL PRACTICE reduction performance and those with reduced performance but can withstand the operating conditions. Cellular materials are used with the attenuator generally lined with a washable surface (e.g. asbestos, plastics). Often an attenuator is designed to act as a gravity settler also (chapter 12). 11.5. Measurement of Droplet and Particle Size Data on particle size of dried products are invariably essential for control of product quality. However, particle size is not always representative of the wet droplet size on atomization. When selecting and testing, atomizers, methods for droplet size determination are required. Full details of measurements are given in the literature. Notable references are given in table 11.4. Section IV SURVEY OF AUXILIARY EQUIPMENT 12 Survey of Auxiliary Equipment 12.1. Air Heaters Five types of air heaters are available to heat drying air in spray dryers. (1) Indirect steam air heater. (2) Indirect oil or gas air heater. (3) Direct oil or gas air heater. (4) Electric air heater. (5) Liquid phase air heater. Direct air heaters are used where spray dried material can be contacted with products of combustion. Indirect heaters are used where contact with combustion products cannot be tolerated. 12.1.1. Steam Air Heaters Steam air heaters are used in spray drying where inlet air temperatures, up to and around 400°F (200°C) are required and steam is available at pressures reaching 350 psig (25 atm). Hence steam air heating is widely used in the food and dairy industries where steam supplies are essential for evaporators and associated equipment. The drying air temperature depends upon the steam pressure (figure 12.1) and is approximately 9-13°F (5-7°C) lower than the steam temperature. As superheated steam is not ideal from a heating viewpoint, dry saturated steam is used with condensate leaving heater at 170°F (80°C). Air heaters are constructed from rows of extended fin coils housed in an insulated metal case. The heater is usually mounted on the discharge side of the supply air fan. The first few rows at the air entry end are arranged to act as a condensate section. Heat load is calculated from the weight and specific heat of the air and temperature rise. Steam consumption is calculated knowing the total heat content of steam on entry and exit. Heater size depends upon the heat 402 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 130 9 120 110 100 7 90 6 80 5 70 I 50 v a: 50 3 30 2 20 10 100 120 212 250 1 60 140 300 180DC 350'F Figure 12.1. Relation between saturated steam pressure and temperature (steam pressure as ordinate), transfer properties of the tubes and fins, i.e. materials of construction. For an air velocity of 1000 ft/min (5 m/sec) over the tubes, heat transfer coefficient values of the order 10.5 BTU/°F hr ft' (50 Kcal/°C hr m 2 ) are attained. A common form of tube construction is to use steel tubes with wound-on steel fins galvanized externally, the tube bore being 0.55 in (14 mm), and the overall diameter of the crimped fin 1.4 in (35 mm). Between 20 and 30 rows of tubes would be used to give an air exit temperature of 400°F (200°C) and these would be grouped in blocks of 2 or 3 rows with the tubes 403 welded into top and bottom steel channel headers. An air velocity of 1000 ft/min (5 m/sec) over a heater of this type would give an air pressure drop of 3 in WG (75 mm). Steam air heaters are relatively cheap, but there are general maintenance problems concerning corrosion, tube distortion and steam leakage. Correct steam trapping and feed water treatment are required for a long heater working life. It is essential to remove condensate as fast as it is formed. Steam traps of the float or thermostatic type are used in conjunction with strainers and provision for air release. Feed water treatment recommended by boiler manufacturers should always be followed, but in addition the condensate from the heater should be checked to ensure that it is not chemically aggressive. Corrosion resistant materials are available from tube manufacture and stainless steel or cupro nickel are often used particularly in the condensate section. The cost of using these materials must be considered against the cost of a heater made from steel and supplied with a spare section, which can be used as replacements should corrosion take place. Heaters can be manufactured so that replacements can be made with the minimum of down time. Positioning the heater is important to ensure that air flow on and off is such that dead spots do not occur. No bends should be made close to the heater and change in shape of the section ducting should be gradual. The heater should be raised from ground level so that condensate piping can be sloped to ensure rapid draining of water. Various arrangements of control and steam trapping (174) are used on steam heaters. One method of temperature control is to locate a thermostat in the air supply duct which acts on a modulating valve in the steam line. To obtain smooth temperature control, only a small part of the heater is regulated, the main heater sections then operate on a constant load. The ideal system for steam trapping is for each block of two or three rows to have its own trap and for condensate to be collected in a flash vessel and then taken to the condensate section. However, it is possible to use group trapping of sections where the load is steady and then allow the condensate to pass to a section, which acts partly as a flash steam and partly as a condensate section. This gives a less complicated piping layout which saves space and cost. Apart from temperature indicating instruments, it is usual to fit a pressure gauge on the steam line after the control valve so that a check can be made on the steam condition at point of entry to the heater. A sight glass after a steam trap will enable an operator to see if condensate is flowing. The use of strainers placed before a steam trap or built into the trap will prevent dirt from blocking up the trap. Strainers must be changed or cleaned at regular intervals. 404 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT Operational data of steam air heaters can be applied to calculate the air flow passing to the drying chamber. From heat balance over the heater the air flow (L a ) is given by Al(H s = Id a — H) (12.1) rl — where M c = condensate (steam) rate, H s = enthalpy of steam at heater inlet, enthalpy of condensate, n = heater efficiency (98-99 %). A steam air heater mounted at the dryer roof of a co-current flow dryer with rotary atomization is shown in figure 12.2(b). 405 removable for tube access for cleaning. Heaters are built in a range of stan6 dard sizes ranging from heat loads of 4 x 10 5 -10 7 BTU/hr (10 5 -2.5 x 10 Kcal/hr). Heater size limits higher loadings. A maximum air temperature leaving this type of heater is approximately 750°F (400°C). The efficiency of the heater depends upon heat load and air temperature. A guide to efficiency is given in table 12.1. An indirect heater is shown in figure 12.2(a). Table 12.1. Efficiencies of Indirect Fuel Oil Air Heaters Air temperature To Efficiency* 350-500°F (175-250°C) 525-610°F (275-325°C) 660-750°F (350-400°C) 80-85 75-80 70-75 * Dependent on heat load. (a) (b) Figure 12.2. Indirect air heaters. - (a) Indirect oil fired air heater. (The combustion fan is to the left of the picture and the servomotor which controls the quantity of oil and air for combustion is placed above it.) (b) Indirect steam air heater. (Mounted at air disperser level. Steam traps and condensate piping are shown at the base.) (By courtesy of Niro Atomizer.) 12.1.2. Fuel Oil Air Heaters In indirect fuel oil heaters, drying air and combustion gases have separate flow passages. The combustion gases pass over or through tubes that act as the heat transfer surface for the drying air. The heater consists of radiant and convection sections. The combustion chamber is fabricated in heat resistant steel. Galvanized tube is used to handle the combustion gas flow. The body of the heater is fabricated in standard steels. The heater end is Direct fuel oil air heaters consist of a combustion chamber that is lined with refractory, and a mixing chamber. The combustion nozzle assembly is mounted in the combustion chamber. The heater can be either horizontally or vertically mounted. Heaters are built in standard sizes with heat loadings 4 6 from 2 x 10 5 -2 x 10 7 BTU/hr (5 x 10 -5 x 10 Kcal/hr). Heaters for higher heat loadings are available, but outside standard sizes they are expensive. Drying air temperatures between 400-1100°F (200-600°C) can be obtained with fuel oil combustion. The cleanliness of the combustion gases depend much upon the quality of the fuel oil. For low sulphur oils, the gases can be so clean to enable use of direct air heater designs with such white products as titanium dioxide (without discolouration) or coffee (with aroma defect). The efficiency of direct fuel oil air heaters is of the order 95-98 %. Economic operation of fuel oil air heaters requires the attaining of high combustion rates with low percentage of excess air, avoidance of black smoke and long refractory life. The conditions are fulfilled if (a) atomization of fuel oil is complete, (b) mixing of oil spray and air is intimate and (c) oil flame does not contact refractory within the heater. Operational data can be applied to calculate the air flow passing to the drying chamber. From the calorific value (Q a ,) of the fuel and fuel combustion rate (W), the air flow (L a ) is given by La WQ c , Cp(To T)'1 (12.2) 406 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 12.1.3. Gas Air Heater In gas air heaters, the gas burner normally operates on the aerating principle. Gas is mixed with part or all of the air required for combustion. The gas flows from a jet at high velocity causing a reduction of pressure around the jet into which combustion air readily flows to give intimate mixing between gas and air. Often this mixing section can be in the form of a venturi, but many types of efficient mixing forms are offered by manufacturers of gas burners. Gas mixtures with air have limits of inflammability, above and below which combustion cannot be sustained. For example, natural gas mixtures must contain between 5 and 14 % oxygen by volume. The whole field of gas combustion has been well investigated and further details are to be found in textbooks on fuel technology (175). The construction and performance of indirect gas air heaters is similar to indirect fuel oil air heaters. Direct gas air heaters are less complicated in construction, consisting of a cylindrical combustion chamber of insulated heat resistant steel. Heaters are built in standard sizes for heat loads covering the range 4 x 10 5 -2.5 x 10' BTU/hr (10 5 -6 x 10 6 Kcal/hr). Drying air temperatures of 1500°F (800°C) can be readily attained, and this temperature range covers most high temperature spray dryer operations. Subject to satisfactory refractories, heaters can be designed to reach air temperatures in the neighbourhood of the gas flame temperature 3600°F (2000°C). Compared with other types of direct air heaters, gas fired are cheaper to fabricate. They are being used more and more in spray dryer layouts due to the increasing availability of natural gas. Apart from complete gas air heater units, simply open ring-jet burners can be mounted after an indirect air heater (steam) to boost drying air temperature, or installed as the sole direct heating source in spray dryers of medium air flow rate. With correct gas jet selection for the inlet duct air velocity, combustion can be so clean to enable use in drying systems involving coloured or aromatic products. Efficiencies of gas air heaters are similar to those of fuel oil air heaters. To calculate the air flow rate through the heater, equation (12.2) can be used where Q c , is the calorific value of the gas. 12.1.4. Electric Air Heaters Electric air heaters are common on laboratory and pilot-plant spray dryers. The heater is cheap to build but expensive in operation. Air temperatures up to 750°F (400°C) are attainable in practice. 12.1.5. Liquid Phase Air Heaters (Thermal Fluid Heaters) Liquid phase air heaters are a relatively new method of air heating on spray dryers. It is used in closed cycle drying systems where temperatures up to 750°F (400°C) are required in inert gas—organic vapour mixtures that constitute the drying gas. The system is also used in medium size spray dryers 407 where inlet drying air temperatures of 400°F (200°C) are required, but where steam for heating is not available. The heater system consists of a special oil or heat transfer fluid circulating at high speed through a boiler and air, heater. The heater consists of rows of finned tube through which the fluid flows. The boiler can be . gas or fuel oil fired. The main advantage of liquid phase heating is the open pressureless system, capable of attaining relatively high air temperatures. Heaters are available with heat loads up to 1.6 x 10 7 BTU/hr (4 x 10 6 Kcal/hr). 12.2. Fans Spray drying is an operation that requires movement of air or other gaseous media. This movement through the dryer is carried out by centrifugal fans. One or two main fans are used in a spray dryer layout. For dryers that operate with a single exhaust fan, the drying chamber is under a high negative pressure. The majority of spray dryer designs, however, operate with the two main fan system. Apart from the exhaust fan, a supply fan is mounted on the inlet side of the drying chamber. This fan forces the inlet drying air through the air heater and air disperser. By using the two fan system, greater flexibility of chamber pressure operation is obtained. The supply fan is sized to balance the exhaust fan, and the chamber can operate at near atmospheric pressure if required. The operating chamber pressure often controls the powder—air loading in the exhaust air leaving the chamber. ONE -FAN SYSTEM usually small dryers) TWO FAN SYSTEM Figure 12.3. One and two fan spray dryer layouts. 408 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT With a two fan system, the chamber pressure can be adjusted to give the optimum powder—air exhaust loading for highest collection efficiency in the powder recovery unit. One and two fan systems are shown in figure 12.3. Only the principles of fan engineering are referred to here. For a detailed account of the subject, the reader is referred elsewhere (176) (177). 12.2.1. Fan Requirements on a Spray Dryer Layout (a) Exhaust Air Fan, always essential and mounted in the exhaust system of the spray dryer. It is good practice to locate the fan after the powder recovery unit, so that the fan operates on clean, powder-free air. The fan is the largest on the unit, as it has to overcome the largest pressure losses of the layout, namely over the powder recovery system. (b) Supply Air Fan, mounted in the inlet duct system to the drying chamber. It is mounted before the heater and thus runs with cool air. The fan supplies drying air to the chamber. It is smaller in size than the exhaust fan and as the pressure requirement is lower, it will use less power. The supply fan is sized in relation to the exhaust fan, so that air flow through the dryer and the drying chamber pressure is controllable. (c) Transport Air Fan. A transport air fan is required for dryer installations where product is conveyed pneumatically away from the chamber base and powder recovery system to the product bagging-off or storage areas (silos). The fan is sized to produce an air flow whose air velocity through the duct will maintain powder conveying. A transport cyclone is invariably incorporated in the system to separate out the powder, and the fan is mounted after the cyclone so as to operate on air of very low powder loading. (d) Cooling Fans. These can be many and varied in application. Fans are used to cool potential hot spots in the chamber structure, or prevent the rise of temperature in certain dryer components. Cooling fans normally require small horsepower drives. Typical cooling fans used are (i) atomizer cooling, (ii) air disperser cooling, (iii) duct cooling, (iv) chamber wall and roof cooling. (e) Air Heater Fans. These include the fans to meet requirements for combustion air and flue gas exhaust on oil and gas fired installations. 12.2.2. Fan Parts and Principles The essential parts of a centrifugal fan are (a) a rotating impeller, (b) its housing (usually spiral), (c) impeller shaft and bearings, (d) inlet and outlet flanges or spigots, (e) a sturdy base plate. These parts are shown in figure 12.4. There are variations in impeller design, each depending upOn how the blades are mounted to form the impeller. Radial, forward curving or backward curving types are available. The forward curving blade is concave in the direction of rotation. The backward curving blade is convex in the direction of rotation. The blade design defines the fan characteristics. Each type is never 100 % efficient 409 in operation due to air movement through the impeller, air, skin and bearing frictions. The number of blades forming the impeller has a greater effect on the fan volume—speed characteristics than on the fan efficiency. IMPELLER SHAFT AND BEARINGS OUT LET AIR FLANGE INLET AIR FLANGE or SPIGOT ROTATING IMPELLER (2 blades IMPELLER --HOUSING STURDY BASE PLATE Figure 12,4. Principle parts of a centrifugal fan, The pressure developed by a fan results from the centrifugal forces of the air enclosed between successive blades, and the energy of the air leaving the blade tip. The pressure developed by the fan depends upon the blade design. At constant fan speed the backward curving blade produces the least pressure, the forward curving blade the most. This can be seen from the vector diagrams in figure 12.5. The backward curving blade is used extensively in spray dryer applications. It meets the requirement of high volume air movement at medium/low pressures. Backward curving blades can be formed to achieve 80 % total efficiencies (75 % static efficiencies), but although the blade has self-cleaning properties, handling sticky entrained powder can cause deposit formation on the back face of the blade. The optimum blade profile can be used for supply fans as filtered air is handled and also for the exhaust fan if installed after a high efficiency product recovery separator, e.g. bag filter. For transport fan requirements, where higher powder—air loadings are likely, use of the optimum blade curve can result in deposit problems especially for conveyed powder with stickiness tendencies. A compromise is often made in the blade design. A blade profile that lies between the backward curving and radial types is adopted to give better self-cleaning characteristics. A reduction in fan efficiency results, the total efficiency of the modified blade decreasing to 70 % (static efficiency = 65 ). In many spray dryer installations, the modified blade design is used on all fans throughout the plant thereby obtaining savings in costs through standardization. However, in cases where total power requirement of the plant is strictly specified, the optimum backward curving blade profile can be used on all fans handling clean air. Only where high powder loadings are expected, will the modified self-cleaning profile be adopted. SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 12.2.3. Fan Characteristics Once a fan is installed in a given ducting system, the operating characteristics can be deduced by plotting the system characteristics on the performance curves. .These characteristics depend upon flow resistances or the pressure required to deliver air through the system at a desired rate. The system characteristic is therefore plotted with air flow rate as abscissa and pressure as ordinate. Fan operation conditions are represented where the system characteristic curve intersects the fan pressure curve. EXAMPLE 12.1 A fan with backward curving blades operates at 1300 rev/min and 300 mm total pressure drop and delivers 42 000 m 3 /hr of air. The fan horsepower requirement is 65 HP. The system characteristics change and the pressure falls to 200 mm at 42 000 m 3 /hr. Use the performance curves in figure 12.6 to determine the new fan operating conditions. Fan characteristics are dependent upon the design of blade arrangement. For a given fan design, the primary characteristics are represented on fan performance curves, where pressure and horsepower are plotted against air flow rate at a fixed impeller speed and air density. The difference in the form of the performance curves for radial, forward and backward, curving blades are shown in figure 12.5. R a . RADIAL BLADES b. FORWARD CURVING BLADES 0 LEI Lc m w m 0 a- AIR FLOW c BACKWARD CURVING BLADES t PRESSURE —. V 1 411 c.r) z z — 300 P 1 ▪ 250 P ▪ 200 2 69 65 cc cr) Li) 1./1 cc Z:13MOd 3S8OH 410 0 42000 47000 3 AIR FLOW —* AIR FLOW —"- Figure 12.5. Performance curves characteristics for radial, forward curving and backward curving blades (for constant fan speed and air density). For forward curving blades, inspection of figure 12.5(b) shows a characteristic not favourable to spray drying plant. Any change in the system pressure that increases air volume flow can cause a marked increase in horsepower requirement Thus power overload cover is required due to the rapid rise of power for relatively small increases in air flow. The backward curving blade, on the contrary, features power limiting characteristics (figure 12.5(c)), and therefore is a good choice for spray drying plant. Performance curves of industrial fans often include more data than is shown in the simplified curves of figure 12.5. Fan efficiency and fan size are also represented. AIR FLOW RATE M /hr La Figure 12.6. Fan performance chart for example 12.1. Initial system characteristic is represented by line A. Line A intersection with operation curve (N = 1300 rev/min) gives initial fan operating conditions, i.e. P 1 = 300 mm WG, (L a ), = 42 000 m 3 /hr, (FHP) 1 = 65 HP. The system characteristic curve alters to form line B denoting a pressure decrease to 200 mm. Reading from the curves, the new operating conditions are (La)2 = 47 000 m 3 /hr, (FHP) 2 = 69 HP and a new total pressure of 250 mm WO at 47 000 m 3 /hr with a constant fan speed of 1300 rev/min. 12.2.4. Fan Laws All fan performance changes are governed by laws, which are independent of the design of fan. They apply to a homologous series and a fixed point of rating. 412 SURVEY OF AUXILIARY EQUIPMENT (a) Law I. For increase or decrease in fan speed for a constant air density and given fan design and size. L a cc N: Volume flow and mass flow (L a ) vary as the fan speed (N). P oc 1\1 2 : Pressure (11 varies as the square of fan speed. HP oc 1\1 3 : Power (HP) varies as the cube of fan speed. (b) Law II. For changes in fan size where geometrically similar fans are involved, but fan blade tip velocity remains constant. L a cc d 2 : Volume flow and mass flow vary as the square of the impeller diameter (d). P = K: Pressure remains constant. HP cc d 2 : Power varies as the square of the impeller diameter. (c) Law III. For changes in air density (p a). L a = K: Volume flow remains constant (mass flow varies as the air density). P cc p a : Pressure varies as the air density. HP cc p a : Power varies as the air density. From the above laws, useful working relations can be developed. (d) If the fan size is varied, but the fan speed is kept constant. La cc d 3 : Flow varies as the cube of impeller diameter. Pressure varies as the square of impeller diameter. P cc d 2 : HP oc d l i 5 : Power varies as the 1/5th power of impeller diameter. (e) If the fan size is varied together with the fan speed. La cc d 3 (N 1 /N 2 ): Flow varies as the cube of diameter and fan speed ratio (N 1 /N 2 ). P oc d 2 ( N1/N2) 2 : Pressure varies as the square of diameter and the square of the fan speed ratio. HP oc d 5 (N1IN2) 3 : Power varies as the diameter to the power 5 and the cube of the fan speed ratio. Use of the relations are illustrated in examples 12.2, 12.3 and 12.4. EXAMPLE 12.2 An exhaust fan draws 40 000 kg/hr of air (80°C) through a cyclone system. The static pressure drop over the system is 225 mm WG and the fan horse power is 60 HP. It is planned to increase the dryer capacity by increasing the air flow by 5 %. If the fan currently runs at 1200 rev/min, what new fan speed is required? Predict the increase in pressure drop and power requirement. N 1 = 1200 rev/min SURVEY OF AUXILIARY EQUIPMENT 413 Using law I N2 42 000 1260 rev/min = 1200 40 000 = 1260) 2 P2 = 225(-12w3 = 248 mm WG 126 13 (FHP) 60 ( 1"06 = 69.5 HP Increase in static pressure = 23 mm WG Increase in FHP = 9.5 HP Required speed = 1260 rev/min 12.3 If a fan produces 40 000 m 3 /hr in a given system, but is replaced by a geometrically similar fan whose impeller is 10% larger, what is the horsepower requirement and pressure drop if the replacement fan is rotated at a speed to give the same blade peripheral velocity? The original fan required 60 HP and the static pressure drop was 225 mm WG. EXAMPLE d 2 = 1.1d 1 (L a) 1 = 40 000 m 3 /hr Using law II 1.1 2 (L a ) 2 = 40 000( 1.0 ) = 48 400 m 3 /hr P2 = P„i.e. pressure remains constant 2 (FHP) 2 = 60( 1.1 ) = 72.6 HP 1.0 EXAMPLE 12.4 A fan rotating at 1320 rev/min draws 44 000 m 3 /hr of air at 80°C. Condition changes- occur so that air flows through the fan at 50°C. What is the air flow through the fan at the reduced temperature. Calculate static pressure increase and fan power increase, if for the original condition P 1 = 270 mm WG and 75 HP. (L a) i = 40 000 m 3 /hr Density of air at 80°C = 1 kg/m (L a ) 2 = 42 000 m 3 /hr Density of air at 50°C = 1.09 kg/m3 414 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT Using law III I I . 1 1 1 . 415 1 WORKING TEMPERATURE 100°F 3 13° C 1 For new conditions, the volume flow remains the same. The total mass flow increases as 44 000 m 3 /hr at 50°C --- 48 000 kg/hr. 160 1.09 P2 = 270 1.0 = 294 mm WG 1.09 1 0 = 81.8 HP (FHP) 2 = 75 12.2.5. Fan Efficiency Fan efficiencies of 100 % are never obtainable and the horsepower supplied to the shaft of a fan is greater than the theoretical horsepower requirements to move the air through a given system. Fan efficiency (ri) is given by the ratio Ls Ls a 10 z fan output or theoretical horsepower x 100 shaft horsepower (FHP) The efficiency of a given fan depends on its point of rating and this varies with air flow and pressure which in turn depends upon temperature and altitude. Efficiencies can be stated either as a total efficiency (based upon total pressure) or as a static efficiency (based upon static pressure) and horsepower input. Static efficiencies are generally lower than total efficiencies as illustrated in table 12.2. Table 12.2. Typical Fan Efficiencies Fan efficiency (%) Fan blade design Backward curving blade Modified backward curving blade with self cleaning properties Radial blade Total pressure basis Static pressure basis 80 75 70 60 65 55 Loss of efficiency is caused by friction and turbulence within the fan. Further losses occur due to friction in bearings and glands, and drive losses must be covered. In considering overall efficiency the electric motor efficiency must be known. The relation between motor horsepower and fan horsepower is shown in figure 12,7. 10 100 INSTALLED FAN MOTOR HORSEPOWER Figure 12.7. Relation between fan horsepower and installed fan motor horsepower. In order to cover these losses and give a safety factor it is usual to select a motor of a standard frame size approximately 15 % up on fan horsepower. The horsepower values in figure 12.7 are based upon an average working temperature of 100°F (38°C). Where temperatures are lower, cold start conditions will demand higher horsepower and sufficient installed horsepower must be available. However, for warmer working conditions, less power will be required. Fan horsepower values are reduced by 5 % for temperatures at 115°F (46°C), while at 140°F (60°C) 24 % decrease is evident. 12.2.6. Fan Horsepower The fan consumption in horsepower (HP) can be expressed in terms of the air flow (L a ) and fan pressure (P). Horsepower can be based on either static (Ps ) or total pressure (P T ). When efficiency is taken into account then the figure will be the same in both cases. L a PT (HP) T 6356 (I P)s = LaPs 6356 or 0.0001571,,PT (12.3a) or 0.000157L a Ps (12.3b) 416 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT at 68°F (20°C) and barometer 30.00 in Hg. Weight of air at this condition is 0.075 lb/ft 3 for a relative humidity of 62 % [i.e. B.S.848, part 1(1963)]. Where L. = air flow (cfm), P = fan pressure (in WG). Incorporating the fan efficiency, it follows from equations (12.3a) and • (12.3b) that the fan horsepower (FHP) is given by The following results were obtained Psord . 0 = 270 mm WG PT(inlet) = — 250 mm WG + 10 mm WG PS(oullet) = FHPtotal pressure = ( L.Pr L a PS FHPstaiie pressure = ( 6356gs Horsepower is inversely proportional to absolute temperature. EXAMPLE 12.5 Calculate the necessary installed motor horsepower for an exhaust fan moving air at a rate of 113 500 lbs/hr at 176°F (80°C). The static pressure requirements for the fan is 81 in WG. The barometer stands at 3000 in Hg. The fan static efficiency can be taken as 70 %. Solution based upon equation (12.3). Wt of air = 30— 10 = 20 mm WG 1/2 Velocity = [2 x 9.81 x 20 Pwater 1000 Pair = PD = PT — Ps = 1891 lb/min Now 36 1891 x = 31 000 cfm Air volume handled by fan — 0.075 528 at all temperatures Static pressure at 68°F = (8.5) x Fan horsepower = If the fan horsepower is 67 HP, and the inlet and the outlet ducts are 900 mm calculate 1. static and total pressure heads produced by the fan, 2. air flow rate, 3. efficiency based upon static pressure. 1. Static pressure produced by the fan = 10 — ( — (250)) = 260 mm WG, Total pressure produced by the fan = 30 — ( 250) = 280 mm WG. 2. Air velocity given by r2gH1 112 , where H' is the velocity head (metres of air) 113 500 60 + 30 mm WG PT(outlet) = 6356riT Pwater 0.7 (at 80°C) = 10 3 Pair 636 = 10.6 in WG 5 28 31 000 x 10-6 x 0.000157 u = 19.8 m/sec 1r 2 3 Air flow rate = 19.8 x — 4 (0.9) x 3600 = 45 350 m /hr = 73.5 at 68°F at a temperature of80°C — 45 350 kg/hr 28 Fan HP at 176°F = 73.5 x636 L- = 61.0 To cover start up conditions size motor 73.5 + (15 %) = 85 Nearest size = 100 HP EXAMPLE 12.6 During the commissioning of a spray dryer, the performance of the exhaust fan under operating conditions is to be determined. This was carried out with a pitot-tube assembly. The duct temperature was 80°C. 417 3. Work done by fan = mass air flow x static head = 45 350 x 0 pair 45 350 260 kg m 3 x 10 = 3270 3600 sec 1000 = 42.7 HP Fan efficiency = 42.7 x 100 = 64 418 SURVEY OF AUXILIARY EQUIPMENT 12.2.7. Effect of Altitude on Fan Performance With the decrease in air density with increase in altitude, higher air volumes must be handled by the fan for a given mass flow requirement. Care must be taken in sizing fans for operation at altitude. Data specifications are based upon sea level conditions and thus compensating factors must be applied to prevent fans and motors being undersized. A mass air flow at sea level is equivalent to a volume that will be 43 % greater if the fan was operating at 7500 ft. (This is computed from taking the atmospheric pressure at sea level at 760 mm Hg and the atmospheric pressure at 7500 ft at 530 mm Hg where increase in volume is in the ratio of 760/530 = 1.43.) Pressure drop will increase substantially if a fan sized at sea level operates at altitude. Pressure drop varies as the square of velocity and for the above example a 43 % increase in velocity will give a 206 % increase in pressure drop. Larger fans and motor sizes are a characteristic of high altitude working due to the additional fan work load. Actual system losses are lower with lower air density, and correct sizing can hold velocities down to reasonable figures. 12.2.8. Fan Mounting Fan operation can be marred by excessive noise and vibration if fans are insecurely mounted. The larger and faster the fan the greater the possible noise and vibration levels. Wherever feasible, fans should be mounted at floor level on solid concrete foundations. However, in spray dryer layouts it is not often convenient to have all fans at floor level, as an extensive duct system would result. Fans mounted at elevated heights cannot have concrete bases due to load limitations of the building structure, but as an alternative, as solid a base as possible must always be provided. Spring loaded or rubber anti-vibration pads should be placed between the fan/motor frame and the building structure to dampen vibration transmitted to the structure. Failure to do this in steel building structures can give rise to vibrations being amplified within the steelwork, leading to vibration and noise problems away from the area of fan mounting. Vibration transmittance can be a problem if automatic control equipment is also mounted on the building steelwork. 12.2.9. Fan Noise Fan noise is becoming a factor of increasing importance to acceptable fan operation, due to the more stringent noise level standards being set as permissible in working areas. Fan noise will increase over normal levels, if (a) the fan mounting is insecure, (b) the fan rotor is out of balance, (c) fan bearings are on the point of failure, or (d) the fan is operating on increased powder—air loadings, (e) incorrect original selection gives too high a speed or poor efficiency. SURVEY OF AUXILIARY EQUIPMENT 419 General maintenance should prevent frame mounting looseness and frequent bearing failure. It is always good practice to check pulley belt tension between motor and fan. The fulfilling of lubrication schedules will do much to prolong bearing life. Out-of-balance operation often occurs through build-up of product on the fan blades. The blades must be regularly washed, and drainage cocks are invariably provided in the fan casing to facilitate easy fan washing. 12.2.10. Fan Selection Selection of fan design and fan size requires data on the operating conditions : (a) Air flow rate as mass flow. (b) Pressure (static and total). (c) Air density (based upon temperature, altitude and moisture content). (d) Available power. (e) Available speed range and application, powder loading, etc. Selection is made from fan curves. Manufacturers and suppliers have available performance curves for each design and size of fan offered. Selection requires finding the fan, whose performance meets the operational data requirements. There are many ways of presenting fan data. Performance curves can apply to a single fan size, or be extended to cover performance of a range of fan sizes of fixed design. The fan design is first selected. This is comparatively straightforward for a spray dryer fan, as the range of suitable designs is not extensive. Fans are normally of the backward curving blade type. For the selected design, the performance curves that cover a range of fan sizes and air rates are inspected. With data on working conditions, the correct fan size is selected automatically. If two or more fan sizes appear applicable, the fan is chosen having the highest efficiency at the required working conditions. Note that when inspecting performance curves, they are related to a standard temperature and barometer. The working pressure must be corrected to the standard basis. Having fixed the fan size, the fan blade speed and efficiency are read off the curves. The required horsepower is calculated using formulae that accompany the performance curves. 12.3. Mechanical Powder Separators Mechanical powder separators for product separation and recovery (collection) are mounted directly after the drying chamber. Dry cyclones, bag filters and electrostatic precipitators are used for dry powder collection. Wet scrubbers, wet cyclones and irrigated fans are used as final air cleaning units. Equipment is discussed from a practical viewpoint. For comprehensive description of equipment, theoretical principles of operation, 420 SURVEY OF AUXILIARY EQUIPMENT mathematical treatment of power—air separation, the reader is referred to other available publications (124) (172) (178) (179) (504). 12.3.1. -Dry Collectors (a) Dry Cyclones A dry cyclone is a centrifugal particle separator. The theory of operation is based upon vortex motion where the centrifugal force acting on each particle causes particle movement away from the cyclone axis. Particle movement in the radial direction is the resultant of two opposing forces. The centrifugal force acts to move the particles to the cyclone wall, while the drag force of the air acts to carry the particles into the central air core. The theory of particle movement in a spinning gas is given in detail elsewhere (178) (180). The centrifugal force is predominant, and particles pass through the air stream, concentrating in the outer layer of air moving around the inner surface of the cyclone body. The centrifugal force acting on each particle is represented by the term mV,2 1r where m = mass of particle, V, — tangential air velocity and r = any given radial distance from cyclone axis. Inspection of this term indicates that particles just outside the central air core of the cyclone are subjected to the greatest centrifugal force as here the velocity is highest while the radial distance is small. Time is required for product to move outwards and reach the cyclone wall, and thus efficient cyclonic separation does depend upon an air residence time in the cyclone being sufficient to permit the completion of product travel to the cyclone wall before air flow turns upwards to the outlet duct. Even when separation has been effected, the upward turn of the air flow must be achieved without re-entrainment of product into the air stream. Aerodynamic parameters of cyclones have been recently (1970) discussed by Muschelknautz and Krambrock (181). The most common form of dry cyclone, used in conjunction with spray drying chambers is the reverse-flow type. The cyclone can operate at either an over-pressure (fan on inlet side) or under pressure (fan on outlet side). In spray drying layouts the fan is mounted on the outlet side, thus enabling the fan to handle powder-free air. Powder and air pass tangentially into the cyclone at velocities that are virtually equal. Powder and air swirl in spiral form down to the base of the cyclone, separating the powder out at the cyclone walls. Powder leaves the base of the cyclone. The clean air spirals upwards along the axis of the cyclone and passes out of the top. Flow through the cyclone is essentially a double spiral. The presence of the upward spiral forms the central core. The central core diameter has been related to the exit cyclone duct diameter (ID ex „) and ranges between D exi , to iD exit . Powder that has not been separated out by the time the air flow direction turns upwards into the central core, will pass out of the cyclone with the air. The double spiral flow concept is only a fair representation SURVEY OF AUXILIARY EQUIPMENT 421 of actual flow patterns in the cyclone. Actual flow patterns are complex, as there are secondary air flows between the two spirals. Although much analysis of flow profiles within cyclones has been carried out using tracer, or pitot-tube techniques (180) (182) the nature of the secondary air flow is still unknown. The secondary air flow..is due to the interaction of axial and radial velocity components, but there is much discussion as to whether the flow is a single vortex covering the whole length of the cyclone, or a double vortex. The complexity of flow within a cyclone results in particle sizes separated out in cyclones to be smaller than predicted theoretically, even when using realistic assumptions. Particle sizes above 20 micron can be removed in practice. The possibility of sizes less than 20 micron being collected falls off rapidly with decreasing size. High efficiency units for removal of sizes 10-20 micron require precise proportioning of the cyclone dimensions. AIR OUTLET AIR INLET AIR INLET PRODUCT OUTLET a, b. Figure 12.8. Basic designs of industrial cyclones. (a) Tangential inlet, (b) Wrap-around inlet. SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT In the basic industrial cyclone design powder-laden air enters tangentially setting up spiral motion within the cyclone. A modification of the basic design is the 'wrap-around' inlet or volute inlet, where higher collection efficiencies are claimed due to more controllable and uniform flow spirals set up in the upper part of the cyclone. The tangential inlet and volute inlet designs (figure 12.8) are widely adopted in spray drying installations. The majority of airborne powder from drying chambers have a size distribution within a range that these designs can handle. The volute inlet is often used to handle very high air throughputs and achieve high collection efficiencies. There are many variations of the above two designs. Special cyclones feature helical shaped roofs, multi-cylindrical and cone sections, powder by-pass techniques, vortex shields, special outlet duct designs and hoppers. The helical shaped roof is aimed at reducing turbulence in the top of the cyclone leading to higher efficiencies at lower pressure drops. Multicylindrical and cone sections of the cyclone body produce controlled and uniform increase in velocity down the cyclone. Powder by-pass techniques permit powder to by-pass the air flow in the top section of the cyclone, an area which for conventional designs gives the greatest likelihood of powder re-entrainment around the entrance of the outlet duct. Vortex shields act to stop the downward spiralling air flow. Through precise adjustment reentry of separated powder into the upward outgoing air flow is minimized. A further attachment is the hopper at the base of the cyclone. The hopper again acts to prevent re-entry of powder back into the outgoing air flow. Scroll outlet ducts are featured enabling air to leave the cyclone with a minimum of resistance, thus contributing to low overall pressure drop. (i) Cyclone Performance. The performance of cyclones when handling spray dried products has great importance in the design, layout and operation of spray drying plant. Performance depends on such factors as product particle size, shape and distribution, bulk density and powder loading in the air. Characteristics that establish whether cyclones are suitable for a spray dryer layout include (a) a size parameter to express particle size that can be collected in a cyclone, (b) the overall cyclone efficiency when handling a product of known size distribution and particle form, (c) pressure drop over the cyclone. These characteristics decide whether a single cyclone or a cyclone battery can suffice and operate as the only collection unit, or whether secondary equipment is required after the cyclone(s). The Size Parameter. Two size parameters are used to define particle sizes a cyclone can remove. These are the critical particle diameter and cut size. The critical particle diameter is defined as the particle size that will be completely removed from the air flow (100 % collection efficiency). This diameter has been adopted as a means of stating the separation expected from a given cyclone design. Equations can be drawn up expressing the critical diameter 423 in terms of the air-flow properties and cyclone dimensions. There are limitations to these equations as assumptions, often unrealistic are involved in their development. Flow patterns within cyclones are complex, whereas the equations express simple systems. No theoretical model is available that adequately covers particle movement within cyclones. It is virtually impossible with `todays state of the •are, to deal mathematically with the flow effects due to particle interference, particle re-entrainment tendencies and the varying velocity profiles within the cyclone. Strauss (178) lists assumptions and quotes the available equations. However, predicted values of critical diameter are not usually borne out in practice. There is no sharply defined point where a particle size is either 100 % separated or 100 % lost in the exhaust air. For the critical particle size to have real practical meaning, the grade efficiency curve (figure 12.9) would have to follow the line ABC. It does not, the line (curve AED) being representative of actual conditions. Referring to figure 12.9 predicted critical particle diameter lies in the range 10-20 micron, but practical conditions indicate 100 % separation to be achieved only for the much coarser particle size of 105 micron. The more favourable parameter to express separation is the cut size. 15 105 C 0. COLLECTION EFFICIENCY % 422 PARTICLE SIZE ( MICRON Figure 12.9. Theoretical and actual grade efficiency curves. The cut size or cut of the cyclone best represents the obtainable separation. It is defined as the size for which 50 % collection efficiency is achieved. (The 50 % level on the grade-efficiency curve gives the cut size.) Grade efficiency curves, obtained experimentally are the most reliable source of information to obtain size separation data. Grade efficiency curves are 424 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT drawn up by systematically operating a cyclone with a uniform particle size dust. The deviation of such a curve from the theoretical case is shown in figure 12.9. Area ABE represents particles that are expected to escape separation, but are separated in practice. This extra degree of separation is due to agglomeration effects and influence of larger particle movement. Area CDE represents particles that should have been collected, but are not due to particle interference, particle re-entrainment and eddy air flow effects within the cyclone. (ii) Overall Cyclone Efficiency. The overall efficiency of a cyclone is that obtained when handling a product of definite size distribution. The grade efficiency curve cannot be applied directly to spray dried product entering cyclones. However, knowing the grade efficiency curve and the product size distribution, the overall efficiency can be calculated. It is common to know with a fair degree of accuracy the particle sizes entering a cyclone from a spray drying chamber. For a layout shown in figure 9.1(b), where all product is exhausted to a cyclone collection unit, size data are obtainable from atomization and spray evaporation characteristics. For a layout shown in figure 9.1(a) size data are not so readily available. However, the chamber design and dryer operation enables the proportion of the total product throughput that is separated out in the chamber to be often estimated or measured. The size range of this separated fraction (chamber fraction) can be analysed. From the atomization and chamber fraction particle sizes, the likely size distribution and quantity of product passing to the cyclone(s) can be drawn up. A calculation of the overall cyclone efficiency is illustrated in example 12.7. 100 EXAMPLE 12.7 A spray dryer produces 1000 kg/hr of dry product, 85 % of the production is recovered from the chamber base, while the remainder passes to two identical reverse flow cyclones. The grade efficiency curve for the cyclones are shown in figure 12.10. Powder samples taken between the chamber and cyclone inlet were analysed to give a size distribution of the airborne product (table 12.3, column 2). Predict the quantity of product not separated out in the cyclones. The solution involves the grade efficiency curve to determine extent of separation for each mean of the size range used during the analysis. The overall efficiency is then calculated from summing the product of percentage efficiency in each size range and percentage occurrence, and dividing by 100. Table 12.3 (1) (2) Particle size (micron) Size occurrence passing to cyclones 0-5 5-10 10-15 15-20 20-25 25-30 30-40 40-50 50-60 60-70 2 (3) (4) Grade efficiency ( %) Overall efficiency ( %) 430 76.0 89.0 94.0 95.5 96.0 96.5 970 97.5 98.0 0.86 3.8 12.46 35.72 18.15 11.59 4.85 2.91 0.97 0.98 5 14 38 19 12 5 3 92.29 GRADE EFFICIENCY 100 Column (4) = [column (2) x column (3)1 x 10 60 425 -2 Overall efficiency = 92.3 1000 x 15 = 150 kg/hr 40 - Product entering cyclones = 20 Product leaving cyclones = 150 x — = 1.155 kg/hr 100 100 7.7 0 10 20 30 40 PARTICLE SIZE 50 60 70 80 90 ( MICRON I Figure 12.10. Grade efficiency curve for cyclones specified in example 12,7. 100 Example 12.7 shows that a low overall efficiency value (i.e. in the neighbourhood of 90 %) does not automatically mean high quantities of product lost with the exhaust air. The grade—efficiency curve indicates the cyclone design to be of the high efficient type. The low overall efficiency is due to 426 SURVEY OF AUXILIARY EQUIPMENT the fineness of the product the cyclone handles. Due to a low powder loading, only low weight loss levels from the cyclone actually result. In fact if all production from the spray dryer was passed to cyclones for collection, overall efficiencies of over 98.85 `)/, are required to improve upon the separation achieved in the example. This may be above the level of collection achievable for handling the total production in cyclones even though increase in powder load to a cyclone often acts to increase the overall efficiency. In many cases, the increase in overall efficiency obtained by increasing the cyclone powder loading does not result in a decrease in powder weight loss from the cyclone. Data pertaining to overall efficiencies of cyclones prove useful when comparing possible cyclone performance with actual performance under operating plant conditions. If it becomes evident during operation that product losses from cyclone(s) are well above values predicted from overall efficiency (while inlet product loading conditions remain approximately the same) faulty cyclone operation can immediately be suspected. The most common cause is leakage of air into the cyclone base. Leakage assists the re-entrainment of product back into the outgoing air stream. Other causes can be (a) change in the particle size distribution of the ingoing airborne product, (b) cyclone overloading, i.e. where a battery of cyclones is involved, partial blockage in one of the inlet ducts may be causing maldistribution of product into each cyclone, (c) the cyclone base is partially or totally blocked. This condition is readily evident by extremely high loss levels. The highest obtainable efficiency of a cyclone depends upon the continuous withdrawal of product from the cyclone base. If withdrawal is impeded and product builds up within the cyclone base, very high loss levels will result from the take-up of powder that settles at the blocked outlet. Efficiencies are reported by Ter Linden (180) and Stairmand (182) to be influenced by cyclone dimensions. If performance is not up to requirement, modification to the dimensions can increase efficiency. Alteration to the cylindrical height, exit duct protrusion within the cyclone, and cyclone base design are the usual features that are modified. Efficiency has been reported to increase as the ratio of cyclone diameter to exit duct diameter is increased. A ratio value of three appears the upper limit for effective improvement. Increasing the cyclone height in relation to the exit duct diameter appears to improve efficiency, where a ratio value of 10-11 seems the optimum order. Other dimensions influencing efficiency are (a) the precise positioning of the exit duct entrance in relation to the inlet duct, and (b) the inlet and outlet duct sizing. How much these dimensions contribute to collection efficiency depend upon the design of cyclone inlet. Increase of air throughput with the accompanying increase in air velocity acts to improve efficiency (181) but any improvement can be offset by pro- SURVEY OF AUXILIARY EQUIPMENT 427 moting greater turbulence within the cyclone and increasing product reentrainment. Increasing the product loading of the cyclone is often suggested as a sure way to improve cyclone performance. This has been found by experiment to be true to certain limits, as increase in the number of large particles will entrain or agglomerate larger numbers of smaller particles that would otherwise be lost in the exhaust air. However, this effect can be more than compensated for by the presence of larger product concentration in the lower parts of the cyclone leading to greater degrees of product re-entrainment. Optimum loadings are determined using standard powders. Particle size distribution of standard powders are shown in appendix 11. However spray dried products deviate from standard dusts in size, shape and density, and reproducing optimum conditions in actual plant depends upon extrapolation of test data to actual conditions. (iii) Pressure Drop over Cyclones. The pressure drop characteristics of cyclones have direct bearing on the economy of the spray drying operation. Pressure drop losses influence power requirements, and decide fan sizing for the exhaust air system. Cyclones used in spray drying applications operate between 3-8 inches of water pressure drop (75-200 mm WG). The effect of powder loadings on pressure drop in cyclones has been discussed by Kriegel (183). The total pressure drop is a combination of many individual losses. Losses are due to friction and air expansion or contraction at the cyclone Figure 12.11. Measuring pressure drop over a cyclone. Item A. Pressure tapping measuring total pressure drop (APT). Item B. Pressure tapping measuring static pressure drop (APO. 428 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT inlet. The kinetic energy losses and static head losses within the cyclone can be measured as dynamic and static pressure differences using a manometer. One limb of the manometer is connected to the inlet cyclone duct, and the other limb is connected to the outlet cyclone duct (figure 12.11). If the pressure tappings in the inlet and outlet ducts record impact pressure, and the inlet and outlet duct areas differ, the total pressure drop will be recorded at the manometer. If the pressure tappings record the static pressure drop (AP,), and the inlet and outlet areas differ, the dynamic pressure difference (AP d ) can be calculated from the equation APd = 1 p a (172 — k r owlet — Vinle t) 2 g (12.4) where V = air velocity, p a = mean air density over the cyclone. Adding (APd ) to the measured (APJ gives the total pressure drop (AP T ) across the cyclone. Use of equation (12.4) is shown in example 12.8. EXAMPLE 12.8 A cyclone handles 22 000 kg/hr of air. The inlet duct area is 1 m 2 and the outlet duct 0.5 m 2 . The measured total pressure drop is 140 mm WG. There is a negligible temperature drop over the cyclone, the air temperature remaining 80°C. What correction to the total pressure drop must be made to obtain the static pressure drop? Now equation (12.4) expressed in mm WG pressure drop and air flow rate (L a ) in kg/hr becomes 11 L a 2 APd = 2 k 3600) 1 1 Pa 9.81 [19!(/0.uunet, nF(A? r.k—inlet) where V= La L a = 22 000 kg/hr 2 Aoutiet = 0.5 m 2 Pa = 1 kg/m' at 80°C 11220001 2 1 r 1 2 d = 2 3600 ) 9.811_1 x 0.5 2 1 37.3 = 2 9.81(4 — 1) = 5.7 mm WG AP, = APT AP, = 140 — 5.7 — 134.3 mm WG Methods of predicting pressure drops have been developed out of flow theories by Ter Linden (180) Stairmand (182) and Shepherd and Lapple (184). The limitations of being unable to adequately define the complex cyclone air flow patterns are apparent, as predicted values from generalized equation are not confirmed in practice. Cyclone manufacturers supply correlations that have been • established from operational data. Various correlations appear in the technical and trade literature for application with certain designs. For wrap-around inlet designs of dimensions conforming to cyclone type 2, table 12.4, the pressure drop (AP) is given by the relation: AP = 1., P c/4T 2 (12.5) where K2 is a constant established in practice, T = air temperature, d = cyclone diameter, / 3,3 = barometric pressure. Expressed in metric units where AP is mm WG, L a = kg/hr, T = D C, PB = mm Hg, d = metres, equation (12.5) becomes 760 L )2 (12.6a) AP = s ( T + 273) PO 6700 d' Expressed in British units, where AP is in WG, T is °F, P„, is in Hg, d is ft, and L a is lb/hr, equation (12.5) becomes AP = 29.92 L )2 —(T + 460) 4 PB 9270 d AP = 0.013v c2 p a APT = 140 mm WO AP Hence (12.6b) The simplicity of the equations, whereby the pressure drop is related directly to the cyclone air rate, air temperature, and barometric pressure and only one cyclone dimension, the diameter, is obtained at the expense of some variation between actual and predicted values. A comparison of values has shown differences between values to be small enough to enable practical use of equation (12.5). For cyclones with the helical inlet design, trade literature reports the pressure drop (in WG) to be predicted by (179) paA Hence &l et = 1.0 m 429 12 (12.7) where p a = air density (lbs/ft 3 ), ye = average inlet velocity (ft/sec). For cyclones with the standard tangential inlet design (i.e. conforming to the dimensions in table 12.4, type 5), the pressure drop (in WG) is predicted by (179) (12.8) AP — 0-024v c2 p a C S aS a, a8 High capacity SURVEY OF AUXILIARY EQUIPMENT 411 n.P.d ":5 6 c, (f) °' o C: A S 0 N 6 N SURVEY OF AUXILIARY EQUIPMENT Cr C :1=2. a t:i 3 • 3 O a 38 O A G a ` N 0 L a = 35 000 kg/hr aDk. T = 80°C AP = a 0 3m Pa = 758 mm Hg 45 N 6 431 EXAMPLE 12.9 A 3 metre diameter cyclone (design type 2, table 12.4) handles an air flow rate of 35 000 kg/hr. The average air temperature over the cyclone is 80°C. The barometer stands at 758 mm Hg. Predict the pressure drop. Using equation (12.6a) where d 99 5 E a (35 000) 2 1 (80 + 6700 34 760 = 120 mm WG 41 (iv) Cyclone Layouts. The mounting of a single or multi-cyclone arrangement after a spray drying chamber is well established. For a multi-cyclone layout, the mounting is usually in parallel (figure 12.12). Where used in series a powder classification is obtained. The choice between single or multi-cyclone units is dependent upon the product application. However, if the exhaust drying air can be handled in a single cyclone unit, and the obtainable recovery efficiency of the order of 98 % is acceptable a single cyclone system is adopted. The ease of product removal and handling, a minimum of interconnecting ducts, and the ease in which the whole layout can be cleaned are important advantages. However, exhaust air can be divided and distributed effectively into two or more cyclones, A higher overall recovery efficiency is obtainable from a battery of smaller cyclones in theory, but any increase in efficiency over the single cyclone layout is dependent upon even distribution of powder and air into each cyclone. (95 - 0 .5 • O a a 99 Table 12.4_ Dimensions of Indus 430 0 .94 Ma a 91 1 9 N N N -5, N N 6 A (-9 9 C C 4 ;7 Tr,' •cl Uj s .5 ro 74 1 3 cn Li .5 -iv 3 -a 0 be a En .5, C C .5 .5 O ,t1 aCa -•-•• 5 co N ro C -' „ ;I 13 N 00 Figure 12.12. Cyclone layout in parallel. 432 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT In practice identical operational conditions within each cyclone of the battery is very difficult to obtain and maintain. Cleaning also is more difficult due to inaccessability, although the mounting of in-place cleaning (CIP) obviates this difficulty. (b) Bag Filters (1) Principles. The bag filter is often the favoured equipment for collection and recovery of powder entrained in the exhaust air of a spray dryer. A bag filter consists of numerous bags, installed so that each bag receives approximately equal quantities of air. The collection of bags is termed the baghouse. The simple principle of passing powder-laden air through a close woven fabric is one of the oldest methods of air cleaning, but, it remains today an efficient means of powder separation, being able to remove particles below 10 micron. With the correct fabric weave, 1 micron particle size can be collected. The performance of bag filters depend upon (a) the type of product handled, (b) the inlet powder loading in air, (c) bag fabric, and (d) bag cleaning procedure. Modern bag filter designs prove reliable in operation, but are subject to strict maintenance and inspection to ensure no bag leakage. The slightest of leaks will quickly diminish the very high collection efficiency levels the units are capable of achieving. A typical grade efficiency curve of a bag filter is shown in figure 12.13. Greater than 99 % efficiency is obtained with 5 micron particles, 99 % efficiency is'obtained with 1-2 micron sizes. (ii) Bag Filter Designs. Bag filters can be classified into three types. Each type is classified according to the bag cleaning operation. • 100 EFFICIENCY 98 - 96 COLLECTION 94 - 92 90 0 2 4 PARTICLE SIZE fi 8 ( MICRON ) Figure 12.13. Grade. efficiency curve for a standard bag filter, 10 433 Type A : Manual cleaning on shut down. Type B: Semi-continuous cleaning (periodic). Type C: Continuous cleaning. Type A. The bag filter is taken out of operation for cleaning. The time between each shut down will depend upon bag area and how quickly the product cake builds up on the bag. As spray drying systems require operation to be continuous, frequent shut-down practice is not acceptable. This type is seldom used, unless the spray dryer is operated batchwise. Such baghouses are a simple construction and form a low cost system. Type B. Cleaning takes place periodically without shutting down the equipment. Cleaning can be accomplished in two ways : (1) The bag filter consists of a series of batch units mounted in parallel. Each unit has many bags. Periodically one of the units is taken out of service for cleaning, while the remaining units handle the total air flow. Each unit is taken out of service in turn, when cleaning is carried out by vibrating the bags. This can be done by swinging the bags to and fro, violent shaking in the vertical plane, or by applying any form of eccentric movement. The cleaning sequence is controlled by a timing device, which can be set to suit the product handled and the powder loading conditions of the baghouse. A complete cleaning cycle of 30-45 minutes is normal. The bag filter requires bags to periodically handle increase in air rate to compensate the loss of air flow to the unit of bags being cleaned. However, the cleaning time per unit of bags can be small in relation to the overall cycle time. For a filter of for example 3-units, the bags may be only out of service 1-2 minutes for cleaning, every 30-45 minutes. The bag filter performance is greatly dependent upon the reliability of the timing device. Failure in the cleaning cycle will result in excess cake layers building up on the bags in filtering service. The increase in pressure drop over the filter bag leads to reduced air flow and difficulties arising in the spray drying chamber. Should minor maintenance be required on any unit of the baghouse, the timing device can be adjusted to extend the cleaning down time cycle, so that work can be carried out on the bags or vibrating mechanism without interrupting plant operation. A series of units mounted in parallel is illustrated in figure 12.14(a). (2) The bag filter can consist of a single unit, where each bag is cleaned periodically during operation. It is not necessary to shut down any part of the baghouse for cleaning. A common form of cleaning device for this type of bag filter is the pulsed air jet (figure 12.14(b)). An air jet can be directed into each bag, and each bag is frequently pulsed with a high pressure air jet. The pressurizing of the bag prevents air flow through the bag, causing the bag to vibrate or puff out and dislodge the product away from the bag fabric. 434 SURVEY OF AUXILIARY, EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT The pulses can be of very short duration; for example 0.1-0-2 seconds. Every bag is pulsed once every 10-15 seconds. 90-100 psig (6-7 atm) air pressure usually suffices. Solenoid valves actuate the air nozzles. COMPRESSED AIR SOLENOID VALVES • GLEAN AIR 435 high volumes of powder-laden air handled per unit area of bag fabric. The continuous cleaning also maintains low pressure drop conditions over the bags. (iii) Bag Filter Performance. The performance of a bag filter, judged by the overall collection efficiency of airborne powder is the best of the collection equipment used in spray drying plant. Achieving and maintaining such high performance does depend, however, upon (a) maintaining a leak-proof bag system, (b) high bag durability to resist rapid wear on each bag due to the mechanical handling each bag receives during cleaning, (c) effective bag cleaning procedure. Failure on these points lead to product losses greater than those from dry cyclones. The air velocity through the bag fabric is kept low (1-15 ft/min, 0.5-7.5 m/sec). For fine powders, air velocities are of the order 1.5-3.0 ft/min, but the coarser the product, the higher the velocity that can be used. Furthermore the shorter the cleaning time per bag, the higher is the permissible air velocity (filter face velocity). Table 12.5 shows typical face velocities in the three types of bag filter designs considered above. The pulsed reverse jet type can operate effectively up to 15 ft/min on particle sizes present in exhaust air from spray dryers, due to the effective and rapid cleaning sequence. -• NOZZLES PRODUCING AIR JETS 000 FILTER DI-DW RING [MOVING UP AND DOWN IN VERTICAL PLANE OVER RAG SURFACE} Table 12.5. Recommended Face Velocities for Bag Filter Designs .--DAD FILTER Bag filter design Cleaning practice Mode of cleaning CLEAN AIR OUT POWDER LADEN AIR PRODUCT Type A Manually cleaned Type B Semi continuous automatically cleaned c. POWDER DUD Face velocity (ft/min) 1-3 Intermittent pulsed air jet 3-6 Frequent pulsed air jet 10-15 Shaking 3-6 Traverse air jet 6-12 Figure 12.14. Designs of bag filters. (a) Bag house consisting of separate bag filter units in parallel, Each unit removed alternatively from system for reverse air flow cleaning, Units 1, 2, 3 filtering powder-laden air. Unit 4 on reverse air flow cleaning. (b) Bag filter using air jet cleaning principle. (c) Bag filter using the air blow ring cleaning principle. Type C Type C. The air jet cleaning system with its short duration pulses can be considered a continuous cleaning operation. However, there are designs that are completely continuous. One established design is the use of blow rings (figure 12.14(c)). Instead of a pulsed air jet, air flows continuously from an air ring that traverses up and down the bags. The air ring blows product away from the bag fabric. Air pressures are of the order 25-35 in WG. The advantage of the blow ring system, apart from the continuous product discharge achieved, and low air pressure system, concerns the Table 12.5 gives the recommended face velocities. Use of too high a velocity causes compaction of the product on the fabric. Compaction causes increase in pressure drop over the bag and possible penetration of product through the fabric. The increase of force on the bag also leads to earlier fabric weave failure, and puts greater demands on the cleaning procedure. The product becomes impregnated within the weave to a greater extent than is normally allowed for when sizing the unit and specifying operating conditions. Continuous automatically cleaned 436 Even with correct face velocities and effective cleaning procedures some product particles remain in the fabric weave. In fact, their presence, to a li mited extent, is a requirement for optimum filtering efficiency. After a new bag has been in operation for a period, the powder content that is not removed during the cleaning cycle remains at a constant level. The presence of this retained product is shown by the pressure drop through a new unused bag at a constant air flow rate to be less than the pressure drop over the same bag when mounted in the baghouse following cleaning, and operating on the same air flow. The constant powder content level in the fabric weave is termed the equilibrium powder content of the bag fabric. The requirement of maintaining correct face velocities, that are invariably low, results in large fabric areas for filtration. Bag filters associated with spray dryer chambers of high evaporative capacity are large units. (iv) Pressure Drop over Bag Filters. The pressure drop over bag filters used in spray drying plant generally ranges between 1.5-8 in WG (40-200 mm WG). The pressure drop value is difficult to predict. Data are obtained experimentally and are made available by manufacturers of bag filter equipment supplied for spray dryers. Semi-empirical methods are available to predict the order of pressure drop for various bag fabrics. The methods are based upon the so-called `channel theory and fibre drag theory'. Full details are given by Strauss (178). (v) Bag Filter Fabrics. The fabric used in a bag filter is selected from considerations of cost, powder characteristics, and operating air temperature. The more exacting the operating conditions for the bag, the more expensive is the fabric. With spray drying plant, air temperatures the bag fabric must withstand are not excessive, 265°F (130°C) being of maximum order, as high temperature prevention is built into the dryer control system. However, if temperatures in excess of this level are to be handled, bag fabrics are available to meet these conditions (silicone treated glass fibre). The properties of various bag filter fabrics have been reviewed recently by Walling (362). Table 12.6 lists properties of common natural/synthetic filter fabrics. (vi) Use of Bag Filters. Bag filters are used where 100 % collection efficiency is required from a one-stage separation unit. The complete range of available bag filter designs are reported by Strauss (178). With the use of top quality bag fabrics and maintenance of leakproof bags, the bag filter proves an efficient unit. Maintenance is constantly being reduced through improved baghouse design, as reported recently (1970) by Pring (186), and (1971) by Akenhead (485). Capital costs can be as much as five times that of a high efficient cyclone and running costs just as high, but these factors are often compensated fully by the increased recovery of product. If the product has a high value per unit weight, the substantial savings in reduced losses quickly accounts for increased capital and running costs. Cases where 437 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT Table 12.6. Properties of Bag Filter Fabrics Natural/ synthetic fibres 1 Cotton Wool Polypropilene Polyamides (nylon) Acrylics Polyesters Fluorocarbons (teflon) Glass-fibre Maximum operating dry air temperature (°C) Resistance to : Flammability Alkalis Biologicals 90 90 1.00 110 120 130 H M H H M H L L H H H 1-1 H L H L L M 260 310 H H L Acids H L L = low, M = medium, H = high. a bag filter is not recommended are (1) handling air of high moisture loading, (air near dew point), (2) hygroscopic or deliquescent airborne particles, (3) products requiring high standards of hygiene in handling, (4) handling very high air temperatures, (5) particles/agglomerates in stringy (fibrous) form. A suitable exception in case (3) is egg white powder (p. 568). (vii) Bag Filter Layouts. Bag filters are often mounted directly after the drying chamber as the main separation unit. The efficiency of the unit is very high, and secondary separation equipment is seldom necessary. High efficiency of separation is dependent upon all bags in prime physical condition and correctly mounted. A baghouse, in view of maintenance requirements should be positioned to enable good accessibility in an area of good lighting and ventilation. (c) Electrostatic Precipitators (1) Principles. Electrostatic precipitators are not used widely in spray drying plant in spite of their forming a low pressure drop device capable of high collection efficiency performance. Initial cost in purchase and erection is high. Where installed electrostatic precipitators form main powder separation units. High air volume rates are handled. There are two types of precipitators (a) plate type and (b) pipe type. The plate type is ideal for dry powder collection. The pipe type is generally not applicable to spray dryers being more suitable in handling volatilized fumes, liquid or slurry droplets (504). The principle of operation is the creation of a strong electrical field into which flows powder-laden air. The high voltages required are produced through rectifier and transformer units. The system is shown in figure 12.15. 438 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 439 100 80 )- 60 z Ui u_ GO Lu POWER SUPPLY RECTIFIER CONTROL TRANSFORMERRECTIFIER UN IT 20 ELECTROSTATIC PRECIPITATOR Figure 12.15. Electrical power system for an electrostatic precipitator. A large voltage difference between a discharge electrode and the collecting earthed plate forms the desired electrical field strength. The earthed plates are mounted in series with the discharge electrode suspended between the plates. The whole plate system is enclosed. The powder-laden air from the spray drying chamber enters the precipitator and flows between the plates at low velocity. Discharge of air ions from the discharge electrode combines with the powder particles. Powder particles obtain a negative polarity, and move towards the positively charged collecting plates. On contact with the plates the particle charge is dissipated. Particles are removed from the plate area by a tapping mechanism, and the powder falls to the hopper beneath. Wet washing of the plates is also possible. There is a very low pressure drop over the system, as force is only applied to the particles. Powder particles that adhere to the plates, and particles of high resistivity (which prevent the electrical mechanism) are not suitable for such equipment. Spray dried products that can be effectively handled include cement, bauxite, gypsum, mineral concentrates and some foodstuffs. (ii) Performance of Electrostatic Precipitators. Electrostatic precipitators can collect airborne powder with up to 99 % efficiency for particle distribution sizes greater than 1 micron. The particle density appears to have little effect on efficiency. High efficiency levels are obtained within the pressure drop range of 0.25-1.0 in WG (6-25 mm WG). The typical grade efficiency curve of an electrostatic precipitator is shown in figure 12.16. Plate face velocities are of the order 2 ft/sec (0.6 m/sec). Available methods for predicting performance are of doubtful validity for many powders. For further details on performance, reference should be made to Strauss (178). Performance data are given by Andersen and Heinrich (187). 5 10 15 20 25 30 POWDER PARTICLE SIZE (MICRON I Figure 12.16. Grade efficiency curve for a dry electrostatic precipitator. (d) Gravity Settlers Gravity settlers can rarely be used as main or secondary separation units of a spray dryer as they are only suitable for collecting particle sizes exceeding 200 micron. However, there is one collection need a gravity settler will readily meet, especially in the food industry. This is the collection of product flakes forming from deposits that gradually build up on the duct surfaces after cyclones or bagfilters and within the air hood. As most powder separation units installed in spray drying plant never achieve 100 % efficiency, there is always the chance that the small quantities of products that do escape to the dryer air hood will deposit out on the duct and air hood surfaces. Deposits are caused by escaped particles becoming wet and sticky in the exhaust air that may well be saturated on being cooled during passage to atmosphere. Over a period of time a deposit layer will build up in the duct system. These deposit layers are not particularly elastic, and after reaching a certain thickness will crack and break away. Break-away is severe during start-up or shut down of the dryer - when deposit layers crack due to duct work expansion, contraction or vibration. The start-up of a dryer may well create a high concentration of product flake discharge from the air exhaust system. This discharge causes fouling of the dryer roof and a pollution nuisance to surrounding property. To catch such flake discharge, gravity settlers are installed on the dryer building roof over the exhaust air outlet duct. They often replace the air hood. The gravity settler is designed for very low pressure losses, and operation does not call for a larger exhaust fan. The principle of operation is the 440 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 441 car sudden reduction of air velocity and change in air flow direction. Wall baffles assist flake fallout. A gravity-settler is shown in figure 12.17. It consists of a lightweight box, having a number of compartments formed by the wall baffles. It is often a wood structure with a washable lining of plastic or rubber. Air flow through the box is of the order of 15-20 ft/sec (4.5-6.0 m/sec). CL EA N AIR WATER KU LES WATER NET DE-ENTFLumm SCRUDDER WATER J el LE 7 INLET impIND ELI EN E BAFFLES AIR OU T ❑ LIGHTS 1 SAFETY NET POWDER LADEN y- AIR EXHAUST ❑RYI NG AIR T BAFFLE PowDER LADEN R INEEwn KVIENDLE ACCESS DOOR FOR CLEANING A BAFFLES SCRUBBER WATER SCESIDECR ELATE. =RIMIER 1.1 ER CLEAN MI TO DRAIN TRAP DOOR IN BAFFLE TO DRAIN Figure 12.17. Gravity settler. After dryer operation, the flake deposits can be swept from the floor using a brush or vacuum cleaner. Often the quality of the product is too good for waste disposal. The product is sold just as an inferior grade. The box has drainage, and wash water is on hand for periodic wet cleaning. This is necessary especially where hygienic standards must be maintained (e.g. when handling food products). 12.3.2. Wet Collectors (a) Wet Scrubbers (0 Principles. Wet scrubbers remove 'solid particles from a powder-laden airstream with liquid. The contact between particles and liquid is carried out by : (A) Flow of powder-laden air through a spray (figure 12.18(a), spray chamber type). (B) Flow of powder-laden air through a plate, or packing over which a head of liquid (usually water) is maintained (figure 12.18(b), (c), i mpingement type). (C) Flow of powder-laden air through a venturi, into which liquid is injected traversely at the throat section (figure 12.18(d), (e), venturi type). Types (A) and (B) form low energy systems, while (C) is a high energy system. All three types are used in spray drying plant, although type (B) is not considered if the product powder does not readily dissolve in the liquid or may cause possible clogging of the plates or packing. For operations requiring hygienic operations, type (C) is generally preferred due to the E. DRAIN I Ras POWDER n. LADEN AIR Figure 12.18. Designs of wet scrubber. A, Spray chamber type. B, Impingement type (plates). C, Impingement type (packed). D, Venturi type (vertical). E, Venturi type (horizontal). relative ease of cleaning and maintaining the unit free from deposits over long periods of operation. Wet scrubbers are invariably used as a secondary unit for removal of particles that escape collection in a primary collection unit, e.g. cyclones. It is an effective method of cleaning the exhaust air of last traces of powder. Powder sizes down to 1 micron can be collected, and 99.5 % collection efficiency is generally achievable on 5 micron particles. Typical grade efficiency curves are shown in figure 12.19. Wet scrubbers are used more for air cleaning than product recovery. This is due to the product recovery being in wet form. The solids content of 442 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT the scrubbing liquid requires further drying to recover product in dry form. Although in many cases it is feasible to recirculate the scrubbing liquid thereby increasing its solid content, rarely is it possible to reach solid content levels that can be fed directly back to the spray dryer and dried economically. Invariably concentration is required. la) 80 EFFICIENCY % 60 40 20 5 10 15 20 25 30 POWDER PARTICLE SIZE ( MICRON ) G. 100 80 60 ;•,,■ )2 40 uJ (.7) lL 11 1 - - 20 2 4 10 12 POWDER PARTICLE SIZE 14 15 18 20 (MICRON b. Figure 12.19. Grade efficiency curves for wet scrubbers. Venturi scrubber. (a) Spray chamber scrubber. (b) 443 (ii) Wet Scrubber Designs Spray Chamber Type. A spray chamber wet scrubber is shown in figure 12.18(a). Powder-laden air enters the base of the chamber and passes upwards through sprays. Sprays are formed from nozzles placed around the circumference and/or in the centre of the chamber. The upward air velocity ranges between 1.5-4 ft/sec (0.4-1.2 m/sec). The actual velocity is selected according to the droplet sizes formed at the nozzles. The air velocity permits the spray droplets to fall to the base of the chamber and not be entrained in the cleaned air leaving the scrubber. The scrubber water can be recirculated to the nozzles or directly discharged to the drain. As a droplet falls through the powder-laden air, it contacts particles and collects them by a mechanism of inertial impaction and interception. Stairmand (188) reports on the optimum particle size for collection by a falling droplet. For water droplets between 100-1000 micron, collection efficiency of a 10 micron particle ranges between 70-80 Z. For a 3 micron particle, collection efficiencies are low, up to 20 Vo . A spray of prominently 1000 micron droplets is considered the most suitable, as relative velocity conditions between droplet and particle are more easily maintained in the scrubber in spite of droplet evaporation. As efficiency of. collection is low for particles under 5 micron the removal of fine particles from airstreams requires repeated impacts between particles and droplets. This is achieved by having multi-level nozzle mountings, and a nozzle layout to ensure spray coverage over the entire scrubber cross-sectional area. A typical grade efficiency curve for a spray chamber scrubber is shown in figure 12.19(a). The collection efficiency of the scrubber operating on low powder-air loadings as a secondary separator of a spray dryer is relatively low at 55-70 Y o . However, pressure drop losses are not high and power requirements low. Impingement Type. Collection efficiency of small particles is increased if the airborne particle contacts an extended liquid surface, rather than the surface of droplets. In the impingement type scrubber, extended liquid surfaces are created by liquid flowing over baffles or plates. The powderladen air impinges on these wetted surfaces. Designs of impingement scrubbers are shown in figure 12.18(b), (c). Powder-laden air enters the base of the unit and passes up in a flow counter-current with the scrubbing liquid. Liquid passes from the base to drain or to a recirculation tank. Clean air passes out at the top of the scrubber via a de-entrainer. In figure 12.18(b) liquid flows from the top of the unit over a succession of sieve plates. To achieve maximum collection efficiency on the plates, the powder-laden air is best saturated on arrival at the lower plate. Water mist jets or steam can be added to the inlet airstream to obtain saturation 444 SURVEY OF AUXILIARY EQUIPMENT conditions, or as shown in figure 12.18(b) sprays of liquid are directed upwards under the lower impingement baffle plate. Figure 12.18(c) shows liquid flow over a packed bed. The collection efficiency of the impingement scrubber is higher than for the spray type. When operating on most spray dried products at low powder—air loadings, efficiencies up to 98 % are obtained. Pressure drop losses over the unit tend to be higher than the spray type under identical air and powder loading conditions. Venturi Type. Designs of venturi scrubbers are shown in figure 12.18(d), (e). Powder-laden air is accelerated through a venturi, and at the throat scrubber water is ejected into the air as liquid jets. The air velocity in the throat is high enough to break up the liquid jets and form sprays with droplets dispersed throughout the air flow. The atomization of these liquid jets follows the pneumatic nozzle principle. The scrubbing liquid is separated out of the air in the body of the scrubber. A de-entrainer is fitted in the outlet to prevent droplets leaving the scrubber with the cleaned air. The separated water drains from the scrubber base for discharge to sewer or for recirculation to the liquid jets. The pressure drop over the scrubber is virtually representative of the energy requirements of the scrubber. The energy used in the water jet formation is a minor contribution. The overall pressure drop is high. The high pressure drop levels can be reduced by preatomizing liquid in nozzles instead of using simple liquid jets. However, the total energy consumption remains about the same due to the increase in energy required at the atomizer nozzles to form fine sprays. However, efficiency levels do not automatically increase. Fine droplets are less effective in particle collection than coarse droplets formed from jets. This complies with spray chamber scrubber theory. There is effective contact between powder particles and liquid droplets in the throat section of the scrubber. Collection efficiencies are of the order of 90-95 % for particles above 1 micron. A grade efficiency curve for a typical venturi scrubber is shown in figure 12.19(b). The obtainable efficiency depends upon the liquid rate at the throat. Increase liquid flow increases efficiency. The efficiency is also increased if the air entering the throat section is of high enough humidity to enable saturation to occur within the throat, which is at a lower pressure. Condensation will take place on the particles as they move on out of the throat into a higher pressure region. To assist achieving saturation within the throat steam can be blown into the duct upstream. Efficiencies of venturi scrubbers have been recently (1970) discussed by Calvert (189). The prediction of venturi scrubber performance is reported in detail by Strauss (178). Operational data is given. Pressure drops greatly exceed that of alternative scrubber techniques described above. SURVEY OF AUXILIARY EQUIPMENT 445 To achieve a 95 % collection efficiency of particles above 1 micron, pressure drop losses are of the order of 12-25 in WG (22.5-50 mm Hg). The scrubber can be fabricated in carbon steel for non-corrosive conditions. For exacting conditions, stainless steel or any suitable lining of plastic or rubber is used. The venturi scrubber is the most common type used as a wet secondary collector. It represents a lower capital expenditure than any of the other scrubber types, while producing a performance of high collection efficiency for particle sizes above 1 micron. The unit handles high air temperatures and humidities. Most designs have no moving parts except where a pump is fitted to supply a mounting of atomizing nozzles. Water rate determines the collection efficiency. There are operational disadvantages. The scrubber does require a sufficient water supply, although water may be conserved through recirculation (not with spray nozzle mountings, as the eventual sludge can block the nozzle orifices). Scrubber water discharge can cause an effluent disposal problem, and many products may on this account have to be collected dry in alternative equipment. The hygiene of scrubbers are often insufficient for many foodstuff operations, as the warm, high humidity air enables rapid bacterial growth. 12.3.3. Powder Removal from Mechanical Separators (Dry Collectors) The technique of powder removal plays an important role in separation efficiency especially if the separator operates at a high underpressure. Poor efficiency results from powder being removed too slowly or too quickly, and where air leakage occurs into the separator. Removal techniques are described below with reference to cyclones. (a) Hoppers Hoppers are fitted to cyclones to reduce powder re-entrainment caused by the intensive vortex area at the cyclone base. Two types are shown in figure 12.20(a). For products that do not flow easily (dead products) the sloped sides have to be steeper, or vibrators and electric hammers mounted on the hopper to assist continuous emptying. For sticky products, some form of scraper has to be used. The hopper is then cylindrical to provide an easier scraping surface. A hopper with scraper is shown in figure 12.20(b). Most hopper designs are offered as cyclone auxiliary equipment and used where powder recovery is critical to the dryer operation. (b) Powder Removal Valves Many types of valves are used for powder removal. The type adopted depends upon whether intermittent or continuous discharge is required. For intermittent discharge : (i) Manual butterfly valves. (ii) Manual push— pull valves. (iii) Self-actuating counter-weighted and mechanical operated single or double flap valves. For continuous discharge : (iv) Rotary valves. 446 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT CLEANING --------- I PORTS a. main advantage of the exchangeable bucket system is the ease of ensuring that the cyclone base is free of air leaks during operation. However, this advantage is greatly offset by excessive leakage that occurs during bucket exchange, as a closed valve does not provide a seal between the low pressure at the cyclone base and atmosphere. Often the instance of bucket exchange can be seen from the high powder emission from the cyclone exhaust duct and fluctuations to the inlet drying air temperature of the spray dryer. These fluctuations occur in one fan dryer systems (figure 12.3). When a cyclone bucket is exchanged, the accompanying air leakage past the valve reduces the air flow drawn through the air heater. Heat input remains constant, and thus at each moment of bucket exchange, a sharp increase in inlet drying temperature is witnessed. The suitability of the bucket removal system is closely connected with the inlet drying temperature the product can withstand in the chamber. (ii) Manual Push Pull Valves. The manual push—pull valve is incorporated with the cyclone bucket removal system (figure 12.21(ii)). The mounting of a push—pull valve instead of a butterfly valve greatly reduces the air leakage occurring during bucket exchange. However, the valve performance is suspect on many products which tend to deposit on the sliding surfaces, and render the valve inoperable by eventual clogging. The disadvantage with the bucket system, whatever type of valve is used, concerns the labour and constant attention the system requires during dryer operation. The task often requires lifting substantial weights, and should the bucket be allowed to accidentally fill, excessive powder losses from the cyclone results. Powder discharge from cyclones on industrial spray dryers of larger outputs, employ either a large capacity hopper mounted under the cyclones, or powder discharge directly to a conveying system (band or pneumatic). This obviates the need for constant attention being paid to the cyclone base operation. It does not matter if the discharge device mounted at the base of the cyclone operates intermittently or continuously as long as operation is self-actuating or mechanical. (iii) Self actuating and Mechanical Flap Valves. Self actuating and mechanical double flap valves are shown in figure 12.21(iii). The self-actuating flap valve is counter-weighted and opens automatically when there is a sufficient weight of powder on the valve to overcome the counterweight. It is a simple arrangement but has disadvantages. Its use is restricted to coarse freeflowing powders. The discharging operation is slow during which time excessive amounts of air can leak into the cyclone. The slightest build-up on the edges of the flap will prevent the valve from closing. This condition will cause continuous and undetectable air leakage. Many of these disadvantages are overcome by the use of the double flap valve. The valve is — SCRAPER MANHOLE ROBUST GEAR MOTOR b. Figure 1220. Hoppers. (a) Designs of cyclone hoppers. (b) Hopper with scraper, scraper speed 25-30 rev/min. (v) Pneumatic air locks (vortex air locks). The choice is governed closely by the product applications and type of mechanical separator. Valves (i—iv) are preferred for separators other than cyclones. (1) The Butterfly Valve. The butterfly valve is normally incorporated with cyclones equipped with detachable buckets. In pilot plant or small industrial size spray dryers the amount of powder passing to the cyclone(s) may be small. This is especially so if primary product discharge from the chamber is adopted. A butterfly valve and bucket are then mounted directly to the cyclone base (figure 12.21(1)). The bucket remains fastened to the cyclone until the bucket is approximately half full. During this period the butterfly valve is open. Powder is removed by exchanging buckets. The butterfly valve is closed during bucket exchange. The period between bucket exchange is readily determined from the dryer evaporative capacity. The 447 - - 448 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 449 mechanically operated (often by an air piston or driven cam arrangement). Each flap is timed to open and close in set sequence. Both valves are never open at the same time. The sequence cycle can be set-up so that small quantities of powder are frequently removed from the separator base. A suitable sequence cycle could be as follows : o sec + 5 sec + 20 sec + 25 sec +60 sec Top flap opens : Top flap closes : Bottom flap opens : Bottom flap closes : Recycle repeats. Bottom flap closed Bottom flap closed Top flap closed Top flap closed PUSH- PULL SLIDE DAMPER BUTTERFLY DAMPER - HANDLE v) b. (U Figure 12.21. Powder removal valves. (a) For intermittent discharge; (i) butterfly, (ii) manual push—pull, (iii) self-actuating flap valve, double flap valve (mechanically operated), (b) For continuous discharge; (iv) rotary valve. (By courtesy of Niro Atomizer.) AIR CYLINDERS ( DOUBLE-ACTING ) PISTON COUNTERWEIGHT mvAA OLVN EESTIC I ME R FLA MANHOLE FLAP ARM SELF-ACTING MECHANICALLY OPERATED COMPRESSED AIR a. Successful valve operation depends upon the flaps and gaskets remaining clean. As with the self-actuating valve any build-up on either flap will cause air leakage and reduce removal efficiency. However the mechanical opening and closing of each flap in the double flap design causes jolting and vibration to act on each flap thus dislodging potential product build-up on the flaps and sealing gaskets. Double flap valves are not ideal for heavy sticky products, but hygroscopic products are successfully handled when the product is in low humidity air. (iv) Rotary Valve. By far the most common discharge arrangement is the continuous product removal obtained with the rotary valve (figure 12.21(iv)). The valve consists of a 6-8 bladed rotor in dust-tight bearings and sealed shaft. The drive system is isolated from the valve interior eliminating any chance of oil or grease contaminating the powder. The rotary 'valve can be operated with many spray dried products, although there are severe limitations regarding those which are sticky and hygroscopic. Any product that tends to hang in the rotor sections and not fall quickly away will render 450 SURVEY OF AUXILIARY EQUIPMENT the valve inoperable, as a rotating lump of product will form. For products having a tendency to stick, however, an electric hammer mounted just above the valve will generally assist the operation. The clearance between the rotor and the valve body is often adjustable to suit the product in question. A larger clearance is required for coarse granular products than for fine grain products. Products having some sticking tendencies (e.g. those containing fat) require a sizeable clearance. The necessary clearance constitutes the main disadvantage of the rotary valve. Any clearance means a continuous air leakage through the valve if fitted to cyclones or other low pressure separators. As the degree of leakage depends upon the clearance, the wear of the rotor should regularly be inspected to check clearances are not too excessive. Apart from leakage of air via the clearance, a fixed volume of air (i.e. volume of each rotor section) enters every time the rotor section passes up under the separator base. For high humidity levels in a separator, entry of cold air can cause condensation on the metallic surfaces above the valve. Any moisture formation in this region leads to product build-up. An improved design of rotary valve that reduces air leakage to a minimum has been reported recently (358). A tapered rotor facilitates easy and precise adjustment of the clearance between rotor and housing to allow for wear, variations in temperature and variations in product. Easy accessibility for cleaning without need for special tools is a further important feature. (v) Pneumatic (Vortex) Air Lock. A continuous discharge technique for cyclones involving no mechanical operation is the pneumatic vortex air lock (figure 12.22(a)). It can only be associated with a pneumatic powder conveying. Air enters the lock tangentially and forms a vortex rotating in the same direction (although this is not essential) as the cyclone vortex. The vacuum (underpressure) in the middle of the vortex is the same as that in the bottom of the cyclone, consequently there is a continuous flow of powder from the cyclone into the air lock. Product passing to the cyclone base is taken up by the air lock vortex and conveyed away. The system operates on many spray dried products, and is only limited to the ability of the product to be pneumatically conveyed. Efficient operation of the air lock depends upon balancing the air rate through the system to give the required underpressure within the air lock. The air lock has a damper on the inlet side for adjustment of air rate when balancing the air lock. Balancing is straightforward in a one air lock—one cyclone (figure 12.22(bi)) and two air locks—two cyclones in parallel systems (figure 12.22(bii)). Balancing air locks in series is more difficult. The series layout shown in figure 12.22(biii) is difficult due to the differing pressure conditions at the base of the chamber and cyclone. The delicate balancing of the air lock for optimum efficiency constitutes the main disadvantage of the system. Should the air lock falter, excessive SURVEY OF AUXILIARY EQUIPMENT 451 CONVEYING AIR AND PRODUCT ia4p1 OUT FLANGE TO CYCLONE BASE CONVEYING AIR (a) IN. a. AIRBORNE PRODUCT FROM CHAMBER a+p a #p a+p if SINGLE (ii) IN PARALLEL ( Hi) IN SERIES Figure 12.22. Vortex air-lock. (a) Layout. (b) Arrangements. powder losses from the cyclones results. When an air lock falters, the reason is invariably concerned with the accompanying conveying system. The air lock is best controlled by maintaining the pressure drop level established at the time of balancing. A low pressure drop reading indicates a reduction in conveying air rate through the lock. Reduction is normally caused by a partially blocked conveying duct, or lumps of product falling from the cyclone and building-up in the centre of the air lock. Actual equipment in use for powder removal from cyclones is shown in figure 12.23. 12.4. Pneumatic Powder Conveying 12.4.1. Principles Pneumatic conveying is a common technique for transporting dried product within a spray dryer installation and is applied to : (a) Conveying powder from the base of the drying chamber and/or mechanical powder separators to a packing or storage area (figure 12.24(a)). (b) Conveying powder, usually fines, back into the drying chamber usually for agglomeration purposes (figure 12.24(b)). 452 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT 453 Figure 12.24(a) represents a low pressure system. The positioning of the conveying fan makes it a 'draw-through system'. Centrifugal fans are used. Air velocities in the ducts are fairly low (65-80 ft/sec, 20-25 m/sec). The air—product weight ratios are high. Large duct diameters are used. The draw-through system enjoys widespread use. The fan is mounted after the transport cyclone and runs on powder-free air minimizing fan cleaning and maintenance. Figure 12.24(b) represents a high pressure system. A blower is incorporated instead of a fan. The blower is usually of the rotary type (vane or cycloidal ■ A . a Figure 12.23. Powder removal from cyclones, equipment in practice. (a) Hopper with scraper. (b) Automatic double flap valves (air operated). (c) Rotary valve. (d) Vortex air lock. Figure 12.24, Pneumatic conveying layouts. A, low pressure (vacuum or draw-through) system. B, Positive pressure system. 454 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT (Rootes)). The conveying system is operated at an overpressure. Leakproof connections between the conveying duct and the drying chamber or recovery unit require special rotary valve designs. Ducts are small with standard pipe (2-3 in diameter) often forming the conveying system. To maintain adequate conveying conditions, high air velocities are used. The system is capable of operating on low air—product weight ratios, but this feature is not always utilized, unless further powder addition to the system supplements.the small quantities of fines normally produced during drying. The system is often called the `fines-return system'. The blower is placed before the powder inlet. Pneumatic conveying systems are highly flexible being able to transfer product anywhere in the dryer installation. Setting up a conveying system only requires having nearby structures for duct support and the possibility of making holes in walls, floors or ceilings for duct traverse. A conveying system involves little maintenance expense. Trouble-free operation is achieved, where required conveying velocities are maintained and where powder being conveyed has no tendency to stick to duct bends. Although the minimum conveying velocity is often thought to be the terminal velocity, this is never true in practice. This is because (a) Stokes law does not often apply due to many conveyed particles having sizes over 100 micron, (b) particles must be accelerated and not just suspended in the duct system, (c) the conveying velocity must overcome friction between particles and between particles and duct/pipe surfaces and (d) minimum conveying velocities differ for transfer in horizontal or vertical runs. Friction increases substantially with increase in product—air weight ratios. If powder is conveyed in quantities to give a product—air weight ratio of 6, friction losses can reach three times the losses created for air passing alone through the system. On the other hand, if the quantity of product conveyed is small, as in a low pressure system, and an air—product weight ratio of 4:1 prevails, friction losses barely exceed the losses incurred by clean air conveying. Friction losses can be calculated using the standard D'Arcy or Fanning formulae for duct/pipework given in all chemical and mechanical engineering textbooks. These formulae really apply to incompressible fluids, but they may be used for air when the total pressure drop is less than 1/10th of the initial absolute static pressure. Friction of product along the conveying duct/pipe wall surfaces is less for vertically than horizontally mounted duct/pipe runs, but the slip between individual particles is greater and is reflected in a greater static pressure requirement to create the necessary lift. In all cases the critical velocity for pneumatic conveying will exceed the terminal velocity by at least a factor of four. No general factor magnitude can be stated as this will depend upon each product conveyed. Minimum velocities for conveying are dependent upon product bulk density, particle 455 size and shape. For details on the theory of pneumatic conveying the reader is referred to Molyneux (190), Zenz and Othmer (191), Kraus (192), Coulson and Richardson (193) and Murty and Rey (194) or any chemical engineering textbook covering the unit operations. Pressure drop calculations for powder transport in straight ducts and bends have been recently described (1970) by Schuchart (195). Equations and an extensive reference list is given. 12.4.2. Pneumatic Conveying Systems in Practice Conveying velocities exceeding 65 ft/sec (20 m/sec) are recommended for most spray dried products. The conveying ducts are sized to give the recommended air—product weight ratio found in practice to prevent product WT RATIO _ POWDER;AIR POW RATE CONVEYING AIR VELOCITY 100 - 1 ' rrvsec) DUCT DIAMETER (cm } 50 - 2CONVEYI NG AIR RATE ( rrr/sec) 4- .1.0 10 . -01 5- 15 20 - -10 — 3050701- 100 - Figure 12.25. Determination of air rate and duct size for pneumatic conveying. Guide: Given powder rate (1), weight ratio (2), join to obtain conveying air rate (3). Given recommended velocity (4) and calculated air rate (3) join to obtain duct diameter (5). 456 SURVEY OF AUXILIARY EQUIPMENT deposition in the system. Estimation of duct size and air rate is given in figure 12.25, based upon data by Murty and Rey (194). A conveying duct system should not have a duct/pipe run larger than absolutely necessary. There must also be a minimum of 90° bends. Extended duct lengths and bends increase pressure drop losses, leading to greater power requirement to operate the system and extensive duct surfaces to maintain clean. Where bends are inevitable, these should be widely curved to reduce friction losses and the possibility of product build-up and duct blockage. A vertical bend with a horizontal approach is most prone to blockage if a product has the tendency to adhere to duct surfaces. A horizontal bend is also prone but not to the same degree. A vertical bend with a vertical approach in any system will be the region of least likelihood of blockaging. Velocity losses in conveying systems have been reviewed by Haag (196). It is always poor operational practice to hammer ductwork heavily in order to free a blockage. Invariably once a blockage has been discovered, it is in too advanced a state to be cleared by hammering the duct. Little effect is achieved and any resulting dents in the duct increase frictional effects and aggravate the deposit formation tendencies. A heavily dented duct (especially an upward vertical bend with a horizontal approach) can, for instance, give constant trouble. If a product has the tendency to deposit out at the bend or in a straight duct section reappraisal of the conditions is required, i.e. air rate, air temperature and humidity, powder temperature. If deposit formation persists in local areas even under the best possible conditions, special duct surface treatment should be applied to reduce the friction between powder and duct surface. 12.4.3. Operational Difficulties with Pneumatic Conveying Systems Problems arising in pneumatic conveying can usually be attributed to (a) insufficient conveying air, (b) powder too moist, (c) powder too warm, (d) air too humid, (e) duct cleanliness insufficient. Any one, or combination of these conditions can lead to a blocked pneumatic system. Re (a). Insufficient conveying air can arise from a dirty filter through which air is drawn into the conveying system. These filters are usually washable or can be cleaned by a vacuum cleaner. A dirty filter will register as a high pressure drop over the filter material. The pressure drop over the filter should always be checked as part of the daily operational routine. Re (b). Too moist a powder is heavy and tends to cake into lumps. Under these conditions the conveying velocity, stipulated for a free-flowing powder, is insufficient to convey away lumps. The lumps fall to the duct floor or lodge in duct bends. Once a lump causes an obstacle in the duct, build-up rapidly continues until duct/pipe blockage results. Moist powder can arise from deviations in drying air temperatures, atomization, drying air rate and SURVEY OF AUXILIARY EQUIPMENT 457 poor air dispersion in the chamber. These deviations are readily apparent on the dryer control instruments. Re (c). Too warm a powder has increased tendency to cake together and lump. This leads to conditions as mentioned in Re (b). Powder temperature control must be carried out frequently on products that have caking tendencies due to heat. Powder temperature is best measured during powder packing. The product temperature in the bag or other container remains constant during normal operation and any marked deviation can be readily detected. Powder leaving a spray drying chamber or recovery unit is warm, and often the pneumatic conveying system is used to cool the product while it is conveyed to the packing or storage area. This cooling is often necessary to prevent powder caking. To obtain optimum cooling conditions, the inlet conveying air temperature must be as low as possible. Normally conveying air is drawn from atmosphere within the dryer base vicinity. For indoor plants, the ambient temperature at the conveying air inlet often rises during the day, but these increases are normally small and do not effect the degree of product cooling to any marked extent. If the conveying air temperature does rise significantly over ambient conditions, the cause is often traced to excessive amounts of warm drying air passing from the drying chamber into the conveying system. This results from either (a) too high an overpressure in the drying chamber blowing warm air into the conveying system, (b) too low an underpressure in the conveying system drawing air from the drying chamber or (c) a dirty filter at the air intake. Conditions (a) and (b) are remedied through adjustment to the air flow dampers of the dryer system. Condition (c) is discussed under Re (a). Re (d). Conveying systems handling hygroscopic products require conveying air of low humidity. Any increase in humidity above that specified as permissible will result in the product taking up moisture from the air with eventual lumping and increased likelihood of deposit formation within the duct horizontal runs and bends. When operating a low humidity air conveying system, air conditions entering the system can be continuously monitored at the dryer unit control panel. Alternatively for periodic control, a wet and dry bulb thermometer can be used in the air duct leading to the powder entry point. Deviations in humidity must be rectified quickly as moist deposits formed in the duct and left for some time cannot be removed just by'return of acceptable air conditions. Failure in air conditions often requires plant shut-down followed by inspection and washing of the bends in the conveying duct system. Re (e). Incomplete washing of a duct system can lead to poor conveying performance. Should product remain as a deposit lump in a duct after washing, the lump will dry out and act as a nucleus for further rapid build-up 458 SURVEY OF AUXILIARY EQUIPMENT SURVEY OF AUXILIARY EQUIPMENT once the system is in operation again. Extra time spent on thorough cleaning is always repaid in longer periods of trouble-free operation. Pneumatic transport and its hazards have been recently reviewed by Smith (325). 459 The transfer pump can also supply product directly to the atomizer feed pump (figure 12.27(b)), The use of the transfer pump and an atomizer feed pump in series is common, where heavy pastes are involved. Preheating is necessary to assist feed flowability and enable continuous pumping performance when the height of the atomizer above the pump is large. 12.5. Pumps Pumps are required in the feed system to either transfer product within the feed system or supply product to the atomizer. These duties involve variable speed pump drives, throttling of pump discharge or recirculation of a proportion of the pump discharge. Various types of pumps are used due to the variety of feeds that are encountered. There is an applicable pump design for feeds that are in solution, slurry, suspension, melt or paste form. Pump selection is based not only upon the feed properties, but on the atomizer incorporated in the feed system. Where rotary atomizers or two fluid nozzles are used, low pressure pumps suffice. Where pressure nozzles are employed, high pressure pumps are required. A TO ATOMIZER PUMPS FOR SPRAY DRYERS CENTRIFUGAL POSITIVE DISPLACEMENT B ROTARY SCREW RECIPROCATING GEAR LOBE El PISTON TO ATOMIZER PLUNGER DIAPHRAGM Figure 12.26. Classification of pumps. 12.5.1. Pump Duties in Spray Dryers Pump duties are illustrated in the feed system layouts shown in figure 12.27. (a) Transfer Pump Duty This involves the transfer of feed from main feed tanks through preheating or pretreating equipment into a smaller atomizer feed tank. The atomizer feed tank supplies the atomizer feed pump. Transfer pump duties call for pump characteristics of constant head and constant discharge, or variable discharge with nearly constant head. High pumping rates are required if recirculation, is to maintain mixing in the main feed tanks. Much lower pumping rates are involved if level control in the atomizer feed tank brings the transfer pumping rate to equal the atomizer pumping rate (figure 12.27(a)). C TO ATOMIZER D Figure 12.27. Feed system layouts. A, Preheater and level controlled feed tank. B. Preheater and direct piping to atomizer. C. Direct feed system (variable speed pump or throttling valve). D. Constant head feed system to atomizer. 460 SURVEY OF AUXILIARY EQUIPMENT (b) Atomized Feed Pump Duty This involves one pump to supply the atomizer from the main feed tanks (figure 12.27(e)). Under steady state drying conditions, the required pump characteristics are of constant capacity at constant head. In practice, dryer control calls for slight variations in pump capacity at constant head. Pumping requirements to the atomizer are generally low when compared with pumping requirements in many chemical process industries. (c) Gravity Feed Tank Pump Duty This involves the pumping of feed to a constant head tank that supplies the atomizer (figure 12.27(d)). This calls for a constant head and constant capacity. Often high capacity pumping is required to assist feed mixing by creating a high overflow rate. 12.5.2. Pump Types and Uses The main classes of pumps for spray dryers are shown in figure 12.26. Rotary pumps of the screw type meet the requirements for the majority of installations. They are successfully used on such diversified products as milk, tomatoes, pharmaceuticals and clay slips. Gear pumps are used with heavy pastes. Diaphragm pumps are used with slurries containing large irregular insoluble solids. Centrifugal pumps are used with both solutions and slurries. High pressure dual or triple piston or plunger pumps are successful for pressure nozzle atomization arrangements. Details of these pumps are to be found in textbooks on the unit operations. Recent literature includes developments in screw pump performance and design by Polley (197) and analysis of likely pump breakdowns by Clements (198). Pumps for special conditions of low suction pressure are discussed by Pearsall and Scobie (199). Hattiangadi (200) reports on specifying centrifugal and reciprocating pumps. SURVEY OF AUXILIARY EQUIPMENT K 461 AR MAINS WATER A. MAINS WATER NOZZLES OR JETS 12.6. Washing Equipment Washing equipment for spray dryer installations include (a) equipment handled manually, (b) equipment continuous in operation (non-manual), (c) equipment for cleaning-in-place (CIP). The most common manual equipment in use is the spray water jet gun. Available designs operate on cold water, or utilise steam to form hot water. Hand operated spray guns are available from numerous nozzle manufacturers. With manual washing, thorough cleanliness can be obtained, but it does depend upon good accessibility to all plant items, and sufficient time within a production programme to enable operators to complete a thorough washing. Continuous operating equipment is often based upon tank-cleaning requirements. A common equipment is the rotating nozzle head. The ROOF LAY OUT B. CHAMBER LAYOUT Figure 12.28. Automatic washing equipment. (a) Rotating nozzles/jets. (b) Roof mounted nozzles/jets. 462 SURVEY OF AUXILIARY EQUIPMENT nozzle arrangement is lowered into the chamber or cyclone (figure 12.28(a)). Water is pumped to the rotating head (consists of 2 or 4 nozzles) at a high rate. The head acts as a water turbine. The nozzles rotate in the vertical plane while moving around the vertical axis. The water flow determines the nozzle rotation rate. Over a fixed time interval, every point on the chamber surface is impinged directly by a water jet. The wash water can be recirculated or passed directly to drain. For washing a co-current drying chamber (having rotary atomizer), the atomizer is first removed and the cleaning nozzle arrangement lowered into the chamber. This is convenient since the atomizer is withdrawn anyway to dismantle the wheel/disc and liquid distributor. The nozzle arrangement is normally located one-third the way down the chamber. A plate is fitted on to the supporting hose to prevent water being sprayed into the air disperser. The arrangement is ideal for cleaning large surface areas. It is unsuitable for cleaning items of li mited surface area (e.g. ductwork), or chambers with central air dispersers. CH' equipment involves the mounting of water nozzles at strategic positions in the dryer installation. The nozzles douse surfaces that have become coated with product during operation. The nozzle heads can be placed in position prior to the cleaning operation and removed for the drying operation, or can be a permanent fitting. CIP of a drying chamber is shown in figure 12.28(b). The use of CIP methods are becoming more and more popular in drying plant, especially those handling food products (201). Section V APPLICATIONS OF SPRAY DRYING IN INDUSTRY 13 Applications of Spray Drying (A Literature Survey) This chapter forms an updated version of a literature survey compiled by the author in 1968 (1). References up to and including April 1972 are now given. Products that have been spray dried on industrial or pilot plant scale are given in table 13.1. A comprehensive list of patents concerning spray dried products is given in table 13.2. Patents date from 1965 inclusive, although a few older patents are given where of special significance. Two decades of research and development have made spray drying a highly competitive means of drying, whether the situation is a delicate operation under sterile conditions or a high tonnage production of chemical products. The range of products suitable for spray drying continues to expand. Unit sizes and capacities have increased substantially through advancements in technical know-how and an appreciation of spray dryer mechanisms, especially in the atomization field. The chemical industry continues to broaden its range of application. The dairy industry shows increased plant capacity with the domestic demand for instant products and the wide-spread utilization of milk products as constituents of animal feedstuffs. The food industry remains an active field following the trend to food dehydration. The chemical industry already applies spray drying to a great extent. The spray drying of p.v.c. plastics is a typical example. Emulsion and suspension (e-p.v.c. and s-p.v.c.) are the two main types requiring drying. Spray drying is the only practical way for drying e-p.v.c. Particles are colloidal and the emulsion is fed to the dryer at 30-60 % solids. Either rotary or nozzle atomization is employed. Excessive inlet temperatures are not used due to the heat sensitivity of the product. The dried product consists of hollow globules from tiny cohesive particles. The degree of cohesion is regulated by the drying temperatures. s-p.v.c. consists of larger particles. Mechanical dewatering is possible in a centrifuge from which a 75-80 % solids having a very loose consistency 466 APPLICATIONS OF SPRAY DRYING IN INDUSTRY (p.v.c. snow) is obtained. Spray drying can then be conducted with a rotary atomizer of special design for non-liquid feeds. Such a method is of great interest to firms having large capacity e-p.v.c. spray drying, but require limited s-p.v.c. production. p.v.c. is discussed further in chapter 14 (14.1). The ceramic industry widely utilizes spray drying especially in the production of ceramic pressbody following the wet process, The advantages of direct transformation of the slip into an immediate pressable material are in this instance particularly attractive. The physical properties of spray dried material are ideal for pressing and firing operations, thus decreasing rejection percentage. The properties of materials spray dried for dry pressing have been reviewed by Storm (202). With the development of wear resistant atomizing devices either rotary or nozzles can be applied. Choice is dependent upon the most suitable particle size for the pressing operation. Wheel atomization has been used in large capacity units producing clays, ferrites, aluminium oxide, and wall-tile material. Nozzle atomization is widely applied to steatites, carbides and wall-tile material. Use of spray drying for ferrites has been reviewed (203) (204) (205) (206). Different types of spray dryers for ceramic products have been reviewed recently (1969) by Ries (207). Other recent publications on spray drying in the ceramic industry include Helsing (208) on oxide-ceramics, Lengersdorff (209) on ceramic jiggering bodies, and Storm (210) on electronic press bodies, and an alumina patent (211). Ceramics are discussed further in chapter 14 (14.2). For detergent manufacture, dryer design is dependent upon product type. Heavy-duty detergent units feature pressure nozzle atomization in tall and slender counter-current drying towers. Light-duty detergent units can be co-current designs. Special product handling prevents particle fracture. Solids content of the feed can be up to 65 % and the poWder is dried to 10-12 % moisture content. Inlet drying temperature range to 660°F (350°C). Silvis (212) and more recently (1970) Duckworth (213) report all aspects of detergent drying. Fundamentals have been given by Milwidsky (214) and Chaloud et al. (215). The adjustment of slurry formulations is reviewed in further articles (216). Improved preparation techniques of sodium tripolyphosphate for detergent slurries is based on a novel plant design featuring a combination of spray dryer and calciner (217). Further references to slurry preparation include improved dryer operation (218) and detergent processing (219). Moore (121) reports on the effect of drying variables on detergent powder characteristics. Detergents are discussed further in chapter 14 (14.3). In the field of agricultural pesticides, spray drying is applied to fungicides, insecticides and herbicides. Rotary atomization (atomizer wheels) is preferred as the resulting fine powder grain-size enables even dosage distribution. Ethylenebisdithiocarbamates of zinc and manganese, colloidal APPLICATIONS OF SPRAY DRYING 467 sulphur, copper oxychloride are examples of spray dried fungicides. In the production of herbicides, the sodium salts are usually spray dried. The sodium salt of di-chloropropionic acid requires strict outlet drying temperature control as product decomposition is likely if variations of only 10°F (6°C) occur. Automatic control and built-in water spray safety devices feature the plant design. Further examples of spray dried herbicides include the sodium salt of methyl chlorophenoxy-acetic acid and the series of products having similar chemical structures. Pesticides are discussed further in chapter 14 (14.4). Both dyestuffs and pigments are spray dried. There has been much recent interest in these products. Dryer designs use rotary atomization (atomizer wheels) as a fine grain size is normally required. Maximum inlet drying temperatures of 500°F (260°C) for organic dyestuffs are generally imposed. Inorganic pigments are dried at much higher temperatures. For coarser, non-dusty specifications, nozzle atomization is applied. Dyestuffs are often produced in small quantities, and the cleaning aspects of dryer design receive careful consideration. It is advantageous, however, to use one drying unit for one product. Dye-slurry drying with rotary atomizer has been reviewed (220). Kirady (221) reports experimental spray drying of pigment slurries with pressure nozzle atomization. The use of two-fluid nozzle atomization in the spray drying of aqueous acrylic polymer dispersion paints is claimed to advantage (222). Feed solids up to 45 % and low outlet drying air temperatures result in a 4 % moist Product bearing the exact proportions of solid resin, pigment and pigment extender. The use of high velocity air in two-fluid atomization applications is claimed to improve the final quality of aqueous dispersion paint composition (223). Kaolin clay was one of the first inorganic materials to be spray dried in vast tonnage for use as a white pigment in paints. Other important uses include paper, plastics, rubbers, pesticides and ceramics. Clarke (224), Fanselow (225), Agnello (226) and Freeport kaolin (227) report spray drying operations on kaolin. Titanium dioxide (228) is another white pigment extensively spray dried. Either rotary or nozzle atomization can be used. Product collection is by bag filters. Dyestuffs and pigments are discussed further in chapter 14 (14.5). The past few years have seen spray drying become established in the mining industry. Recent articles on spray drying of minerals (45) and spray drying in the mineral processing industry by Damgaard-Iversen (229) have described the developments that enabled spray drying to be accepted as a heavy industry operation. Kleeman (46) describes the spray drying of nickel concentrate ores in Australia. Spray drying of copper, molybdenum and nickel ores in U.S.A. has also been recently reported (47). Mining applications are discussed further in chapter 14 (14.7). 468 APPLICATIONS OF SPRAY DRYING IN INDUSTRY New applications in the chemical industry are reported for silicon carbide abrasive (230), carbon black (231), super-phosphate fertilizers (232) (233), phosphorous-phosphoric acids (234), toners (235) (236) and cement slurry (237) (238). The successful application (239) to spent sulphite liquors, a by-product of the pulp and paper industry, has enabled marketing of powder for uses including dispersing agents in insecticides, gypsum board manufacture, leather tanning, furnace clays, and animal feed and mineral ore pelletizing. The conversion of crills from the pulp into a useful product can be accomplished by spray drying the crills in aqueous suspension (240). Application in the cellulose industry is discussed further in chapter 17. Application of spray drying offers almost limitless possibilities for the food industry. Entwistle (241) and Patsavas (242) have reviewed spray drying from the food industry's viewpoint. Dairy products continue their rapid growth through the diversity of specialized purposes to which such powder can now be utilized. This has been accompanied by increased demand for more stringent milk powder specifications. Spray drying of milk was the subject of a symposium organised by the Australian Society of Dairy Technology (243) (244). The definition of stable powder forms most suitable for specific production applications is reported in further literature (245) (246) (247) together with the development of processing techniques for high tonnage production of premium grade powder of special physical characteristics. The structure of milk powders and new forms of marketed powder are reviewed elsewhere (248). Instant powder forms the basis of a further review (246). For recent developments in spray dryer design for milk the reader is referred to (249)(250) (506) (518). Recent developments (1970) in the agglomeration of milk powder to instant products have been reported by Bergmann (251). Some recent patent claims for instant powder production include agglomeration during nozzle atomization (252) (253), lecithin dosage (254) (255) (256) (257) (258) and use of binding agents (259). The other main by-prodncts of the dairy industry, apart from the skim milk is whey formed from cheese making and from the manufacture of casein. Spray dried whey powder is now utilized as a fodder additive and as a constituent in the confectionery industry. Three spray drying processes for producing ordinary and non-caking whey are discussed by Galsmar and Bergmann (260). Two methods are reported for fresh whey, which includes virtually all types of cheese-whey where further bacterial acidification has been stopped by cooling. One method is reported for acid whey (pH less than 4.6). Weber (261) reviews methods of whey utilization. Protein from whey using spray drying has been reported elsewhere (262) (498). Special techniques for the spray drying of other dairy products include drying of fat-containing milk products (263) (264), ice-cream mix (265), APPLICATIONS OF SPRAY DRYING 469 sour cream (266), cheese (267), dietetic products (268), casein (269) and buttermilk (270). Dairy products are discussed further in chapter 15 (15.1). The role of spray drying in the coffee industry is given by Sivetz (271). Recent literature is limited, as at present more attention is being paid to freeze drying techniques. However, improved continuous extraction techniques are yielding improved quality extracts for either spray or freeze drying. Improved flavour and aroma retention is claimed with a spray drying process which includes coffee fines stabilization through encapsulation of the fines with extract (272). Beverages are discussed further in chapter 15 (15.2). Flavour retention in spray drying preconcentrated liquid foods, e.g. coffee, tea, milk, fruit juices, is discussed by Thijssen (477). Spray drying is applied in the food processing industry. The production of tomato powder from concentrated pastes is growing with drying facilities in Europe, U.S.A. and North Africa. The techniques of tomato spray drying have been reported (273) (274). Descriptions of industrial installations are available (275) (276) (277) (278). Adoption of spray drying to citrus fruit (279) has enabled improvements in the quality of fruit powders reports Urbanek (280). The mechanism of spray drying is suited for such heat sensitive products, and the use of a carrier gum and inert gas packing aids flavour retention and product handling of the hygroscopic powder. The production of soluble citrus fruit powder free from preservatives using spray drying techniques results in retention of natural fruit flavours (281). A successful application to raspberries is also evident (282). The spray drying of tomatoes, apple, banana and vegetables, where skim milk is used as a carrier is reported by Breene and Coulter (283). For flavouring materials, an imitation brown sugar processed by spray drying has been marketed (284). There is news of a production of a low caloried sweetener based on dextrin and at least one noncaloric sweetening agent (285). Pressure nozzle atomization is employed with up to 65 % feed solids. The dried powder contains 6-10 % moisture. An experimental investigation into the spray drying of flavouring materials is reported by Brooks (286). Measurements were made on the loss of ethyl-caprylate dispersed in aqueous gum arabic. Details on spray drying in the flavouring industry is reported elsewhere (287). A process for the preparation of dry flavouring materials from crustaceans for human consumption is reported by Gray (288) to utilize a spray drying stage. Dry free-flowing glucose production from starch conversion also includes a spray dryer (289) (290). The dryer features a special fines return system, whereby powder is returned to the atomization zone. Spray drying of molasses for animal fodder is described (291) (517). Feed contains 3-8 % kaolin, and is atomized by a rotating disc into a chamber having air swept walls. The development of spray drying to potato processing has resulted in three patents (292) (293) (294). A pneumatic paste nozzle is 470 APPLICATIONS OF SPRAY DRYING APPLICATIONS OF SPRAY DRYING IN INDUSTRY featured for atomizing the mashed potato, and the process is claimed to prevent the breakage of potato cells, which results in the formation of a glutinous mass on reconstitution. A 9-inch bowl atomizer in a co-current flow drying tower features the patent coverage (292) (293) where powder at 5-6 % moisture (bulk density 0.5-0.6 g/cm 3 ) yields prime mashed potato flavour on reconstitution with water/milk. The bowl design and operating conditions prevent excessive shearing effects that cause cell rupture. The spray drying of starch (both pregelatinized and coldsetting starch) is reported (295). High pressure nozzle atomization is used in the production of pastry mixes (296). The production of high protein food additives from soyabean, plant extract (297) (298) is growing in importance. Drying of liquorice extract has been recently reported (519). The modification of basic spray designs to meet sterile processing conditions is reported (299). The use of one and two stage units are described to deal with the low feed solid contents usually dried. Blood serum application is referred as an example. A laboratory dryer design for biological materials is described by Freeman (300). A thesis on spray drying enzyme rennet has been presented by Shah (301). Amylase drying appears elsewhere (302). Processing of cellulose to produce protein using micro-organisms, involving spray drying is reported recently (303). Application in the biological industries are discussed further in chapter 16. By utilizing spray drying for processing abattoir products, a hitherto considered waste can be converted into highly profitable commodities. Abattoir by-products include blood, hair, glands, tissue and organs. Bergsoe and Fakstorp (304) describe the production of dehydrated glands and tissues, and layout the flow sheets for blood processing to ordinary and soluble blood powder, blood cell powder and blood albumin. The production of high protein foodstuffs by spray drying of meat extracts and hydrolysate is noted. Gelatine drying in spray dryers is also practised (305). In the following chapters 14-18, many of the above mentioned products are considered in more detail. Chapter 14 deals with the important applications in the chemical industry, i.e. plastics, ceramics, detergents, pesticides, dyestuffs, fertilizers, mineral ore and sundry organic and inorganic chemicals. Chapter 15 is devoted to applications in the food industry with special emphasis given to milk products, eggs, extracts, fruit and vegetables and some carbohydrates. Chapter .16 describes the spray drying of pharmaceuticals and yeast in the biochemical industry. The tannin and cellulose industries are briefly mentioned in chapter 17. The chapters on various applications are completed with descriptions of spray drying in the offal and fish industries (chapter 18). 471 Table 13.1, Products Suitable for Suspended Particle Processing Systems, involving Atomization. (Spray Drying, Spray Cooling, Spray Reaction, Spray Purification.) 14. Chemical industry 14.1. Plastics, resins AB and ABS latex Melamine formaldehyde resin Phenol formaldehyde tesin Polyacrylate-emulsion-type Polyacrylonitrile Polyethylene Polyvinyl acetate Polyvinyl butyrate Polyvinyl chloride emulsion-type Polyvinyl chloride suspension-type Polyvinyl pyrrolidone Polyvinyl toluene Rubber latex SBR latex Urea formaldehyde resin 14.2. Ceramic materials Aluminium oxide Beryllium oxide Carbides Carborundum Electro-porcelain Enamels Floor tile material Ferrite Glass powder Insulator material Iron oxide Kaolin Silicium oxide Spark plug material Steatite Titanates Tungsten carbide Uranium oxide Wall tile material Zirconium silicate 14.3. Detergents and Surface active agents Alkyl-aryl sulphonates Detergent enzymes Dispersing agents Emulsifying agents Fatty alcohol sulphate Heavy-duty detergents Light-duty detergents. Mono- and dipotassium orthophosphate Mono- and disodium orthophosphate Nitrilo tn-acetic acid salts Optical brightener Phosphates Saponine Soap Tetra potassium polyphosphate 14.4. Pesticides Calcium arsenate Copper oxychloride Cuprous oxide 2,4 DBA sodium salt 2,4,6 TBA sodium salt DDT with filler 2,4 dichloro-phenoxyacetic acid 2,4 dichloro-phenoxypropionic acid mono-methylamine salt Dichloro-phenoxypropionic acid Dichloro-propionic acid sodium salt Diemthyl-dipyridyl dichloride Lead arsenate Mangano-ethylene-bis-dithiocarbamate Methyl-chloro-phenoxyacetic acid Methyl-chloro-phenoxypropionie acid Methyl-chloro-phenoxybutyric acid sodium salt Sodium aluminium fluoride Sodium fluoride Sodium methyl arsenate Sodium penta-chlorophenolate Sulphur colloidal Zinc-ethylene-bis-dithiocarbamate Zinc diethyl dithiocarbamate Zinc dimethyl dithiocarbamate 14.5. Dyestuffs, pigments Basic dyes Ceramic colours Chrome-yellow Copper oxide Cosmetic colours Dyestuff intermediates Formulated dyestuffs Food colours Indigo dye Ink pigments 472 APPLICATIONS OF SPRAY DRYING APPLICATIONS OF SPRAY DRYING IN INDUSTRY Table 13.1—continued Inorganic pigments Iron oxide Kaolin Lithopone Milori blue Organic pigments Paint pigments Paper colours Phthalocycanines Plastic pigments Soluble and microdisperse textile dyes Titanium dioxide Water colours Zinc chromate Zinc potassium chromate Zinc tetroxychromate 14.6. Fertilizers Nitrogen fertilizers Ammonium salts Urea Phosphoric acid fertilizers Superphosphates Potash fertilizers Two component fertilizers (N–P, P–K) Three component fertilizers (N–P–K) 14.7. Mineral flotation concentrates Copper ore Cryolite Iron ore Lead ore Manganese ore Molybdenum ore Nickel ore Silver ore Tungsten ore 14.8. Inorganic chemicals Abrasive grits Aluminium (metallic) Aluminium chloride Aluminium hydroxide Aluminium oxide Aluminium phosphate Aluminium silicate Aluminium sulphate Ammonium chloride Ammonium molybdate Ammonium nitrate Ammonium phosphate Ammonium sulphate Antimony sulphide Arsenic oxide Barium carbonate Barium chloride Barium hydroxide Barium sulphate Barium titanate Bauxite waste liquor Bentonite Beryllium dioxide Bismuth aluminate Bismuth carbonate Borax Boric acid Boron phosphate Calcium carbonate Calcium chloride Calcium hydroxide Calcium chromate Calcium hypochlorite Calcium nitrate Calcium phosphates Calcium silicates Calcium sulphate Catalysts Cement Chrome-iron oxide Chromium sulphate Copper chloride Copper oxide Copper oxychloride Copper sulphate Copper sulphide Cupric oxide Cryolite Feldspar Ferric sulphate Ferrous sulphate Graphite Gypsum Kaolin Lead zirconate Lithopone 473 Table 13.1—continued Lithium chloride Magnesium aluminium silicate Magnesium carbonate Magnesium chloride Magnesium hydroxide Magnesium phosphates Magnesium sulphate Magnesium trisilicate Magnesium uranate Manganese carbonate Manganese chloride Manganese oxide Manganese sulphate Molybdenum disulphide Nickel carbonate Nickel chloride Nickel sulphide Potassium acetate Potassium carbonate Potassium bicarbonate Potassium bichromate Potassium carbonate Potassium chlorite Potassium chromate Potassium metaphosphate Potassium nitrate Potassium permanganate Potassium phosphate Potassium silicate Powdered metals Silicon dioxide Silicon carbide Sodium aluminate Sodium aluminium sulphate Sodium arsenate Sodium bicarbonate Sodium bichromate Sodium bisulphate and sodium sulphate Sodium bisulphide Sodium borate Sodium carbonate Sodium chloride Sodium hypochlorite Sodium fluoride Sodium formate Sodium hydroxide Sodium perborate Sodium phosphate Sodium silicate Sodium silicon fluoride Sodium sulphate Sodium thiosulphate Thorium carbonate Thorium nitrate Titanium dioxide Titanium tetrachloride Tungsten carbide Uranium dioxide Zinc arsenate Zinc carbonate Zinc chloride Zinc sulphate Zirconates 14.9. Organic chemicals Aluminium stearate Aluminium triformate Amino-naphthol-sulphonic acid para-Aminosalicylic acid Amino acid Ascorbic acid Ammonium-di-nitro-ortho cresol Barbituric acid derivate Barium ricinoleate Calcium acetate Calcium butyrate Calcium gluconate Calcium caseinate Calcium lactate Calcium proprionate Calcium saccharates Calcium stearate Carboxymethyl cellulose Chloramine Chlorohexidine gluconate Chloromycetine succinate—calcium salt Chlorophyll Choline salts Citric acid Dicyandiamide Dicyclohexylphthalate Diethyldiphenylurea 2,4 dichlorophenoxy-acetic acid sodium salt Dodecylbenzenesulphonate sodium salt Glutamic acid 474 APPLICATIONS OF SPRAY DRYING IN INDUSTRY Table 13.1—continued Glyoxal Lactose Lysine Maleic acid Methyl acrylic acid Methyl arsenic acid–disodium sulphate Mono-carbonic acid Mono-ethanol aminosulphate Monochloroacetic acid sodium salt Oxalic acid para-nitro phenol Pantholtenates Perfumes Potassium acetaldehyde sulphoxylate Potassium acetate Potassium isopropylxanthogenate Potassium phthalate Potassium sorbate Quinoline sulphonate Sodium acetate Sodium benzene sulphonate Sodium benzoate Sodium di-oxalate Sodium dimethyl dithiocarbamate Sodium monochloroacetate Sodium salicylate Stearic acid Tartaric acid Thiocarbamates Thionine Urea Waxes Xanthates Zinc stearate 15. Food industry 15.1. Milk products and eggs Baby food Butter (high fat products) Buttermilk Casein Caseinates Cheese Cocoamilk with sugar Coffee whitener Cream Egg—Egg white Egg yolk Whole egg Ice cream mix Malted milk Milk replacer Mixed milk products Skim milk Whey Whey mother liquor Whole milk 15.2. Food products and plant extracts Artichoke extracts Beef broth Bouillon Cake mixes Camomile tea Cereals, pre-cooked Chicken broth Chlorophyll Cocoa mixtures Coffee-extracts Coffee-substitute extract Decaffeinated coffee extract Fat flour mixtures Fish proteins Flavourings Food colouring Garlic Hip-extract Lactose Liquorice extract Malt extract Meat puree Milk coffee mixture Pimento Plant protein Proteinhydrolysate Rennet Soup mixes Tea extract Whiteners (coffee/tea) 15.3. Fruit, vegetables Apricots Asparagus Banana APPLICATIONS OF SPRAY DRYING Table 13.1—continued Beans Beetroot Carrot Citrus fruits Mangoes Onion Peaches Soft fruits Tomato 15.4. Carbohydrates and similar products Baking compounds Corn steep liquor Corn syrup Glucose Gum arabic Maize gluten Pectin Sorbitol sorbose Starches Sugar/gelatin mixtures Total sugar Wheatflour Wheat gluten 16. Biochemical industry 16.1. Pharmaceutical products Antibiotics and moulds Bacitracin Penicillin Streptomycin Sulphatiazole Terramycin Tetracyclin Dextran Enzymes Hormones Lysine (Amino acids) Pharmaceutical gums Sera Spores Tabletting constituents Vaccines 16.2. Yeast products Brewers yeast Fodder yeast Yeast extracts Yeast hydrolysates 17. Industries utilizing chemicals from timber 17.1. Tannins Tannins from bark Mangrove extract Mimosa extract Oak extract Pine and fir extract Tannins from wood Quebracho extract Chestnut extract Tannins from fruits Dividivi extract Myrobalan extract Tannins (synthetic) 17.2. Cellulose Sulphite waste liquor Lignosulphonates 18. Offal and fish industries 18.1. Slaughterhouse products Animal protein Blood Bone glue Excreta Gelatin Glands Tissues 18.2. Fish products Fish flour Fish hydrolysates Fish meal Fish pulp Fish stickwater (solubles) Whale stickwater (solubles) 475 (Dates given for both patent specifications and applications are the dates of publication. If equivalents in various countries have been published preference has been given to US. or British, if possible.) Product group M. (See table 13.1) Product 14 Chemical industry 14.1 p.v.c. Plastics, Resins Rubber lactices Acrylic paint Chlorinated polyisoprene Epoxy polyamide a.o. Organopolysiloxanes. p.v.ac. paint p.v.ac. Polyethylene Polyethylene Various Patent or application no. Brit. pat. 952 628 U.S. pat. 3 194 781 U.S. pat. 3 325 425 German pat. appl. 2 003 528 Brit. pat. 1 138 180 U.S. pat. 3 383 773 U.S. pat. 3 287 290 Danish pat 106 467 Brit. pat. 1 033 657 Japanese pat. appl. 70.05146 Danish pat. 107 901 Patentee and/or inventor(s) Date Farbwerke Hoechst Aktiengesellschaft March 18, 1964 Du Pont de Nemours and Company, Hedberg, J. G., O'Donnell, H. B., Peet, G. W. Monsanto Company, Bray, W. J. July 13, 1965 June 13, 1967 Imperial Chemical Industries Ltd., Felstead, E. Sept 17, 1970 Yarsley Research Laboratories-Ltd., Lanham, B. J., 'Tyke', V. C. Dec. 27, 1968 Owens Illinois, Inc., Nugent, D. C. May 21, 1968 Monsanto Company, Bray, W. J. Nov. 22, 1966 Edison Societa per Azioni May 8, 1967 Eastman Kodak Company, Wright, J. F., Shahan, N. D. June 22, 1966 Sakamoto, N. Feb. 20, 1970 Rohm & Haas Company July 17, 1967 -11.• a. Alusn,amNI ONIAlltaAvuds30 SNOLINDrIcicni Table 13.2. Recent Patents and Patent Applications dealing with Products to which Spray Drying or Spray Cooling is Applied Table 13.2—continued 14.2 Ceramic materials 14.3 Detergents and surface active agents Product Patent or application no. Patentee and/or inventor (s) Date Oxide ceramics Plastic bodies Calcium zirconate a.o. Cellular clay material Brit. pat. 1 081 730 German pat. appl. 1 268 551 French pat. 1 452 220 General Motors Corporation, Fenerty, M. J., Somers, A. V. Rheinisch-Westfdlische Isolatoren-Werke GmbH., Draeger, K. Societe de Fabrication d'elements Catalytiques Aug. 31, 1967 French pat. 1 537 564 Synfibrit GmbH Aug. 23, 1968 Detergents U.S. pat. 3 357 476 U.S. pat. 3 369 304 U.S. pat. 3 380 922 Brit. pat. 1 159 643 Brit. pat. 1 189 543 Brit. pat. 1 208 372 German pat. appl. 1 961 450 Colgate-Palmolive Company, Toffiemire, R. H. Dec. 12, 1967 Monsanto Company, Clark, S. G., Feierstein, H. E. Feb. 20, 1968 Purex Corporation, Ltd., Shields, G. G., Patterson, C. B. Mo och Domsjo AB Apr. 30, 1968 July 30, 1969 Colgate-Palmolive Company Apr. 29, 1970 Colgate-Palmolive Company Oct. 14, 1970 Unilever, N. V., Bauer, H. E. July 2, 1970 Detergents Detergents Detergents Detergents Detergents Detergents May 16, 1968 Sept. 9, 1966 ONIAIICI AV MS JO SNOLLVDMIcIY Product group no. (See table 13.1) Table 13.2—continued –4 cc Product Detergents Detergents Detergents Detergents Detergents Detergents Optical brighteners. Emulsifier 14.4 Pesticides 14.5 Dyestuffs and pigments General Dyestuffs Dyestuffs Patent or application no. Patentee and/or inventor(s) Date Henkel & Cie GmbH Nov. 5, 1970 Witco Chemical Company, Inc., Mausner, M. L., Rainier, E. T. Colgate–Palmolive Company Nov. 10, 1967 Feb. 27, 1970 Colgate–Palmolive Company May 22, 1970 Unilever, N. V, Kerkhoven, F. J., Troost, S. Sept 22, 1968 Colgate-Palmolive Company, Reinish, M. D. Oct. 26, 1968 Farbenfabriken Bayer Aktiengesellschaft, Kleinheidt, E. A., Meier, E., Scholermann, W., Schonol, K. Aktieselskabet Grindstedvxrket, Jensen, K. S., Andreasen, J. Dec. 10, 1969 Dutch pat. appl. 70 01446 German pat. appl. 1 812 574 Farbwerke Hoechst A.G. Aug. 7, 1970 Riedel-de Haen A.G. June 11, 1970 British pat appl. 1 233 479 Brit pat 1 064.924 Brit. pat 1 069 380 Farbenfabriken Bayer Aktiengesellschaft, Mols, H., Hornle, R., Raab, H. Farbenfabriken Bayer Aktiengesellschaft, Breig, K., Blum, W., Muller, G., Steinmetz, G. Farbenfabriken Bayer Aktiengesellschaft, Breig, K., Blum, W., Miiller, G., Raab, H. May 26, 1971 German pat. appl. 1 922 451 French pat. 1 501 615 French pat. appl. 2 011 190 French pat. 1 590 487 Dutch pat. appl. 67 04145 Danish pat appl. 1807/68 Brit. pat. 1 173 806 Danish pat. appl. 112 247 APPLICATIONS OF SPRAY DRYING IN INDUSTRY Product group no. (See table 13.1) Nov. 25, 1968 Apr. 12, 1967 May 17, 1967 Table 13.2—continued Product group no. (See table 13.1) Product Patent • or application no. Dyestuffs Belgian pat. 677 910 Carbon U.S. pat black 3 433 660 Electrostato- U.S. pat. graphic toner 3 326 848 Electrostato- U.S. pat. graphic toner 3 338 991 Kaolin U.S. pat. clay 3 372 043 Opacifiers German pat. appl. 2 019 765 Zn yellow Polish pat. a.o. 58 625 14.6 Fertilizers General (prilling) General (prilling) General (prilling) General (prilling) General (prilling) U.S. pat. 3 334 160 Brit. pat. 1 209 454 Brit. pat. 1 209 886 German pat. 1 227 429 German pat. 1 228 231 Patentee and/or inventor(s) Date Farbenfabriken Bayer Aktiengesellschaft, Breig, K., Blum, W., Muller, G., Raab, H., Steinmetz, G. Cabot Corporation, Jordan, M. E., Hardy, J. F. May 31, 1966 Xerox Corporation, Clemens, C. F., Lenhard, M. J. June 20, 1967 Xerox Corporation, Insalaco, M. A., Clemens, C. F., Lenhard, M. J. Engelhard Minerals & Chemicals Corporation, Fanselow, J. R. The Champion Paper Company, Ltd., Vassiliades, A. E., Nauman, E. F., Shroff, S. Instytut Cheminieorganicznej, Bednarczyk, K., Chejduga, A., Bandrowska, C. Aug. 29, 1967 March 18, 1969 March 5, 1968 Nov. 12, 1970 Nov. 5, 1969 2 Gulf Oil Corporation, Wisneski, P. M., Mosier, C. F. Aug. 1, 1967 Fisons Fertilizers Limited, Bradley, J. K., Sherwin, K.A. Oct. 21, 1970 ( Fosfatbolaget AB Oct. 21, 1970 Pzt Badische Anilin- & Soda-Fabrik Aktiengesellschaft, Zapp, K. H. Badische Anilin- & Soda-Fabrik Aktiengesellschaft, Jockers, K., Gettert, H. Oct. 27, 1966 Nov. 10, 1966 0, ,. Product group no. (See table 13.1) Product Patent or application no. General German pat. appl. (prilling) 1 263 707 General French pat. (prilling) 1 589 598 Ammonium U.S. pat. nitrate 3 533 776 Ammonium German pat. appl. nitrate 1 964 614 Ammonium U.S. pat. phosphate 3 214 260 Ammonium Danish pat. appl. phosphate 113 926 Mixed U.S. pat. fertilizers 3 539 326 Mixed Brit. pat. fertilizers 1 104 253 Mixed French pat. fertilizers 1 519 801 Mixed Dutch pat. appl. fertilizers 69.06224 Calcium German pat. appl. ammonium 1 907 361 nitrate Urea German pat. appl. 1 246 681 Patentee and/or inventor(s) Date Potasse & Engrais Chimiques, Quanquin, B., Le Clerc, G. M., Pierre, J.-L. Norsk Hydro-Elektrisk Kvelstofaktieselskab, Friestad, I. A. Fisons Fertilizers Limited, Coates, R. V., Curtis, M. F., Harris, G. J., Smith, P. S. Dzerzhinsky Filial Nauchno-Issledovatelskogo I Konstruktorskogo Instituta Khimicheskogo Mashinostroenia, Vagin, A. A. Nissan Chemical Industries, 0i, Y., Kusanagi, S., Arata, M. Norsk Hydro-Elektrisk Kvxlstofaktieselskab, Friestad, I. A., Skauli, 0. Mitsui Toatsu Chemicals Incorporated, Otsuka, E., Takada, M., Matsuo, K., Murozono, H., Nagayama, T. Fisons Fertilizers Limited, Chapman, J. D., Dee, G. T., Janikowski, S. M., Peters, R. H. Ugine Kuhlmann, Gittenait, M. March 21, 1968 March 31, 1970 Oct. 13, 1970 Oct. 8, 1970 Oct. 26, 1965 May 12, 1969 Nov. 10, 1970 Feb. 21, 1968 AWISCIUNI NI 9NIIAII0 A.V1MS AO SNOIIVOlicicIV Table 13.2—continued April 5, 1968 Stamicarbon N. V. Oct. 27, 1970 Ruhrchemie AG, Weitendorf, K. F., Traenckner, K. C. Aug. 27, 1970 The Lummus Company, Summerville, R. N. Aug. 10, 1967 Table 13.2—continued Product Urea 14.7 Minerals— ore flotation concentrates 14.8 Inorganic chemicals Catalysts Catalysts Catalysts Catalysts Catalysts Cement Cement Cement Lead powder Sodium carbonate Patent or application no. Patentee and/or inventor(s) Date French pat. 1 475 268 The Chemical and Industrial Corp. March 31, 1967 Swedish pat. appl. 325 242 A/S Niro Atomizer, Damgaard-Iversen, J. June 29, 1970 U.S. pat. 3 347 798 U.S. pat. 3 433 587 Belgian pat. 741 001 Danish pat. 107 416 Danish pat. 113 217 German pat. appl. 2 048 178 German pat. appl. 2 044 457 Danish pat. 108 487 Danish pat. appl. 115 422 U.S. pat. 3 202 477 Badische Anilin- & Soda-Fabrik A.G., Baer, K., Sperber, H., Goehre, 0., Leibner, G. Engelhard Minerals & Chemicals Corporation, Haden, W. L., Dzierzanowski, F. J. Nitto Chemical Industry Limited, Nakamura, Y., Saito, S., Sasaki, Y. The Standard Oil Company Oct. 17, 1967 March 18, 1969 Apr_ 1, 1970 Sept. 25, 1967 National Lead Company, Granquist, W. T. March 3, 1969 A/S Niro Atomizer, Damgaard-Iversen, J., Kruse, F. Apr. 15, 1971 A/S Niro Atomizer, Gude, K. E., Lund, B. March 11, 1971 Dyckerhoff Zernentwerke A.G. March 28, 1967 Associated Lead Manufacturers Limited, Kinsell, D. Oct. 6, 1969 Diamond Alkali Company, Loeffler, J. E. jr., Springer, R. A., Bolick, E. L. Aug. 24, 1965 ONIAIICI AVIIcIS JO SINIOLINDI1c1c1V Product group no. (See table 13.1) Table 13.2—continued Product Iron sulphate Alkali metal perborate Alkali metal perborate Aluminium oxide Aluminium oxide Aluminosilicate Aluminosilicate Calcium chloride Calcium chloride Metal oxides Metallurgical powders Nickel and Cobalt sulphate Patent or application no. U.S. pat. 3 195 981 U.S. pat. 3 510 269 Dutch pat. appl. 69.10222 U.S. pat. 3 411 878 Swedish pat. appl. 313 553 U.S. pat. 3 472 617 Japanese pat. appl. 70.19167 U.S. pat. 3 339 618 U.S. pat. 3 196 930 U.S. pat. 3 273 962 Brit. pat. 1 110 386 Belgian pat. 734 953 Patentee and/or inventor(s) Date British Titan Products Company Limited, Hansford, K. R., Roberts, A. L., Evans, A. W. Deutsche Gold- und Silber-Scheideanstalt, Bittner, F., Simmerback, E., Dahm, F. L., Schaller, A. Dec. 10, 1962 May 5, 1970 Deutsche Gold- und Silber-Scheideanstalt Feb. 17, 1970 Produits Chimiques Pechiney-Saint-Gobain, Graulier, M., Michel, M. Universal Oil Products Company, Moehl, R. W. Nov. 19, 1968 W. R. Grace & Co., McDaniel, C. V., Maher, P. K., Pilato, J. M. Universal Oil Products Co. July 1, 1968 Oct. 14, 1969 July 1, 1970 Wyandotte Chemicals Corporation, Bowden, J. H., Terry, C. T. Knapsack-Griesheim Aktiengesellschaft, Ebert, H., Giesswein, K., Harmsen, E., Vomberg, H. Monsanto Company, Walsh, R. J. Sept. 5, 1967 Cabot Corporation Apr. 18, 1968 A/S Niro Atomizer, Nielsen, K., Nielsen, H. B. Aug. 29, 1969 APPLICATIONS OF SPRAY DRYING IN INDUSTRY Product group no. (See table 13.1) July 27, 1965 Sept. 20, 1966 Table 13.2—continued Product group no. (See table 13.1) Product Brit. pat. 1 189 656 U.S. pat. 3 383 172 French pat. 1 431 784 U.S. pat. 3 538 200 U.S. pat. 3 338 671 U.S. pat. 3 385 661 U.S. pat. 3 387 924 U.S. pat. 3 499 476 Brit. pat. 1 026 675 Brit. pat. 1 158 178 German pat. 2 011 336 Patentee and/or inventor(s) Date Fisons Fertilizers Limited, Smith, P. S. Apr. 29, 1970 Deutsche Gold- und Silber-Scheideanstalt, Biegler, H., Kallrath, G. Produits Chimiques Pechiney-Saint-Gobain, Golovtchenko, M. V. Shell Oil Co., Hite, J. R. May 14, 1968 Feb. 7, 1966 FMC Corporation, Marschall, H. L., Coykendall, J. W. Aug. 29, 1967 Central Glass Co., Hayakawa, M., Yasutake, Y. May 28, 1968 Knapsack Aktiengesellschaft, Hartlapp, G., Heymer, G., Traulsen, K. Knapsack Aktiengesellschaft, Hartlapp, G., Klee, H., Koch, J. Buttner-Werke Aktiengesellschaft June 11, 1968 Apr. 20, 1966 Albright & Wilson (Australia) Limited July 16, 1969 FMC Corporation, Herink, J. F. Oct. 1, 1970 Nov. 3, 1970 March 10, 1970 APPLICATIONS OF SPRAY DRYING Potassium chloride Silicon dioxide Sodium bisulphate Sulphur molten (prilling) Tripolyphosphate Tripolyphosphate Tripolyphosphate Tripolyphosphate Tripolyphosphate Tripolyphosphate Tripolyphosphate Patent or application no. Table 13.2—continued 14.9 Organic chemicals Product Borate sequestering agent Diphenylolpropane Fumaric acid a.o. Urea, sodium glutamate a.o. 15 Food Industry 15.1 Milk products and eggs 15.1.1 General Milk products General General General General Patent or application no. 00 Patentee and/or inventor(s) . Date U.S. pat. appl. 3 539 463 W. R. Grace & Co. Nov. 10, 1970 Dutch pat. appl. 66.16683 Japanese pat. appl. 70.32217 Japanese pat. appl. 70.22926 Stamicarbon N.V. May 27, 1968 Ueno Seiyaku KK. Oct. 17, 1970 Nippon Shiryo Kogyo KK. Aug. 3, 1970 U.S.A. (Secretary of Agriculture), Hanrahan, F. P., Bell, R. W., Webb, B. H. Foremost Dairies, Inc., Hutton, J. T., Nava, L. J., Shields, J. B., Kempf, C. A. Koopmans Meelfabrieken N.V., Giddey, C. May 25, 1965 Jan. 25, 1966 Industrie-Werke Karlsruhe AG Sept. 28, 1966 Dr. Max E. Schulz Nov. 10, 1966 U.S. pat. 3 185 580 U.S. pat. 3 231 386 Brit. pat. 992 758 Brit. pat. 1 044 268 German pat. 1 228 567.. APPLICATIONS OF SPRAY DRYING IN INDUSTRY Product group no. (See table 13.1) May 19, 1965 Table 13.2—continued Product group no. (See table 13.1) Product General General Skim milk Whole milk Whole milk Whole milk Whole milk Whole milk Whey Whey Whey Whey German pat. appl. 1 262 114 Japanese pat. appl. 70.32223 U.S. pat. 3 410 701 U.S. pat. 3 164 473 U.S. pat. 3 278 310 U.S. pat. 3 300 315 U.S. pat. 3 301 682 Brit. pat. 1 005 825 Brit. pat. 1 196 501 U.S. pat. 3 222 193 Brit. pat. 1 137 228 Brit. pat. 1 212 258 German pat. appl. 1 492 787 Patentee and/or inventor(s) Date Foremost Dairies, Inc., Hutton, J. T., Nava, L. I., Shields, J. B., Kempf, C. A. Meiji Milk Prods. Co. Ltd. Feb. 29, 1968 Etablissements Laguilharre, Ciboit, J. J. Nov. 12, 1968 Dairy Foods Incorporated, Shields, J. B., Nava, L. J., Kempf, C. A. Borden Company, Williams, A. W., Busch, A. A. Jan. 5, 1965 Foremost Dairies, Inc., Nava, L. J., Hutton, J. T., Shields, J. B., Kempf, C. A. Carnation Company, Loo, C. C. Jan. 24, 1967 Nestle's Products Limited Sept. 29, 1965 Battelle Memorial Institute June 24, 1970 U.S.A. (Secretary. of Agriculture), Hanrahan, F. P. Dec. 7, 1965 Foremost Dairies, Inc. Dec. 18, 1968 Emery Carlton Swanson, Swanson, E. C., Henderson, R. J., Kyle, R. C. Flachroste Berching GmbH, Schanze, R Nov. 11, 1970 Oct. 17, 1970 Oct. 11, 1966 Jan. 31, 1967 APPLICATIONS OF SPRAY DRYING Whole milk Patent or application no. Sept. 11, 1969 -1=.• 00 Jl Product group no. (See table 13.1) Product Whey Whey Whey Whey Whey Whey Whey Whey Baby food Coffee/tea whitener Coffee/tea whitener Cheese Ice cream mix Patent or application no. German pat. appl. 1 921 793 German pat. appl. 1 943 422 German pat. appl. 2 007 960 Dutch pat. appl. 67.05296 Dutch pat. appl. 70.04843 U.S. pat. 3 522 054 German pat. 2 027 679 French pat. 2 012 982 East German pat. 29 870 U.S. pat. 3 241 975 U.S. pat. 3 321 318 Brit. pat 1 147 105 U.S. pat. • 3 215 532 , continued DC 41 Patentee and/or inventor(s) Date Ralston Purina Company, Arndt, R. H. Nov. 27, 1969 Kraftco Corp., Engel, M. E. March 5, 1970 Kraftco Corp., Singleton, A. D., Eggen, I. B. Sept. 24, 1970 Foremost Dairies, Inc. Oct. 16, 1967 Home Products Corp. Oct. 6, 1970 Cavroy, P. G. P., Rambaud, M. E M., Cousin, C. M. J. E., Savignac, G. G. E. A. Bratland March 7, 1967 Stauffer Chemical Company, Effinger, R. H., Schwartz, M. G. Hampel, Dip1.-Milchwirt Heinz-Georg, Hempel, Dr. Hans-Christoph Henry S. Brochner July 11, 1969 Koopmans Meelfabrieken N.V., Giddey, C. May 23, 1967 Societe Laitiere du Pays d'Auge `Solaipa' Apr. 2, 1969 Top-Scor Products, Inc., Bassett, H. J. Nov. 2, 1965 Dec. 17, 1970 July 5, 1966 AILISfICENI NI °MAIM AVILIS do SHOLLVOIlddV Table 13.2 March 22, 1966 Product group no. (See table 13.1) Product Ice cream mix High fat powders (butter) High fat powders (butter) High fat powders (butter) Casein Cultured buttermilk Honeyrnilk Milk protein concentrate Sour cream Patent or application no. Patentee and/or inventor(s) Date U.S. pat 3 357 840 Brit. pat. 1 041 465 Roberts Dairy Company, Fisher, C. D. Dec. 12, 1967 Commonwealth Scientific and Industrial Research Organization Sept. 7, 1966 Canadian pat. 704 131 Commonwealth Scientific and Industrial Research Organization, Hansen, P. M. T., Linton-Smith, L. Feb. 16, 1965 German pat. 1 201 669 Dr. Max E. Schulz Apr. 28, 1966 Brit. pat. 1 113 871 U.S. pat. 3 468 670 U.S. pat. 3 357 839 U.S. pat. 3 218 173 Vitamin Inc. May 15, 1968 H. C. Christians Co., Nilsson, C. A. Sept. 23, 1969 David Torr Dec. 12, 1967 Crest Foods Co. Inc., Loewenstein, M. Nov. 16, 1965 Beatrice Foods Co., Noznick, P. P. Dec. 12, 1967 Armour and Company, Hull, M. E., Kline, R. W. Nov. 11, 1969 Kuriyama May 20, 1970 U.S. pat. 3 357 838 Sweet cream U.S. pat. buttermilk 3 477 853 Whipped Japanese pat. appl. cream 70.14108 powder DNIAUCt AMIS 10 SNOLLVD1IddY Table 13.2—continued Table 13.2—continued 15.1.2 Egg products Product General Whole eggs Whole eggs Egg white Egg white Egg white Egg white Egg white 15.2 Beverages, flavours, meats, edible proteins 15.2.1 Beverages Coffee (instant) Coffee (instant) Coffee (instant) Patent or application no. Patentee and/or inventor(s) Date U.S. pat. 3 222 194 U.S. pat. 3 475 180 Japanese pat. appl. 70.13426 U.S. pat. 3 170 804 U.S. pat. 3 207 609 U.S. pat. 3 287 139 U.S. pat. 3 362 836 Brit. pat. 1 194 941 Norris Grain Company, Gorman, J. M., Hannah, V. H. Dec. 7, 1965 Tillie Lewis Foods, Inc., Jones, R. E. Oct. 28, 1969 Taiyo Foods Company Limited May 14, 1970 U.S.A. (Secretary of Agriculture), Kline, L., Sugihara, T. F., Meehan, J. J. National Dairy Products Corporation, Gorman, W. A., Stearns, C. K., Weisberg, S. M. Hercules Incorporated, Ganz, A. J. Feb. 23, 1965 Searle & Company, Scott, D. Jan. 9, 1968 Armour and Company, Sebring, M. June 17, 1970 U.S. pat. 3 361 571 U.S. pat. 3 361 572 U.S. pat. 3 406 074 Hills Bros. Coffee Inc., Nutting, L., Chong, G. S. Jan. 2, 1968 Hills Bros. Coffee Inc., Nutting, L., Chong, G. S. Jan. 2, 1968 The Kroger Co., Klein, P., Raben, I., Herrera, W. R. Oct. 15, 1968 Sept. 21, 1965 Nov. 22, 1966 A.IIISclUNI NI oNIAli ❑AVMS JO SNOLLVDIlddY Product group no. (See table 13.1) 41. 00 00 Table 13.2—continued Product Patent or application no. Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) Coffee (instant) U.S. pat. 3 421 901 U.S. pat. 3 436 227 U.S. pat. 3 458 319 U.S. pat. 3 458 320 U.S. pat. 3 514 300 U.S. pat. 3 529 968 U.S. pat. 3 535 119 Brit. pat. 1 099 810 Brit. pat. 1 214 283 German pat. appl. 1 807 308 German pat. appl. 1 933 591 German pat. appl. 2 000 315 French pat. 1 566 489 Patentee and/or inventor(s) Date General Foods Corporation, Mahlmann, J. P., Migdol, Jan. 14, 1969 N. R., Kaleda, W. W. The Folger Coffee Company, Bergeron, R. J., Hair, E. R., Apr. 1, 1969 Joffe, F. M. General Foods Corporation, Block, H. W., Henshall, N. July 29, 1969 The Folger Coffee Company, Niven, W. W. July 29, 1969 Mc°, S. k, Mishkin, A. R., Marsh, W. C. May 26, 1970 The Procter & Gamble Company, Hair, E. R., Dasher, D. F. Klein, P., Raben, I., Herrera, W. R. Dec. 18, 1967 The Procter & Gamble Company Jan. 17, 1968 General Foods Corporation Dec. 2, 1970 Societe des Produits Nestle S.A., van Sise, J. W. July 24, 1969 Oct. 20, 1970 Jan. 22, 1970 The Procter & Gamble Company, Lombana, C. A., Strang, D. E. A/S Niro Atomizer, Mengel, P. AA., Houghton-Larsen, E. July 23, 1970 Ottonia Etablissement, Bach, H., Bottger, M., Pabst, H. AV1MS JO SNOLINDIlddV Product group no. (See table 13.1) May 9, 1969 00 Table 13.2—continued Product Coffee (instant) Coffee (instant) Tea (instant) Tea (instant) Tea (instant) Tea (instant) Cocoa/coffee Fruit beverage 15.2.2 Flavouring compounds Patent or application no. Danish pat. appl. 3418/70 Danish pat. appl. 3419/70 U.S. pat. 3 451 823 Brit. pat. 1 117 102 Brit. pat. 1 117 103 Brit. pat 1 209 055 Brit. pat. 1 106 638 and 39 U.S. pat 3 395 021 Cola U.S. pat. beverage 3 510 311 Encapsulation German pat. appl. 1 255 081 Jelly U.S. pat. dessert 3 264 114 Meat Brit. pat. flavour 1 084 619 Patentee and/or inventor(s) Date A/S Niro Atomizer, Houghton-Larsen, E., Hansen, 0. Jan. 2, 1972 A/S Niro Atomizer, Hansen, 0. Jan. 2, 1972 Afico S.A., Mishkin, A. R., Marsh, W. C., Fobes, A. W., Ohler, J. L. Nestle's Products Limited, Giddey, A., Vuataz, L. June 24, 1969 June 12, 1968 Nestle's Products Limited, Giddey, A., Vuataz, L. June 12, 1968 Tenco Brooke Bond Limited, Plaskett, L. G., Miller, J. M. Rau, Willy Oct. 14, 1970 March 20, 1968 General Foods Corporation, Glicksmann, M., Farkas, E. H. July 30, 1968 Clay, W. C., Swaine, R. L., Beusch, D. W. May 5, 1970 Roha-Werk Walter Biihner & Co., Pilarczyk, W. Nov. 30, 1967 General Foods Corporation, Glicksmann, M., Schachat, R. E. International Flavors & Fragrances, Inc. Aug. 2, 1966 APPLICATIONS OF SPRAY DRYING IN INDUSTRY Product group no. (See table 13.1) Sept. 27, 1967 Product group no. (See table 13.1) Product 15.2.3 Meat 15.2.4 Edible proteins Green plants Soya beans Soya beans Soya beans Soya beans a.o. Tempa Patent or application no. Patentee and/or inventor(s) Date French pat. 1 568 051 Charier-Vadrot, Pierre May 23, 1969 Danish pat. appl. 116 340 Brit. pat. 1 202 678 Brit. pat 1 210 926 German pat. 2 043 490 Japanese pat. appl. 70.31344 U.S. pat. 3 489 570 Budapest Miiszaki Egyetem, Iloilo, J., Zagyvai, I., Koch, L. Ralston Purina Company Dec. 29, 1969 Aug. 19, 1970 Fuji Oil Co. Ltd. Nov. 4, 1970 Rohm and Haas Company July 1, 1970 Fujisawa Pharm Co. Ltd. Oct. 9, 1970 Beatrice Food Co., Noznick, P. P., Ludsas, A. J. Jan. 13, 1970 U.S. pat. 3 222 193 French pat. 1 568 929 French pat. 1 467 207 Brit. pat. 1 108 547 U.S. pat. 3 298 838 United States of America (Sec. of Agriculture), Hanrahan, F. P. Charier-Vadrot, Pierre Dec. 7, 1965 May 30, 1969 Baudot, Georges Jan. 27, 1957 Baudot, Georges Apr. 3, 1968 Villarreal, Jorge Rivera Jan. 17, 1970 15.3 Fruits and vegetables 15.3.1 Fruits General General Almonds Almonds, nuts a.o. Citrus fruits ONIAWG AV)IdS JO SNOLLVDrIcIdY Table 13.2—continued Product group no. (See table 13.1) Product Coconut Raspberries Tomato 15.3.2 Vegetables 15.4 Carbohydrates Corn products Patent or application no. Brit. pat. 1 144 256 German pat. appl. 1 225 952 U.S. pat. 3 353 969 Patentee and/or inventor(s) Date Beatrice Foods Co., Noznick, P. P., Bundus, R. H. March 5, 1969 Meyer-Frohlich, Dr. Hans Sept. 29, 1966 Beatrice Foods Co., Noznick, P. P., Bundus, R. H. Nov. 21, 1967 General Foods Corporation, Hollis, F. Jr., Borders, B. Nov. 30, 1965 General Foods Corporation, Sienkiewicz, B., Hollis, F. Jr. American Potato Company, Rainwater, J. H., Beck, R. G. July 19, 1966 July 20, 1967 Rohm & Haas GmbH, Krebs, J., Hoppe, G. Jan. 4, 1968 Beatrice Foods Corporation, Bundus, R. H., Luksas, A. J. May 11, 1965 Mashed potato Mashed potato Mashed potato Mashed potato Onions U.S. pat. 3 220 857 U.S. pat. 3 261 695 German pat. appl. 1 245 272 German pat. appl. 1 258 251 U.S. pat. 3 183 103 Dextrin and sweetener Pregelatinized starch U.S. pat. 3 320 074 Afico S.A., Gebhardt, H.T. May 16, 1967 U.S. Pat. 3 332 785 Boehringer Ingelheim GmbH, Kuckinke, E., Buchta, K. July 25, 1967 AILISIICINI NI ONIANCE Ad2IdS 40 SNOI1V311cIdV Table 13.2—continued Table 13.2—continued Sugar Patent or application no. Patentee and/or inventor(s) Date Dextrins (encapsulating agents) U.S. pat. 3 455 838 National Starch and Chemical Corporation, Marotta, N. G., Boettger, R. M., Nappen, B. H., Szymanski, C. D. July 15, 1969 General U.S. pat. 3 271 194 Brit. pat. 1 112 553 Japanese pat. appl. 70.07945 Dutch pat. appl. 70.01026 U.S. pat. 3 477 874 Belgian pat. 772 311 Brit. pat. 1 072 816 U.S. pat. 3 533 805 German pat. 1 203 585 French pat. 1 437 582 U.S. pat. 3 519 482 Yokohama Seito Kabushiki Kaisha and Takara Kabushiki Kaisha, Oikawa, H. Nippon Shiryo Kogyo Co. Ltd., Niimi M., Furukawa, T., Masada, H. Yokohama Sugar Refining Co. Ltd. Sept. 6, 1966 March 20, 1970 Hayashibare Company July 28, 1970 Karl Kroyer, A/S Niro Atomizer, Repsdorph, I., Kroyer, K. K. K., Damgaard-Iversen, J. A/S Niro Atomizer, Hansen, 0. Nov. 11, 1969 Foremost Dairies Inc. June 21, 1967 Foremost-McKesson, Inc., Nava, L. J., Palmer, G. M., Hutton, J. T. Brennerei and Chemische Werke Tornesch, Jessen, Dr. V., Hinck, K. H., Menzel, Dr. M. M. Jacques Lespagnol Oct. 13, 1970 CPC International Inc., Walson, G. P. July 7, 1970 Product General General Amylose Glucose product Glucose product Lactose Lactose Molasses Molasses Starch hydrolysate , May 8, 1968 Dec. 13, 1968 Oct. 21, 1965 March 28, 1966 ONIAIICE AV 4S 40 SNOI11011c1c1V Product group no. (See table 13.1) Table I3.2—continued Product Starch hydrolysate Starch hydrolysate Starch hydrolysate Sucrose Topping mix Sugar product colouring Other carbohydrates Cake mix Cake mix Pastry mix Polysaccharides 16 PharmaPharmaceutical– ceuticals biochemical Pharmaindustry ceuticals Patent or application no. Dutch pat. appl. 70.00560 Brit. pat. 1 169 538 Danish pat. appl. 2531/70 Brit. pat. 1 191 908 U.S. pat. 3 414 980 German pat. appl. 1 932 583 U.S. pat. 3 383 217 Brit pat. 1 113 806 U.S. pat. 3 257 213 Danish pat. 116 501 Brit. pat. 944 771 German pat. 1 932 583 Patentee and/or inventor(s) Date CPC International Inc. Sept. 29, 1970 Lyckeby Starkelsegiradling AB, Conrad, E., Frostell, G. Nov. 5, 1969 Lyckeby Starkelseforadling AB, Conrad, E., Theander, 0. Jan. 18, 1971 Nippon Shiryo Kogyo Co. Ltd., Niimi, M., Furukawa, T., Masada, H. National Dairy Products Corporation, Nezbed, R. L. May 13, 1970 Dec. 10, 1968 Boehringer Mannheim. GmbH, Rieckmann, P., Groppenbacher, G., Schellhorn, J., Rothe, W. Jan. 7, 1971 The Pillsbury Company, Meade, R. E., Greenberg, S. I. May 14, 1968 The Pillsbury Company May 15, 1968 The Procter & Gamble Company, Colby, E. E. June 21, 1966 The Pillsbury Company, Halleck, F. E. Jan. 19, 1970 S. A. Orsymonde, Lafon, V. Dec. 18, 1963 Boehringer Mannheim GmbH, Rieckmann, P., Groppenbacher, G., Schellhorn, J., Rothe, W. Jan. 7, 1971 APPLICATIONS OF SPRAY DRYING IN INDUSTRY Product group no. (See table 13.1) Table 13.2—continued Product group no. (See table 111) Product Enzymes Enzymes Enzymes Enzymes Active yeast Active yeast Food yeast Food yeast Vitamins Vitamins German pat. appl. 1 442 107 Danish pat. appl. 5370/68 Danish pat. appl. 804/69 Danish pat. appl. 1770/70 Danish pat. 108 847 Japanese pat. appl. 70.33753 U.S. pat. 3 407 072 German pat. appl. 1 227 413 French pat appl. 1 594 829 Danish pat. 114 040 Danish pat. appl. 117 265 German pat. 1 767 499 Danish pat. appl. 2755/68 Patentee and/or inventor(s) Date Instituto de Biologis y Sueroterapia, Sornovilla, N. M. U . Oct. 24, 1968 Pfizer & Co., Ayers, R. C., Kolb, C. A. May 7, 1969 Aktiebolaget Astra, Delin, P. S., EkstrOm, B. A., Sjoberg, B. O. H., Thelin, K. H., Nathorst-Westfelt, L. S. Aktiebolaget Astra, Delin, P. S., Kiessling, K. H. F., Thelin, K. H., Nathorst-Westfelt, L. S. Arbejdernes Fmllesbageri A/S Sept. 15, 1969 March 7, 1967 K. Takai Oct. 29, 1970 Toyo Jozo Co. Ltd., Aizawa, M., Matsuda, T., Omura, Amano, I., Nakamura, T. Standard Brands Incorporated, Johnston, W. R. Oct. 22, 1968 Oct. 27, 1966 Distillers Co. (Yeast) Ltd. July 17, 1970 Unilever N.V., Burt, A. W. A. May 19, 1969 Commercial Solvents Corporation, Miescher, G. M. Apr. 6, 1970 Oct. 11, 1970 E. Merck Aktiengesellschaft, Niirnberg, Dr. E., Pich, Dr. C. not yet published Dec. 16, 1968 F. Hoffmann-La Roche & Co. Aktiengesellshaft, Klan', Dr. H. APPLICATIONS OF SPRAY DRYING Lactic acid bacteria Medicinal yeast Active yeast Patent or application no. Product group no. (See table 13.1) 17.2 Cellulose industry 18 Offal and fish industries Gelatin Fish products Product Patent or application no. Resins and U.S. pat. crills in 3 364 101 paper pulp Resins and Danish pat. appl. crills in paper 117 738 pulp Patentee and/or inventors} Date A/S Niro Atomizer, Eek, T. Jan. 16, 1968 Tee-Pak, Inc., Bridgeford, D. J. May 25, 1970 Gelatin/ vitamins Gelatin/ vitamins Brit. pat. 1 142 147• Swiss pat. 389 505 Olaxo Laboratories Limited, Clegg, J. B., Elliot, L. G. Feb. 5, 1969 F. Hoffmann-La Roche & Co., Klaui, Dr. H. July 15, 1965 Crustaceans U.S. pat. 3 264 116 French pat. appl. 2 014 817 Dutch pat appl. 69.14370 Danish pat. appl. 5568/69 Gray, Robert D. Aug. 2, 1966 Louis Sanders S.A. April 24, 1970 Koninklijke Zout-Organon N.V. Oct. 26, 1970 Litton Industries Inc., Anderson, E. E. Apr. 22, 1970 Fish protein Fish protein Whole fish AILLSCIGNI NI ONIAIKI AVIRIS 10 SNOIIV3I1c1cIV Table 13.2—continued Product group no. (See table 13.1) Product Patent or application no. U.S. pat. Miscellaneous Fatcarbohydrate 3 514 298 products U.S. pat. Fat 3 295 986 emulsion U.S. pat. Fat 3 383 219 emulsion Danish pat. appl. Fat emulsion 1805/68 U.S. pat. Shortening 3 393 075 Patentee and/or inventor(s) Date Beatrice Foods Co., Noznick, P., Tatter, C. W. May 26, 1970 General Foods Corporation, Saslaw, I. M., Brady, J. J. Jan. 3, 1967 Patterson, Bernard A. May 14, 1968 Abbott Laboratories, Chapman, J. D. Oct. 27, 1968 Nippon Oils & Fats Company Limited, Hayashi, Y., Takama, N. July 16, 1968 ONIAIIGAV MSJO SNOIIVDrIddV Table 112—continued APPLICATIONS IN THE CHEMICAL INDUSTRY 14 Applications in the Chemical Industry 499 new area of application, establishing spray drying in the hydrometallurgical field with the handling of very high flotation concentrate feed rates to produce powders for smelting or chemical refining. Categories 14.8, 14.9 on inorganic and organic chemicals lists product groupings. New and/or specialized applications in the chemical industry (category 14.10) conclude the chapter, and include examples of spray cooling, spray reaction, and spray purification. 14.1. Plastics, Resins It is in the chemical industry that applications of suspended particle processing systems involving atomization (spray drying, spray cooling, spray reaction, spray purification) have grown most in the last decade. The time has long gone since detergent spray drying was the lone application of real capacity in the chemical industry to counteract the spray drying of milk and coffee in the then dominant food industry. To-day, applications in the chemical industry are extremely varied as shown in table 13.1 (chapter 13) where nine main categories are featured. It is impossible in the scope of this book to deal with all the applications mentioned. There is only space to briefly mention established and new applications, considered of wide appeal. Whenever possible, additional references are given to supplement the text. Category 14.1 on plastics, resins has evolved through the increasing use of synthetics. The spray drying of p.v.c. stands prominent in this category. Category 14.2 deals mainly with ceramics, where the spray dried product has shown itself ideal for pressing and sintering operations. In fact, spray drying has rationalized the production of pressbodies. Category 14.3 is devoted to detergents and washing agents, an area of application where spray drying first became established in the chemical industry. Category 14.4 deals with pesticides and here spray drying applications are widening as the product characteristics are proving ideal for effective and economic utilization, especially crop spraying. Category 14.5 (dyestuffs, pigments) is another of expanding interest. The dried product has all the desired properties, especially redispersibility, Category 14.6 on fertilizers is a relatively recent application, where spray drying has been incorporated with established production techniques to improve the economy of these techniques. The industry is dominated by prilling, which, being a spray cooling mechanism, is carried out in equipment similar to tall spray drying towers. Mineral ore concentrates, discussed in category 14.7 is the latest and a most important 14.1.1. Polyvinylchloride (p.v.c.) Vinyl chloride, produced from ethylene is polymerized catalytically in autoclaves to form polyvinylchloride (p.v.c.). There are three main polymerization techniques (359): emulsion polymerization (e-p.v.c.), suspension polymerization (s-p.v.c.) and bulk polymerization of liquid vinyl chloride (producing a dry polymer) (359). e-p.v.c. and s-p.v.c. are the two main types requiring drying. The nature of polymerization determines the type produced. Emulsion polymerization techniques give a particle size range sufficiently small for the particles to remain in colloidal suspension. Emulsions in water of uncoagulated p.v.c. are being produced under such names as paste polymer, paste resin or latex. s-p.v.c. particles are the result of large particle growth during polymerization, giving a granular polymer that lends itself to centrifuging, filtering and rinsing. Spray drying is the only practical way for drying e-p.v.c. Spray dryers can be operated to give the desired p.v.c. particle size distribution and degree of case hardening. Moisture contents down to 0.1 % can easily be achieved from the dryer chamber. s-ps.c. is sometimes dried in available dryers with powder rotary atomizers. Alternative drying processes are used, however, for large capacity s-p.v.c. drying. Drum drying is the popular method, but flash/fluid bed dryers offer a number of advantages that are now becoming recognized by many producers. (a) Emulsion p.v.c. The polymerized p.v.c. particles move within the colloidal range. Predewatering is not possible. Solids content can be increased by multi-stage vacuum evaporation. e-p.v.c. is spray dried applying either rotary or nozzle atomization to obtain a white powder of very low moisture (0.01-0.1 %). Feed solids range from straight emulsion (30 %) to pre-evaporated emulsion 55-60 %. Drying temperatures vary greatly. Maximum hot inlet air temperatures are around 575°F (300°C), but there are kinds of p.v.c. that are so heat sensitive that inlet temperatures may not exceed 330°F (165°C). However, all p.v.c. require drying chamber conditions that prevent retention of particles in an environment whereby scorching takes place. Presence of scorched particles is readily visible in the white powder. Areas around 500 APPLICATIONS OF SPRAY DRYING IN INDUSTRY the air disperser are the most likely source of scorched particles. HoweVer, it must always be borne in mind that it is possible for such particles to be present in the feed and it is clear that these particles cannot be diminished during the drying process. The size of dried p.v.c. particles is usually critical to the p.v.c. use. Product demands can be 90 % greater than 80 micron, or 90 % less than 60 micron (with mean size less than 40 micron). The mode of atomization is chosen according to the size requirement. Coarse powders are produced by pressure and two-fluid nozzles, or rotating inverted plates or cups. Fine powders are produced by rotating atomizer wheels of special design, or two-fluid nozzles. Where very fine particle sizes are required (e.g. 100 % less than 30 micron) pneumatic sieving of spray dried powder is applied. The atomizer is selected to produce a dried powder form, giving a minimum of oversized particles. Powder consists of hollow globules formed of cohesive colloid particles. The degree of cohesion is adjusted by means of temperature. Thus in the manufacture of dry product of paste quality, only slight cohesion is required and thus low temperatures are used. For strong linking demands higher temperatures are applied, but there is a maximum above which the individual particles melt to form fully sintered particles. When sintering or 'case hardening' of coarse particles is used, spray dried p.v.c. is marketed as such (without being pelletized) so as to enable the user to make his own formulations through dry mixing of p.v.c. with fillers, pigment stabilizers, etc. Case hardening effects can occur during atomization, but use of atomizer wheels and nozzles of special design can reduce this effect to be negligible if so desired. For many applications, paste-p.v.c. powder is mixed with a plasticizer. The viscosity of this mixture generally depends on influence of heat during spray drying, particle size, and mixing time. Although smaller particles lead to a lower mixture viscosity, grinding of powder to form smaller particles can result in higher viscosities. Cyclones and bag filters are used to recover airborne powder. The powder is rather brittle and the comminution effect associated with flow through cyclones can be utilized if even finer particles are required. However, product recovery from cyclones usually is insufficient to prevent powder emission levels that cause air pollution, and thus in these cases bag filters are installed. (b) Suspension P.V.C. s-p.v.c. contains larger particles than e-p.v.c. Mechanical de-watering is possible. By centrifuging, p.v.c. of 75-80 % solids can be obtained. This has a consistency of a filter cake and is termed p.v.c. (suspension) snow. It can be dried in a spray dryer using a special powder rotary atomizer. The atomizer wheel is of open design, and a powder chute feeds p.v.c. into the APPLICATIONS IN THE CHEMICAL INDUSTRY 501 wheel. The use of a spray dryer is usually restricted to manufacturers who have large e-p.v.c. capacity, but who also demand smaller amounts of s-p.v.c. For plants processing only s-p.v.c., flash /fluid bed dryers are used. 14.1.2. Resins Resins (polycondensates) are widely used today in powder form (496). For certain synthetic resins, a conversion to powder is required because the removal of water, organic solvents or diluents is necessary for further processing of the resin. Other resins are converted into powders because the liquid resin tends to undergo a slow change in characteristics due to continued polymerization. Powders can be stored practically indefinitely without changes in characteristics. Resins in powdered form are often preferred to liquid resins because of the much easier packing and handling. Powders require less freight expenses for transportation over long distance. However, the resin is eventually used in liquid form, but spray dried powder is readily reconstituted to liquid thereby meeting this requirement. Melamine urea, and phenol formaldehyde resins are dried in co-current flow dryers with air-broom attachment and dried product handling in cool air. S.B.R. and A.B.S. (Acrylonitrilebutadienestyrene) resins use similar equipment. Polycarbonate can be dried in counter-current flow nozzle towers. Melamine/Urea Formaldehyde Resins Melamine and urea formaldehyde resins are spray dried in large quantities (306). The resin powders are used in laminating, wet and dry adhesives in paper textile and leather treatment. The largest outlet is the board industry ; paper, composite, straw board and plywood etc. In the manufacture, formaldehyde is mixed with melamine (or urea) in a stirred glass lined kettle. Catalysts are added. Condensation is recorded by temperature and pH measurements. Reacting time depends upon the specific resin and product characteristics required. The finished liquid is pumped out of the kettle through a filter into holding tanks that are agitated and steam jacketed. The liquid resin (50-70 % solids) (120°F, 50°C) is pumped to the spray dryer with air broom (figure 5.12). A rotary atomizer (vaned atomizer wheel) is used (V1 = 140-160 m/sec). Inlet drying temperatures are 390-530°F (200-275°C), and outlet 150-165°F (65-75°C). At this outlet air temperature the resin particles are dry, but soft and tacky. Cold air is introduced at the dryer outlet to cool the particles well below the softening point and form a free-floWing powder. Cyclones are normally used to remove product from the exhaust air. The powder bulk density is 0.6-0.8 g/ml. Higher density can be obtained if the product is pulverised, and blended prior to packing. Spray dried resins are free-flowing powders of negligible moisture. Spray drying is well suited to handle the heat sensitive nature of the product. One of the first large resin spray dryers has been described by O'Connor (307). 502 APPLICATIONS OF SPRAY DRYING IN INDUSTRY 14.1.3. SBR Lattices Products with a styrene/butadiene ratio of at least 67 : 33 can be spray dried without the addition of fillers in e-p.v.c. spray dryer designs. 14.2. Ceramic Material The use of spray drying in ceramic manufacturing commenced in the midfifties, and today over 50 % of the total European volume of wall and floor tiles and electronic ceramics are made from spray dried pressbodies. With spray drying, the processing of slip preparations to finished pressbody is continuous without product hold-up. The unit operations involved in a typical example of processing are illustrated in figure 14.1. Raw material is blunged, milled, screened and mixed prior to drying, pressing and firing. In traditional operations of wet preparation the production of pressbody requires filter pressing, drying, crushing, rewetting and classifying, but modern operations with spray drying reduce these five stages to only one. RAW MATERIALS PRE-TREATMEN T WET-MILLING BLUNGING SCREENING APPLICATIONS IN THE CHEMICAL INDUSTRY 503 Spray dryers utilize either rotary or nozzle atomization. For dryers with rotary atomizers, slip is fed to the wheel by gravity or low pressure diaphragm pumps. Wheel periphery speeds are low to produce a coarse atomization. For large capacity wall-tile dryers, speeds are adjusted to around 300 ft/sec (90 m/sec). Wear resistant atomizer wheels incorporating either carbide or alumina bushings (figure 6.26) are used as the slip is abrasive. The wheel atomization is insensitive to fluctuations in feed characteristics and the wheel itself is not liable to clog. The particle size is controlled through regulation of wheel speed. The dryer installation is shown in figure 14.2(a). Direct oil, gas, or solid fuel heaters raise the air temperature upwards of 1100°F (600°C) prior to entering the drying chamber. Co-current flow conditions are used. The majority of the product leaves the chamber base, and the air is exhausted via a cyclone. The cyclone powder is normally mixed with the main chamber product in a common transport system. Alternatively, powder can be recycled to the drying chamber or to the slip preparation section. A wet scrubber of the liquid recirculation type is fitted after the cyclone to clean air of any powder escaping separation in the cyclone prior to passing to atmosphere. Scrubber liquid can be concentrated through recirculation, and passed back to the dryer feed tanks. For rather coarse powders, nozzle atomization can be used in low capacity dryers. The flow diagram is shown in figure 14.2(b). The slip is pumped by a diaphragm pump to nozzles operating at 150-300 psig (10-20 atm). Wear resistant nozzle orifices are essential. MAGNETIC SEPARATION spray drying processing traditional wet processing a. ROTARY ATOMIZATION FILTER PRESSING DR Y, ING CRUSHING SPRAY DRYING RE-WETTING AIR CLASSIFYING b. SILL PRESSES NOZZLE ATOMIZATION SORTING DRYING FIRING Figure 14.1. Examples of unit operations associated with wet preparation as compared with spray drying process. Figure 14,2. Spray dryers for ceramic pressbody; (a) with rotary atomization, (b) with nozzle atomization. 504 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE CHEMICAL INDUSTRY Dried pressbody must be free-flowing in order to rapidly fill the pressing dies. Spray dried pressbody has a controllable particle size distribution, consists of spherical particles, and with the absence of fines it is ideal for pressing operations. Moisture content and bulk densities are maintained constant, and the particle structure can be controlled by the spray dryer operation. The importance of binders in spray dried pressbody is discussed by. Hoffman (484). Particle shape and size distribution vary widely from pressbody produced by traditional techniques. Figure 14.3(a) shows a microphoto of a pressbody prepared according to the traditional wet process of filter pressing, drying, milling, etc. The pressbody consists of irregular shaped particles, has numerous very large particles and a noticeable amount of fines. The spray dried pressbody (figure 14.3(b)) has spherical particles and a narrower particle size distribution. These characteristics meet the correct degree of free flowability required for conveying, handling and pressing operations. 505 14.2.1. Wall Tile and Floor Tile Ceramics Recent advances in spray drying have enabled successful application of spray drying in the field of wall and floor tile production. Developments in both the chemical and mechanical preparation of highly concentrated slips and in the atomization of these slips to form a spray dried product of desired characteristics have rendered spray drying economically competitive to the traditional wet processing methods. The important product characteristics of average particle size, particle size distribution and moisture content of the finished pressbody can be adjusted in the spray dryer operation, within limits, through regulation of the slip properties, atomizer and drying conditions. Both wheel and nozzle atomizers are used. Typical screen analyses from industrial spray dryers operating with tile material are given in figure 14.4. The curves show the practical upper size limits for wheel and nozzle atomizers. There is an absence of fines. The spherical shape of the dried particles yields a freeflowing product which fills the pressing dies both uniformly and rapidly, thus securing the same density in all parts of the tile. In the tile manufacturing industry the nozzle atomizer generally has its optimum performance at capacities lower than 1.5-2 t/hr water evaporation. The rotary atomizer is more suitable in handling higher capacities. FEED 56-60% T.S.t 3% dispers/ng agent 1 (a) 1 1 1 1 1 1 r ' , i t .. - 99 . . 95 .. .. -. ... 75 50 I I I I 25 I I 5 I 1 I I 1 10 I I The flexibility of the spray dryer in producing pressbodies of various characteristics is important as pressing operations often require a specific pressbody quality to overcome product sticking to the dies. Sticking leads to non-uniformity in ceramic surfaces (especially tile surfaces). The preparation of the slip requires care to prevent impurities that can effect pressbody quality. The inorganic salts in water used to prepare the slip, and the salts added as deflocculants (to enable increase in solids content by reducing slip viscosity) remain in the pressbody. Combinations of salts can cause die sticking and choice of deflocculant is vital. 1- Ili Figure 14.3. Micro-photographs of pressbody. (a) Pressbody produced by traditional wet process. (b) Pressbody produced by spray drying. (By courtesy of Niro Atomizer.) i I (b) CUMULATIVE PERCENT LESS THAN SIZE D. 1 50 PARTICLE SIZE 100 ea) . micron) Figure 14.4. Particle size distributions of wall tile material produced by atomizer wheel and pressure nozzle atomization. A. Atomizer wheel 210 mm diameter 8300 rev/min, B, Pressure nozzle (swirl insert) 8 kpfern2. 506 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY 14.2.2. Oxide Ceramics (Ferrite, Aluminium Oxide, Steatite, Glass) Spray drying is used extensively in manufacturing oxide ceramics. Slips are sprayed into drying air at temperatures normally between 575-1375°F (300-750°C). The drying process is accomplished in 2-5 seconds, and after ..discharge from the dryer, the powder particles have a shape related to the original shape of the droplets formed during atomization. Spray dried powder is suitable for both isostatic pressing and the more conventional die pressing. A sample of steatite press powder is shown in figure 14.5. Spray dryers for oxide ceramics feature rotary or nozzle atomizers. Plant layout is similar to that described earlier in relation to figure 14.2. Feeds can be heat sensitive, e.g. glass and ferrite with organic binders and lubricants—softeners. 1mm Figure 14.5. Spray dried steatite. (By courtesy of Niro Atomizer.) Dryers are normally of limited size. Rotary wheel atomization is used where particle size distributions having a mean size within the range 50-150 micron are acceptable. Nozzle atomization is selected for sizes within the range 250-300 micron. The rotary atomizer holds many practical operational advantages as described by Helsing (208). The choice of atomizer is generally governed by the oxide ceramic powder size requirement. Where size distribution is critical both types can be incorporated in the drying chamber. Table 14.1 illustrates the particle size distribution of oxide 507 ceramics produced by nozzle atomizers. Where both atomizers are used simultaneously, feed rates to each atomizer are approximately equal. Table 14.1. Particle Size Distribution of Oxide Ceramics according to Atomizer Used Atomization type % by wt greater than (micron) 420 250 177 120 60 40 Wheel Nozzle %) ( %) Combined wheel-nozzle ( %) 0 6 27 55 84 94 6 60 76 86 96 98 6 32 52 73 94 96 Powders produced by rotary atomizers are widely used for isostatic pressing. The press powders are highly free-flowing and fines-free (no particles smaller than 15 micron). In die pressing flowability is important to enable the powder to rapidly fill all edges and cavities in the die during the pressing. Press powder prepared by conventional methods cannot produce such flowability. There are greater amounts of rejects. Due to low degree of abrasiveness, dies for pressing spray dried ferrite, for example, can be used for up to five times as many pressings as when conventional powder is available. Figure 14.3 illustrates pressing characteristics of conventional and spray dried powder. For steatite, pressing often requires a constant bulk density (1.0-1.2 &m') to meet existing tooling requirements. Strict control of the dryer outlet temperature and atomization of feed can meet specifications of constant bulk density. The characteristics of electronic ceramic pressbodies have been discussed by Storm (210). (a) Ferrites Ferrites are nowadays used in many areas. Electronics, communications and entertainment industries use soft ferrites in television, radio, lighting, telephones, and high frequency welding. The automotive industry uses hard ferrites in small motors that power windows, seats, etc. Power tools, cordless electrical goods, and a range of household appliances use hard ferrite. The ferrite industry is very extensive, based upon the use of permanent magnets (hard ferrite) and electromagnets (soft ferrite). Hard ferrites (barium and strontium iron oxides) and soft ferrites (manganese-zinc and nickel-zinc iron oxides) are manufactured from spray dried material by dry pressing. 508 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE CHEMICAL INDUSTRY The ferrite press powder produces a pressing devoid of imperfection such as cracks and voids, which could cause poor electrical and magnetic properties. The green strength of the pressing has been found to increase when using spray dried powder. This is an important feature since it is possible to subject the pressed (but not yet fired) components to high mechanical loads without fracture. Binders and lubricants, added to improve component strength can thus be reduced. Polyvinyl alcohol is commonly used as a binder, with softening agents of glycerine or ethylene glycol. The flow diagram for a ferrite production line is shown in figure 14.6. Raw material is analysed for foreign matter, then wet milled, spray dried and calcined. Calcined powder is reground by wet milling with lubricants, binders and deflocculents added. The resulting slurry is spray dried. Two RAW MATERIALS Fei 0 4 MnCO Zn O spray dryer ( rota ry{wh ee t) atomizer otory calciner LUBRICANT DEFLOCCULEN T BINDER pneumatic conveying spray dryer ( nozzle atomizer} bolt mill slurry teed tank PRESSI NG POWDER Figure 14.6. Flow diagram for production of ferrite by spray drying. 509 spray drying stages are utilized. A spray dryer with rotary (wheel) atomization is selected for the initial drying of green materials prior to calcining. A spray dryer of similar capacity with nozzle atomization produces the final pressbody of rather coarse nature from the calcined material. (b) Aluminium Oxide Aluminium oxide is used in vast quantities as spark plug insulating material. Completely homogeneous pressing is required for optimum electrical insulation performance. During production, there is direct transfer of powder from the dryer to the presses. Feed slurry to the dryer is approximately 70 % solids and contains additives to give powder improved pressing performance. Organic binders (e.g. polyvinyl alcohol) are preferred nowadays to wax binders, as the press powder is soft enough to maintain clean die presses but not soft enough to create turning difficulties when machining insulators on the lathe. Rotary (wheel) atomizers are used, where coarse atomization is achieved with low peripheral speeds (V T = 90-100 m/sec). Drying outlet temperatures are in the range 230-240°F (110-115°C) to give powder moisture contents between 0.1 and 0.25 %. Powder size distribution is narrow, an accepted distribution being of the order of 75-80 % greater than 60 micron, 12-20 % greater than 125 micron. (c) Steatite Steatite is produced generally on spray dryers with nozzle atomization. High bulk density requirements for pressing are achieved through control of slip composition and drying conditions. Steatite is used as insulator material. Homogeneity of the pressing powder is critical in achieving constant electrical insulating properties. Pressing produces a pressbody of smooth surface, which has the advantage of less adherence of surface dust and improved electrical insulation chracteristics. Increase in bulk density is achieved by increase in slip concentration. Concentrations as high as 85 have been successfully dried. Deflocculants are added to the slip. Where organic or volatile deflocculants (that volatilize during the drying or firing) cannot meet pressing requirements, electrolytic deflocculants are used. These deflocculants are carefully chosen so that they cause no adverse effect on the mechanical or electrical properties of the ceramic product. 14.2.3. Plastic Bodies (Ceramic Jiggering Bodies for Fine Stoneware and Art Ceramics) This is a relatively new application of spray drying in the ceramic industry. Jiggering bodies require 15-25 % moisture contents. Products with such high moisture contents cannot be produced directly in spray dryers, and thus part of the slip is dried to 5 % moisture followed by a mixing of powder with slip to obtain the desired moisture content. The layout is shown in figure 14.7. When using a planetary mixer to mix the powder and slip, an extremely homogeneous body with very exact water contents is achieved 510 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY PREPARATION OF CERAMIC SLIP in AIR LIFT gaol , 11[111 1[1 1 1J1 1 11 SPRAY SILO WEIGH INC VESSEL MIXER Figure 14.7. Flow diagram for preparation of spray dried jiggering bodies. in only 5 minutes of effective mixing time. Mixing proportions, to obtain 100 kg of 20 % moisture jiggering body, would be 123 kg of slip at 65 % solids, of which 73 kg is spray dried to 50 kg of 5 % moisture powder, which is then mixed with the remaining 50 kg of slip to form the jiggering body. Use of spray drying in the pottery industry has been described by Lengersdorff (209) and Helsing (509). 14.2.4. Glass Spray dried glass powder is used for insulating material. The powder must have a form whereby bubbles formed during sintering escape readily. Each particle must have a high physical strength and be extremely free-flowing. Acrylic resins are used as binders. Traditional binders like polyvinyl alcohol make the particles too brittle. Carboxymethylcellulose and a long range of low molecular binders destroy the free-flowability of the product and thus are not suitable. 14.2.5. Carbides (Tungsten, Titanium, Tantalum, Niobium) Carbide suspensions (carbide in organic milling liquid) are being spray dried nowadays in increasing quantities. Compared with older processing techniques, handling and labour costs are reduced and there is less risk of contamination. Carbides of the chemically pure analysis grade are readily obtainable by spray drying, The greater control of particle size achievable during the spray drying process is a further notable advantage in obtaining powders for such applications as pressings and flame spraying. 511 With the presence of organic liquids in the feed, a closed cycle spray drying system is adopted. The drying gas is a mixture of nitrogen and milling liquid vapour. The carbide is ball milled with an organic milling liquid, and a binder (2 %), e.g. hydrocarbon wax, added as lubricant. The suspension of carbide (75 % solids) is transferred from feed tanks to the spray dryer under nitrogen pressure. Alternatively, a feed pump system can be used. The closed cycle dryer is shown in figure 14.8. The drying chamber is a 'fountaintype' (see figure 5.9) with nozzle atomization. The suspension is atomized at the nozzle into a relatively coarse spray. The outlet temperature depends upon the organic milling liquid. A bone dry carbide is obtained from the chamber base. Particles that are exhausted with the gas leaving the chamber are recovered in a cyclone. (In the case of tungsten carbide the amount passing to the cyclone is very small.) The cleaned gas enters a scrubbercondenser, where the gas is cooled by cool milling liquid. The milling liquid in the feed evaporated during drying is condensed. The remaining gas is heated prior to returning to the drying chamber. The gas heater is of the indirect type, i.e. electric or liquid phase oil—heat exchanger. As with all closed cycle systems involving explosive mixtures, there is pressure and temperature instrumentation throughout the dryer layout. An oxygen analyser monitors the oxygen level in the drying gas. Sealed cleaning systems are also designed into the dryer. GAS DISPERSER GAS H EATER ( I NDIRECT } COOLER DRYING CHAM BER PRESSURE NOZZLE N FEED SYSTEM SCRUBBER/ CONDENSER 2 MILLI NG LIQUID MAKE- UP MAKE- UP DRY CARBIDE Figure 14.8, Flow diagram for spray drying carbides in closed cycle. 14.3. Washing Powder (Detergents, Soaps, Surface Active Agents) Washing powders are one of the best known of spray dried applications. The free-flowing, non-dusty, non-caking products in bead form are produced in either co-current or counter-current flow dryers with rotary or nozzle 512 APPLICATIONS OF SPRAY DRYING IN INDUSTRY atomization. The use of counter-current flow with nozzle atomization is the preferred layout for high bulk density household products. Feeds are homogenized and fine-filtered prior to passing to nozzles operating at high pressure. Air vessels are used to dampen pump pulsations. Hot air from direct fired air heaters enters from a circular channel at the base of the cylindrical part of the tower with slight rotary motion. The exhaust air is drawn from the top of the tower. Inlet temperatures vary according to product. Up to 750°F (400°C) is used for some detergents, but lower temperatures are used for fine washing agents, the exact value being determined by the organic content in the feed. Product recovery from the drying tower is very high (99 %). The fines fraction is usually returned to feed preparation. Washing powders fall into four groups: Heavy Duty Detergents (high and low foaming). Light Duty Detergents. Soap Powders. Soda Products. Detergent formulations consist basically of (a) an active ingredient, (b) sodium tripolyphosphate, (c) silicates, (d) sodium sulphate. The active ingredients can be cationic, anionic or nonionic. The most common are anionic, namely fatty alcohol sulphates, primary and secondary alkyl sulphonates and alkyl aryl sulphonates. Synthetic detergents are currently based upon linear alkyl benzene sulphonates, obtained from n-paraffins via alkylation and sulphonation. Formulations have been recently (1970) discussed by Duckworth (213). The composition of detergents vary according to their use. Light duty products have a low (or even no) phosphate and high sulphonate content whereas the proportions are opposite for heavy duty detergents. Heavy duty products are for tough cleaning jobs in the home and in industry. Light duty products are for dish washing, light household cleaning and laundering of delicate fabrics. Low foam products have a soap constituent and low sulphonate content, and are especially used in automatic washing machines. Soap powders rarely contain high proportions of soap, but are sold containing 45% soap with soda and additives. Soda products consist of sodium carbonate and waterglass. 14.3.1. Heavy Duty Detergents Synthetic detergents are widely used in cleaning of all types and operate successfully with hard water. The coarse powder granules in bead form are free-flowing, non-dusty and readily dissolve in water. Shelf-life is excellent, with no tendency to instability or lumping. The feed can be formulated batchwise or continuously. The preparation technique has definite influence on the final dried properties. Precise weighing/metering, mixing, homo- APPLICATIONS IN THE CHEMICAL INDUSTRY 513 genizing and de-aeration, takes place before spray drying. As high a solid content as possible is used (50-65%) to give the highest powder bulk density and best economic use of the spray dryer. The feed must be free of air and free of material that can clog the nozzle atomizer. The product is dried in a counter-current flow drying tower at inlet temperature 660-750°F (350400°C), outlet 195-230°F (90-110°C). Nozzle atomizing pressure is in the range 30-60 atm. The dried powder leaves the base of the drying tower and is transported via a conveyor belt to an air-lift. During passage on the belt product dosing is carried out. Dosing can be products that would be damaged during spray drying, e.g. lauryl alcohol, enzymes (505). Bleach in the form of sodium perborate is also added at this stage, and sometimes a specially protected enzyme product (enzyme encapsulated in wax). Perfume is added after the following air lift. Physical properties of heavy duty detergents can be generalized as Active ingredient, e.g. alkyl benzene sulphonate 14-20 % Foam booster, e.g. lauryl alcohol 0-5 % Sodium tripolyphosphates 30-45 % Anti-soil redeposition agents, e.g. sodium carboxymethyl0.1-1.5% cellulose Anti-corrosion agent, water glass 5-8 Filler, e.g. sodium sulphate 10-15 Optical brightener 01-05 % Perfume 0.1-0-2% Bleach (sodium perborate) 6-15% Enzymes 0.3-0.75 % Perborate decomposition preventives (ethylenediamines of % fatty acids) Moisture content 8-13 0-30-0.35 g/cm 3 (after spray drying) Bulk density 0.35-0.40 g/cm 3 (after perborate dosing) 2-3% Size distribution > 1500 micron 10-20 > 500 50-75 > 250 85-95% > 120 95-100 > 60 The addition of sodium silicate reduces corrosion in washing equipment and pitting of enamel glosses. Carboxymethylcellulose (CMC) prevents the redeposition of soil especially in the case of cotton garments. Optical whiteners are used in all formulations, as these absorb ultraviolet light and reflect it as visible light making the fabric appear brighter. The addition of enzymes to synthetic heavy duty detergent powder is a new development that has created a substantial market. The development 514 APPLICATIONS OF SPRAY DRYING IN INDUSTRY arose out of enzyme pre-soak powders. Proteolytic enzymes are used. The majority of protease preparations are fermented products of the microorganism, bacillus subtilis. The enzyme is added as a spray dried product (503). The activity of the enzyme depends upon temperature with optimum activity between 120-160°F (50-70°C). The addition of ethylenediamines of fatty acids (e.g. ethylenediamine tetra-acetic acid) acts as organic sequestering agents. These organic agents tend to sequestrate the metallic salts naturally present as trace impurities in other materials that catalyse the decomposition of hydrogen peroxide. These agents are added to act as perborate stabilizers. Low foam washing powders have been developed to meet the increasing use of automatic washing machines. Synthetic detergents foam substantially under the severe agitation produced in washing machines. Low foam powders are based upon soap. The powder is free-flowing, readily dissolvable, and in fact the physical properties are similar to heavy duty detergents. The particle size distribution is about the same, but bulk density is around 0.35 g/cm 3 . Spray drying procedure is similar to heavy duty detergent. A low foam formulation can be generalized as 5-7 % soap 4-5 % alkyl aryl sulphonate 4 % ethylene oxide condensation product 8-9 % silicate (water glass) 10-15 % filler, e.g. sodium sulphate 35-40 % phosphates 12-15 % perborate Traces of CMC, enzymes, optical brightener and perfume The moisture content is approx. 8 %. 14.3.2. Light Duty Detergents Light duty detergents are used less than the heavy duty. They find wide application only in dish washing and light household cleaning (janitoring). Light duty detergents are produced in nozzle towers with either co-current or counter-current flow. The particle size is much finer than heavy duty products. Inlet drying temperatures are also lower 480-530°F (250275°C). Outlet temperature is in the range 210-230°F (100-110°C). Nozzle pressures are around 20 atm. The physical properties are 30-35 % alkyl aryl sulphonates 0-5 % fatty alcohol sulphates 50-60 % sodium sulphate Moisture content 0-3 % Bulk density 0.15-0.20 g/cm 3 Size distribution > 1500 micron 0 X500 10-15% APPLICATIONS IN THE CHEMICAL INDUSTRY > 250 > 120 > 60 515 40-60 70-80 95-100 14.3.3. Soap Powder Soap powder for hand use requires low temperature operation and is usually flash dried under vacuum. The spray drying of a 60 % soap feed with wheel atomization (320-170°F, 160-75°C) or nozzle atomization (440-195°F, 225-90°C) in co-current flow dryers is rarely used these days. Products based upon soap and soda are varied in composition. Products consisting of mainly soap and soda are spray cooled, but such products these days require added constituents which have increased the water content so that spray drying must be used. A typical formulation may well contain 45 % soap, 20 % soda, 5 % silicates, 5 % phosphates, 23 % moisture and 2 % as CMC, optical brightener and perfumes. Such a product consists of particles 20 % > 300 micron, 50 % > 200 micron and 80 % > 85 micron. This is much finer than synthetic detergents. If the soda content is in the range 20 40 %, the powder is dusty. The spray drying of neat soap, and soap-soda formulations, are described by Stockmann (308). A dryer with two-fluid atomization of neat soap is cited. 14.3.4. Soda Products Soda bleach contains sodium carbonate and water glass. Formulations can be made more forceful by the addition of a little soap or active ingredients. These products are relatively dusty, but of high bulk density, 0.6 g/cm 3 , and are produced by spray cooling or spray drying with either rotary or nozzle atomization. Dryers are similar to those used for soap powders. Spray Dryer Layout for Washing Powders In current high tonnage production of spray dried detergents, continuous mixing of ingredients are used to form formulations that are spray dried in counter-current drying towers with nozzle atomization. Many spray towers have built-in flexibility of both co-current and counter-current air flows in order to handle special formulations and achieve specific bulk density. The plant layout for detergent formulations consists of a feed preparation section (automatic feeding, proportioning and mixing) feed pumping to the nozzle atomizer, dried powder conveying and dosing, followed by thorough blending, screening and packaging. The layout is shown in figure 14.9. Linear alkyl benzene sulphonate paste, the preparation of which has been recently discussed by Duckworth (213), is metered into a slurry preparation tank together with metered sodium silicate solution, and solid phosphates, sulphates and additives. The blending of these ingredients has been described 516 APPLICATIONS OF SPRAY DRYING IN INDUSTRY SOLIDS FROM SILOS APPLICATIONS IN THE CHEMICAL INDUSTRY EXKAUST AIR SLURPS' ADEIN CRUTCH. FILTERS RONDO NIZER MGM PRESSURE FEED PUMP WITH FILTER AND AIR VESSEL DIRECT FIRED AIR HEATER DETERGENT PAC KIRA Figure 14.9. Flow diagram for spray drying of detergent formulations. by Silvis (212) in detail. The slurry preparation tank acts as a coarse mixer. Here lumps are broken down and air pockets are eliminated. Materials after blending are conveyed to an ageing vessel. Mixing is carefully controlled to prevent aeration of the slurry. Feed slurry passes through a coarse filter, homogenizer (colloid mill) and fine filter. Deaeration of product is carried out if necessary. The slurry of constant solid content and viscosity is ready for spray drying. The handling of product in the feed treatment section plays a large role in the quality of the dried product (e.g. granulation, degree of fines, etc.). The slurry (120-180°F, 50-80°C) is fed to the spray dryer by a high pressure pump. Counter-current product—air flows are mainly used, although parallel co-current and mixed flow can be used where a definite air flow profile results in a special quality of detergent bead. Counter-current flow systems give product bulk densities 0.2-0.4 g/cm 3 and moisture contents 6-15 %. Co-current flow systems give low bulk densities 04-0.15 g/cm 3 with moisture content 3-8 %. Mixed flows give high moisture contents 20-25 %. The vast majority of powder leaves the base of the chamber. The entrained fines fraction is recovered from the exhaust air in cyclones or bag filters. 517 These fines are returned to the wet zone in the drying chamber for agglomeration or reslurried. The main product is belt conveyed to an air lift. Any after-drying dosing is carried out on the belt. This can be organic foam boosters (lauryl alcohol), enzymes (proteolytic) and sodium perborate. The air lift raises the powder to a storage hopper from where gravity feed takes the product through screens, a perfuming chamber to packing machines. 14.3.5. Bleach Powders Active ingredients in bleach powders can be divided into four groups (a) inorganic chlorine releasing compounds, (b) organic chlorine releasing compounds, (c) oxygen releasing compounds, (d) optical brightening agents. The groups are fully discussed by Milwidsky (309). Group (a) consists of salts of hypochlorous acid, group (b) compounds are very varied and new chemicals are proposed month by month (chloramines, chlorinated isocyanuric acids). Group (c) are reactant products of hydrogen peroxide and inorganic salts. Sodium perborate is well known as a bleaching additive in washing powders. Perborate dosing is carried out after spray drying as incorporation of the product before drying is difficult. Bleaching activity requires quite hot temperatures as perborate is stable in cold water. Stability in storage is often assisted by addition of magnesium sulphate, or organic sequestrating agents (ethylenediamine tetra-acetic acid) that prevent decomposition of hydrogen peroxide. Optical brighteners in group (d) are discussed separately below. Household bleach powders are produced by spray drying in co-current flow dryers with rotary atomizers. Granular powders can be produced by maintaining a high powder moisture content in the drying chamber to form agglomerates that are after-dried in a fluid-bed mounted at the chamber base. Low outlet air temperatures are used. The final product is granular and non-dusty. Dryers with air-broom attachments (figure 5.12) and pneumatic product cooling are also used but products are not so granular due to comminution effects during conveying. 14,3.6. Optical Brighteners These products are chemicals for brightening fabrics during washing. The mechanism is one of ultra-violet absorption, which is reflected as visible light. Hence fabrics appear brighter than untreated fabric when viewed in daylight. These products are fluorescent dyes which tend to fluoresce in the blue and ultra-violet end of the spectrum. There is a difference between optical brighteners and blues of the older technique. In bluing, the blue pigment absorbs yellow and red light falling on fabric, thereby removing the apparent yellowish tint of linens, etc. Blues (e.g. ultramarine, phthalocyanimes) reflect less light than they receive, whereas an optical brightener reflects the same amount of light in a different shade. Optical 518 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY brighteners are spray dried in co-current flow dryers with rotary atomizers or low pressure nozzles. Choice of brightener depends upon the presence of powder bleaches, as many are susceptible to oxidation. 14.3.7. Perfumes for Washing Powders Spray drying of perfumes involves micro-encapsulation. The droplets of perfume oil are dispersed within a protective colloid (emulsion) and when dry, the colloid forms a protective skin to prevent fragrance losses due to diffusion into atmosphere. Colloids generally used are gum arabic or dextrin. They are water soluble. Each microcapsule contains numerous minute droplets of perfume oil. A microphoto of an encapsulated fragrance is shown in an article by Barreto (310). The spray dryer for perfumes incorporates either nozzle or rotary atomization in a co-current flow chamber. The drying procedure is straightforward. It is the preparation of the perfume feed that determines the success of the operation. The feed consists of the perfume oil, the emulsion and water. The ratio of oil to emulsion is important as too little emulsion leads to poor encapsulating during spray drying and fragrance losses. Too much emulsion leads to a high viscosity feed that is difficult to dry due to poor atomization. General feeds to the dryer contain 40 % solids. The spray drying process is ideal for perfumes, as during the evaporation process droplet temperatures are low and fragrance volatilization is negligible during the time it takes for the protective skin of the droplet to harden. Spray dried perfumes are used in the manufacture of soap powders, synthetic detergents, cleansers and chemical specialities. These are of special interest in chlorinated products since they do not react with other chemicals of the formulation. The powders are free-flowing, easily blended and require no special packaging, as long as water is absent. 14.4. Pesticides Spray drying has been adopted worldwide for pesticide preparation using either open, semi-closed or closed cycle drying systems. Spray dryers are designed for a given pesticide, or with built-in flexibility to enable the drying of a number of formulations. Pesticides can be divided in herbicides, fungicides and insecticides. Herbicides are (a) phenoxy derivatives, (b) halogenated acid derivatives, (c) benzoic acid and phenyl acetic acid derivatives, (d) others (e.g. chlorates). Fungicides are (a) dithiocarbamates, (b) colloidal sulphur, (c) copper compounds, (d) thiuram disulphides. Insecticides are (a) chloride containing compounds (D.D.T.), (b) arsenates, (c) thiophosphates (parathion), (d) others, 519 Examples of pesticides that are successfully spray dried HERBICIDES Methyl-chloro-phenoxyacetic acid sodium salt (MCPA-salt) Methyl-chloro-phenoxybutyric acid sodium salt (MCPB-salt) Dichloro-phenoxybutyric acid sodium salt Methyl-chloro-phenoxyacetic acid (MCPA) Dichloro-phenoxypropionic acid Dichloro-phenoxypropionic acid mono-methylamine salt Dichloro-propionic acid sodium salt Dimethyl-dipyridyl-dichloride Chlorates FUNGICIDES Mangano-ethylene-bis-dithiocarbamate Zinc-ethylene-bis-dithiocarbamate Zinc-dimethyl-dithiocarbamate Zinc-diethyl-dithiocarbamate Tetramethyl-thiuram-disulphide Copper oxychloride Cuprous oxide Colloidal sulphur INSECTICIDES Pentachloro-phenolate Sodium pentachloro-phenolate Sodium methyl-arsenate Sodium aluminium fluoride Calcium arsenate Lead arsenate Sodium fluoride DDT Thiophosphates Most pesticides are dried as liquids. Where feeds are filter cake, powder atomizer wheels are used (figure 6.67). Operating conditions are varied due to the complex range of pesticide formulations. Due to the toxicity of pesticides, prevention of environmental pollution is one of the most important problems of manufacture. The degree of hazard caused by pollution depends upon the product. Insecticides being poisonous to humans must not contaminate working areas. Herbicides and fungicides are not poisonous to humans but emission to atmosphere can readily cause damage to surrounding flora, especially with herbicides. Such conditions are prevented by the use of semi-closed or closed cycle spray drying layouts. A suitable semi-closed cycle dryer is shown in figure 14.10. The drying medium is air, which is exhausted via a scrubber system. 520 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE CHEMICAL INDUSTRY INDIRECT AIR HEATER CONDENSER/COOLER HERBICIDE Figure 14.10. A semi-closed cycle spray dryer for herbicides (a part of the exhaust air is used as combustion air in heater). Part of the scrubber air is recycled through an indirect oil/gas fired air heater to the drying chamber. The remainder is used as combustion air in the heater. Any herbicide present in the air leaving the scrubber is decomposed (inactivated) during passage through the heater combustion zone. The quantity of air passed through the heater combustion zone equals the air entering the dryer layout as powder conveying air. Closed cycle systems (figure 0.2) are used where an organic solvent in the feed requires an inert gas drying medium. For recovery of solvent following evaporation in the drying chamber, a condenser-cooler replaces the scrubber. If the toxicity of the product and plant location permit open cycle dryers, very low emission levels can still be obtained by use of scrubbers in series with cyclones or bagfilters. 14.4.1. Herbicides The sodium salt of organic herbicide formulations is generally spray dried for products used for spraying (crop dusting) operations. Examples of such salts are methyl-chlorophenoxyacetic acid-sodium salt (MCPA-sodium salt) and dichloropropionic acid-sodium salt. The free acid form of herbicide formulations is spray dried using powder wheel atomizers (figure 6.67). Free acids are manufactured as intermediate products. All herbicides require efficient exhaust cleaning air equipment. Cyclones are usually used as the primary collector, but these are followed by bag filters or wet scrubbers in open cycle systems or scrubbers (cooler condensers) and air heaters in semi-closed and closed cycle systems. MCPA-sodium salt is often dried in semi-closed cycle systems. A 50 % liquid feed is atomized with a vaned wheel (VT = 500 ft/sec, 150 m/sec) in a co-current flow dryer. Inlet hot-air temperatures are of the order 500°F (260°C). The MCPA 521 (pure acid) can be dried as a filter cake using a powder atomizer wheel at lower speeds (VT = 360 ft/sec, 110 m/sec). Drying air temperatures are lower (280°F, 140°C). Dichloropropionic acid sodium salt is spray dried in special designs that need very exact control of the exhaust air temperature. Low moisture content levels in the powder are required. If air temperature falls and the powder becomes moist, decomposition occurs with product condensation in the bag filters. 14.4.2. Fungicides Fungicides are generally spray dried with rotary atomizers (vaned wheel). Two important fungicides, the ethylenebisdithiocarbamates of zinc and manganese are spray dried in this way. Close control of exhaust air temperatures is required for the manganese form. If powder becomes too dry (moisture less than 2 %) product heat degradation occurs through product smouldering. 14.4.3. Insecticides DDT (Dichloro-diphenyl-trichlorethane). DDT melt is spray cooled. Cocurrent flow chamber is used. Inlet air temperature of 140°F (60°C) and feed temperatures of 195°F (90°C) are observed. A rotary atomizer forms a spray with 100 % greater than 60 micron and approx. 30 % greater than 500 micron. Spray cooling eliminates the stickiness associated with conventional methods. The powder bulk density ranges between 0.35-0.42 g/cm 3 . The powder is quite brittle. It has excellent solubility. 14.5. Dyestuffs—Pigments Organic dyestuffs can be classified as soluble dyes (direct, acid, basic), vat dyes (indanthrene dyes, indigo, indigosol dyes), azoic dyes (naphthols, diazo compounds), microdisperse (formulated) dyes and reactive dyes. Organic dyestuffs are highly suited to spray drying. For organic dyestuffs a maximum hot drying air temperature of 480°F (250°C) applies for the vast majority of products. Rotary and nozzle atomization is applicable. Hollow particles or agglomerates are formed. These are rather brittle and are easily dispersed into dissolvers or similar aggregates. Desired moisture or residual diluent content can generally be achieved by the spray drying operation, but for extremely low moisture contents, after-dryers (pneumatic or fluid-bed) are incorporated at the base of the drying chamber. Cyclones are used as the product separation and recovery equipment. These are easily cleaned enabling different dyestuffs to be dried in the same unit. Wet scrubbers are mounted after cyclones to remove traces of dyestuff leaving the cyclones. It is usual these days that, on account of cleaning requirements, each product has its own spray dryer. In these cases bag filters are often used instead of cyclones. Co-current flow spray 522 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY dryers with rotary atomization is the standard lay-Out for most dyestuffs. For special requirements, e.g. coarse, non-dusty, or extremely heat sensitive products, nozzle atomization is applied in tall co-current flow towers having parallel (streamline) air flow conditions. To create and maintain this air flow, the air disperser is a perforated plate. The exhaust air is drawn from the tower via a ring having six equidistant apertures. The apertures converge to two exhaust ducts. Product recovery from the drying tower is approx. 98 %. For coarse product requirements, the fines are returned to the wet zone around the nozzles for agglomeration. Organic and inorganic pigments can be spray dried. Rotary and nozzle atomization is applicable. Particle characteristics are similar to dyestuffs. Pigments are used in rubber, paint, ink and plastics manufacture. Wellknown inorganic pigments include titanium dioxide, kaolin, zinc chromate, iron oxide and carbon black. For dyestuffs or pigments that occur as suspensions in organic liquids or as dispersions in resin, closed cycle dryer layouts are used (figure 0.2(b)). If the dried product can cause powder explosion conditions in air, semiclosed cycle dryer layouts are used, designed on the self-inertizing principle. The recycled drying air/gas is heated by direct gas firing at an open ring burner. A controlled percentage of excess air is used at the gas burner. The layout is similar to figure 0.2(c) but after the cooler/condenser, a volume of exhaust gases equal to that used as combustion air is bled from the system. The 0 2 content in the dryer is thus held low preventing explosion hazards. The 0 2 content in the dryer is approximately 1/5 the excess combustion air (i.e. 2 % 0 2 content for 10 % excess combustion air). 14.5.1. Titanium Dioxide White thixotropic filter cake (up to 60 % solids) is dried at inlet/outlet temperatures (1110/250°F, 600/120°C). The moisture content of the powder is 0.5 %. Co-current flow dryers are used with rotary atomizers, or mixed flow with nozzle atomization. Choice of atomizer depends upon requirements to particle size distribution of the dried product. The flow diagram is shown in figure 14.11. The filter cake is fed into a disperser to worksoften the paste. Vigorous agitation reduces the titanium dioxide viscosity to a level whereby a pumpable smooth paste is formed. Diaphragm pumps are used to supply the rotary atomizer. The pump must have large suction and discharge parts. A strainer/disintegrator can be placed between the pump and atomizer to prevent any undispersed product passing to the atomizer where plugging can occur. Use of a flooded disintegrator for spray dried titanium dioxide has been reported by Young and Ireland (311). Direct gas fired heaters (open jet ring) are used, with combustion controlled to prevent formation of soot that can taint the white powder. The dried powder is collected in a bag filter. The dryer is normally controlled 523 by maintaining a constant feed rate and controlling gas combustion rate to maintain a constant outlet temperature and prevent bag filter damage. Safety devices to safeguard the bag filters against excess heat are standard. The bags are of polyacrylonitrile or polyester fibres. The powder is often micronized after drying. Hence there is little need for a coarse powder unless sold in this state. Titanium dioxide is most widely used as a white pigment in paints, paper, etc. Ti TANIUM DIOXIDE FILTER CAKE STRAINER — SI N TE GRA TOR DIRECT AIR HEATER DISPERSER DIAPHRAGM PUMP SPRAY DRI ED Ti 0 PIGMENT 2 HIGH SHEAR FEED PREPARATION [ work-softening of thixotropic Ti 0 2 ] Figure 14.11, Flow diagram for spray drying titanium dioxide. 14.5.2. Kaolin (China Clay) Kaolin clay was one of the first inorganic materials to be dried in spray dryers of large capacity. Figure 4.13 shows a complex of four spray dryers, (30 ft (9 m) in dia), each producing 12-15 tons dried kaolin per hour. The purity and uniformity of spray dried kaolin has established wide usage in the paper, paint, plastics, rubber, and ceramic industries. Kaolin is a hydrous aluminium silicate (Al 2 0 3 .2Si0 2 .21-1 2 0). It is a leading white pigment consumed in vast tonnages. The bulk goes to the paper industry as coating material in high gloss and quality printing grades and as a low cost filler. The process diagram for kaolin is shown in figure 14.12. Crude kaolin from the mine is milled, crushed and slurried in a blunger with water and chemical dispersants (sodium silicates or phosphates). The resulting clay slip (25 % solids) is fed through sets of degritting wet cyclones, screened and left to settle in large settling tanks for up to 14 hours. The bottoms are passed through wet cyclones and pumped to the filter clay plant. The fine clay slip drawn off the top of the tank consists of approx. 524 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE CHEMICAL INDUSTRY 525 Figure 14,13. High tonnage spray dryers on kaolin in Georgia, U.S.A., each producing 15-25 tons per hour. (By courtesy of Nichols/Niro Atomizer.) 85 `)/, less than 2 micron particle size. This is immediately treated with acid, flocculating the slip, and bleached (zinc or sodium hydrosulphite). pH is adjusted to 3.5 with sulphuric acid. The clay slip changes from a cream to blue—white colour. After bleaching, the slip is thickened to 12% solids, passed through 150 mesh screens and centrifuged to 25 % solids. The solids are increased to a 60-65 % solids cake in a vacuum filter. For spray drying the solids cake must be transformed into a free-flowing slurry, a requirement for acceptable atomization. The solids content must, however, be held high to achieve an economic spray dryer operation. A free-flowable slurry is obtained by the addition of dispersants (tetrasodium pyrophosphate, tripolyphosphate or sodium hexametaphosphate) on a 0.3 % dry solids basis. The feed slurry is passed through 150 mesh screens and a magnetic separator before entering the spray dryer. The spray dryer is a co-current flow conical based design. Rotary atomization is employed using abrasion resistant wheels (figure 6.26). Drying air (oil or gas heaters) at 1100°F (600°C) enters the dryer via a central air disperser located just beneath the wheel. This arrangement prevents local hot spots on the roof, which could cause product discolouring. Drying air is exhausted at 250°F (120°C) and product falls to the base of the chamber for discharge into conveyors. The dried product temperature is around 526 APPLICATIONS OF SPRAY DRYING IN INDUSTRY 160°F (70°C). Clay fines that are exhausted with the air are recovered in cyclones or bag filters. The dried clay (1 % moisture) consists of microspheres and are non-adhesive. It is an essentially 100 % pure, free-flowing, high bulk density product. There are several references to spray dried kaolin in the literature (224) (226) (312). 14.6. Fertilizers Application of spray drying in the fertilizer industry is restricted to a few, but important products, e,g. ammonium phosphate and superphosphates. The well-known process of manufacturing phosphate fertilizers by reacting phosphate rock with phosphoric acid has been modified by the introduction of spray drying. Although based upon the traditional wet process, it differs in having part of the phosphate rock—phosphoric acid mixture spray dried before granulation. Other important fertilizers, e.g. compound N—P—K types, ammonium nitrate, and nitro chalk, are produced by the spray cooling principle. The reader is referred elsewhere (233) for flow diagrams of industrial fertilizer production utilizing spray processes. 14.63, Ammonium Nitrate Ammonium nitrate is mostly produced by direct neutralization of nitric acid with ammonia according to the basic equation : NH 3 + HNO 3 = NH 4 NO 3 + 20 600 cal The neutral solution of NH 4 NO 3 is concentrated to more than 90 %, in most cases by utilization of the heat of neutralization. The concentrated solution is then treated according to either of the three methods in order to obtain a dry product. (1) Graining is normally effected by evaporation of the ammonium nitrate to 98 %. The product obtained is discharged into a jacketed kettle equipped with heavy plows that keep the material stirred as it cools and solidifies. The mass breaks apart into grains which are subsequently cooled, screened and mixed with anticaking agent before bagging. The particles produced by this method are suitable for munition use, but, due to the wide range of particle size distribution and the small average size, not for fertilizer use. (2) Crystallizing of ammonium nitrate is performed in continuous vacuum crystallizers. The crystals are dried in rotary dryers. The crystallization process is relatively safe, and yields products of a shape suitable for fertilizer use. The investment cost, though, is rather high. (3) Spray cooling of ammonium nitrate is the cheapest method for obtaining a dry product from the solution, both with regard to operational cost and investment. As early as 1918, a German application was filed for a patent APPLICATIONS IN THE CHEMICAL INDUSTRY 527 covering the production of particulate dry ammonium nitrate through spray cooling. For atomization, a two-fluid nozzle was applied using either cold or hot compressed air. The atomized ammonium nitrate was cooled in a chamber by means of cold air. In 1927 (313), a method for spray cooling of ammonium nitrate was patented in the United States. The atomization was effected by means of a fountain pressure nozzle, and the final product was claimed to be characterized by low density and low hygroscopicity. The bulk density was controlled by adjustment of the concentration of the ammonium nitrate solution, its temperature, and the degree of atomization. Atomization could for example be adjusted to give a diameter between 400 and 2000 micron for 95 % of the particles. After solidification, the particles were dried in a rotary dryer. A similar plant, however, provided with rotating disc atomizer instead of nozzles, was patented in 1938 (314). The rotating disc atomizer was claimed, among other advantages, to facilitate the adjustment of the particle size and thereby of the bulk density. The purpose of the above methods was to produce an ammonium nitrate powder well suited for munitions. However, in 1946 (315) the first spray cooling method for production of ammonium nitrate in granular form suitable for use as fertilizer was published. This method was called `prilling'. The concentrated ammonium nitrate solution is atomized at the top of a high tower. Falling through the tower, the droplets cool and solidify to pellets or prills when meeting cold air in co-current or counter-current flow. Figure 14.14 shows the flow sheet for a prilling plant. The concentrated ammonium nitrate solution is atomized at the top of a tall tower. The atomization can be effected by pressure nozzles adjusted to spray either upwards or downwards. In the original patent it is stated that the solution is preferably sprayed upwardly into the tower at an angle of about 45° to the horizontal. Later research work, however, indicated that this angle is not decisive and that the same result is obtainable by downward nozzle spraying f.inst. at an angle of 60° to the horizontal downward. The atomization can also be effected by rotary atomization, f.inst. by means of a rotating spray bucket. The spray bucket consists of perforations. Clogging of the holes is prevented by a blade shaped element which is rotated on the inside of the perforated wall. The concentration of the ammonium nitrate solution of 99.5-98.8 % results in high density prills (0.95 g/cm 3 ). A 95-97 % concentrate gives low density prills (0.75 g/cm 3 ). During the prilling process, very little moisture is removed. It is, therefore, necessary to after-dry the product, either in a rotary dryer, or in a fluid-bed, if the solution contains more than 0.3-0.5 % moisture. Before coating with, for example, clay to prevent caking during storage, prills are cooled in a rotary cooler, or fluid-bed. 528 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY CONC. NH4 NO3 SOLUTION ATOMIZING DEVICE AIR OUTLET PRILLING TOWER COOLING AIR COOLING AIR MEM III DRYER COOLER FINES SCREENS AMMONIUM NITRATE FRILLS TO COATING AND BAGGING Figure 14.14. Production of ammonium nitrate prills by spray cooling. Nitro-chalk, a mixture of ammonium nitrate and calcium carbonate, is spray cooled similar to ammonium nitrate. A slurry consisting of about one part ground chalk to two parts molten ammonium nitrate is atomized either by means of nozzles or a rotary atomizer. 14.6.2. Ammonium Phosphate Ammonia and phosphoric acid (free of aluminium and iron phosphates) are reacted at 120°F (50°C) in a spray absorber. The diammonium phosphate ((NI1 4 ) 2 HPO 4 ) liquor is concentrated, centrifuged and spray dried. Further addition of phosphoric acid will form the monoammonium phosphate (NH 4 )H 2 PO 4 for spray drying. The reactions are given by 529 (180-190°C), but is stable at 210-250°F (100-120°C). Diammonium phosphate will decompose at about 180°F (80°C) to ammonia and free phosphoric acid giving a sticky product. Triammonium phosphate is only stable under . pressure. Normal commercial grades of monoammoniurn phosphate contain some diammonium phosphate (= 5 %). Spray drying of ammonium phosphate produces a free-flowing low dusting product. Moisture content (3-5 %) and powder temperatures are controlled to prevent tackiness and caking in storage. In the spray drying of monoammonium phosphate, a 60 % solids feed is pre-heated to 190°F (90°C) and pumped to a co-current flow dryer. A coarse product is required, although particle size is not critical as the spray dried product is not the end product, being further granulated with other chemicals. Pressure nozzle (15 atm) or low speed rotary atomization is used. Inlet drying temperatures up to 750°F (400°C) are obtained from a direct fired gas or oil burner. Outlet temperature is in the range 230-380°F (110-195°C). High powder temperatures can cause an after-crystallization following drying leading to cakingtendency conditions. If free acid is present, the product will cake at moisture contents above 5 %. If there is no free acid, products of moisture content up to 9 % will remain free-flowing. A flow diagram with nozzle spray drying is shown in figure 14.15. Spray dried product particle size, 50 % over 300 micron, is the normal requirement, but adjustment of atomization conditions can produce coarser or finer products. Ammonium phosphates are a prime fertilizer source. NH 3 H3 P O 4 nozz H PD 3 4 (NH4 ) H 2 PO4 4 NH4 2 air 2NH 3 + H 3 PO 4 (NH 4 ) 2 HPO 4 MONO AMMONIUM . PHOSPHATE , (NH 4 ) 2 HPO 4 + H 3 PO 4 2NH 4 H 2 PO 4 Control of pH values in the recirculating liquor determines the type of ammonium phosphate formed. Monoammonium phosphate forms below a pH 5, diammonium phosphate above this value. Strict control of outlet temperature is required during spray drying. Monoammonium phosphate will decompose at a temperature of 355-375°F „ REACTORCONCENTRATOR CRYSTALS TO FLASH DRYER CENTRIFUGE SECONDARY REACTOR SPRAY DRYER Figure 14.15. Flow diagram for production of mono-ammonium phosphate by spray drying, 530 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE CHEMICAL INDUSTRY 14.6.3. Superphosphates The processing of double superphosphate features as an important application of spray drying within the phosphate fertilizer industry. Double superphosphate is the end product of phosphate rock, i.e. phospherite or apatite treatment with phosphoric acid. The principal reaction between tricalciumphosphate and phosphoric acid results in the desired monocalciumphosphate monohydrate Ca3 (PO 4)2 4 H 3 P0 4, + 3H 2 0 3CaH 4 (PO 4 ) 2 . H 2 0 The reaction mixture contains several other compounds including dicalciumphosphate, CaHPO 4 , tricalciumphosphate, Ca 3 (PO 4 ) 2 , calciumfluophosphates, CaP0 3 F. The reaction may be effected either with electric furnace phosphoric acid having a high P 2 0 5 content (about 60 %), or with wet process phosphoric acid having a lower P 2 0 5 content (30-47 %). In the latter case, the water originating from the dilute phosphoric acid must be removed, either before mixing with phosphoric rock, i.e. the dilute phosphoric acid must be concentrated, or after the initial phase of the reaction between phosphate rock and acid has taken place, i.e. the product must be dried. The steps involved in the three different methods of double superphosphate manufacture are shown in table 14.2. The reaction between phosphoric acid and raw phosphate is influenced primarily by the concentration of acid, the type and particle size of phosphate rock, the time and temperature of mixing, and the duration storage of mixture. The most significant factors are concentration of acid, and storage ti me of reaction mixture. Table 14.2. Methods of Double Superphosphate Manufacture Steps involved 1 Manufacture of phosphoric acid 2 Concentration of acid 3 Mixing of acid and rock 4 Drying of product 5 Final curing Electric furnace phosphoric acid x II III Wet process acid Phosphoric acid Acid concentrated before Product dried after reaction x X x x x x x X X 531 In order to obtain the maximum conversion of the phosphate raw material into the required phosphate form (principally monocalciumphosphate), it is necessary to store the reaction mixture for some days or weeks in a curing pile. During this period the reaction goes to completion resulting in a decreased moisture and free acid content in the final product. Many attempts have been made to develop quick-curing processes both for double superphosphates and normal superphosphates. These have been based upon curing at elevated temperatures, and applying the fact that reaction rates are increased if the dilute phosphoric acid is concentrated in contact with the ground phosphate rock. The principal features in the continuous production of quick-cured granular double superphosphate are the use of relatively dilute (39 % P2 0 5 ) phosphoric acid (this produces a fluid reaction slurry), and recirculating a very large proportion of the dried product for mixing with the reaction slurry. Figure 14.16(a) shows a simplified process flow sheet. The phosphate rock and the dilute phosphoric acid are mixed in the reaction tank at a temperature of 175-212°F (80-100°C). The slurry from the reaction tank goes to a blunger in which it is mixed with dry, recirculated fines. The blunger is discharged into the rotary dryer where the reaction—started in the reaction tank— is completed and the moisture content reduced to 2-3 Z. The product is discharged from the dryer at a temperature of 200-212°F (95-100°C). The dry product is classified as fines, finished product, and oversize. For each ton of finished product leaving the system approximately 10 to 20 tons of fines and pulverized oversize are recycled to the blunger. Recently, the procedure has been modified by the introduction of spray drying. The processing includes a spray drying stage, and differs from the process described above on two main points. Firstly, the major part of the reaction mixture (55-60 %) is spray dried and thus converted into a freeflowing powder before being mixed with the remaining reaction mixture (45-40 %). Secondly, the proportion of dry product that must be recirculated is considerably smaller. Figure 14.16(b) shows a simplified process flow sheet. The phosphate rock and dilute phosphoric acid (30-32%) are mixed in two reaction tanks at a temperature of about 195°F (90°C). From reaction tank I, the slurry is pumped to the spray drying plant equipped with a rotary atomizer, and dried in co-current flow of hot air (inlet temperature 900-1100°F (500600°C)). The spray dried powder is discharged from the dryer at a temperature of about 210°F (100°C). In the blunger, the spray dried powder is mixed with slurry from tank II and discharged into the rotary dryer. The granular product leaves the rotary dryer with a moisture content of about 3 %. .It is then classified as fines, finished product, and oversize. The oversize is pulverized and returned 532 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY PHOSPHATE ROCK PHOSPHORIC ACID spray dried powder, the granules formed in this way are more uniform than those from the process described previously, and the amount of fines and oversize product, therefore, much smaller. (b) The spray dried powder leaves the drying chamber at a temperature of 210-230°F (100-110°C). Although the drying time is short, it appears that the conversion of phosphate rock into available phosphates is accelerated at this stage. As yet, insufficient information is available on the actual operation conditions of existing plants to verify this point. Spray drying of the reaction mixture of phosphate rock and phosphoric acid presents some technological problems due to the stickiness of the product, and the possibility that the monocalciumphosphate may revert to an insoluble form through overheating. It is absolutely necessary for strict control of the air pattern within the drying chamber. The slurry is extremely abrasive and corrosive and necessitates use of special diaphragm or centrifugal pumps. Direct or gravity feed to the wear resistant atomizer wheel is used. REACTION TANK BLUNDER ROTARY DRYER HOT AIR SCRE ENS DOUBLE SUPERPHOSPHATE (FINISHED PRODUCT ) RECYCL FINES RECYCLE RATE = 10 to 20 x FINISHED PRODUCT RATE . REACTION TANK I 533 REACTION TANK II PUMP HOT AIR 14.7. Mineral Ore Concentrates SPRAY DRYER The application of spray drying to flotation concentrates is a completely new technique in the hydrometallurgical industry. In the conventional de-watering of dried concentrate preparation (figure 14.17), a vacuum filter and rotary dryer follow the thickener to produce a 7 % moisture product. BL UN DER ROTARY DRY ER b. HOT AIR — 1 THICKENER SCREENS 1 RECYCLE DOUBLE SUPERPHOSPHATE ( FIN ISH ED PRODUCT VACUUM Fl LTER 1 UNDER FLOW 70% SOLIDS Fl NES A 1 RECYCLE RATE — FINISHED PRODUCT RATE 2 Figure 14.16. Flow diagrams for the production of double superphosphate fertilizers. (a) Conventional process. (b) Spray drying process. to the blunger together with the fines. Only about 0.5 tons of fines and pulverized oversize product is returned to the blunger for every ton of finished product leaving the,system. This substantial reduction in the amount of recycled product is mainly due to the following. (a) In the blunger, and also in the first section of the rotary dryer, the slurry adheres to the surface of the spray dried product (and the returned fines) building up the granules in layers. Due to the free-flowing properties of the B SPRAY DRYER ROTARY DRYER DRIED FLOTATION CONCENTRATE 7% H 2 O DRIED FLOTATION CONCENTRATE SELECTIVE - BONE DRY TO 5% H2O Figure 14.17. De-watering operations for flotation concentrates, A. Conventional system with thickener, vacuum filter and rotary dryer producing dried concentrate with 7 % moisture. B. Spray drying system with only thickener and spray dryer producing dried concentrate with moisture selective between bone dry.and 5%. 534 APPLICATIONS IN THE CHEMICAL INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY The advent of spray drying substitutes vacuum filters and rotary dryers and produces a dried concentrate of moisture content controllable to any value between bone dry and 5 %. The spray drying system is continuous, and enables an efficient concentrate handling system from the thickener to the smelter and eliminates dust losses. The advantages of the spray dryer system have been reported recently (47) (229). Heating of the drying air in spray dryers handling flotation concentrates is by direct fired heavy fuel-oil heaters. Pulverized coal burners or coal stokers are also used, and where available, exhaust gases from diesel powered electric generators, and smelting furnaces as these then minimize fuel requirements. Co-current flow dryers utilize rotary atomizers. Flotation concentrates are abrasive and even corrosive, and the atomizer has a wear resistant wheel (figure 6.26). Dried product is discharged from the base of the drying chamber. Fines exhausted from the chamber with the air are collected in cyclones, bag filters, electrostatic precipitators, scrubbers or selected combinations of such equipment. Electrostatic precipitators are preferred where abrasiveness of the dried concentrate leads to excessive cyclone wear, or where water shortage prevents use of scrubbers. Concentrates dried to bone-dry levels are stored in silos and transferred by pneumatic handling. Concentrate of higher moisture content levels are transported by belt conveyors. FROM FLOTATI ON OPERATION THICKENER THICKENER UN DERFLOW IOR WATER I FOR REWET TI NG 1 EXHAUST AIR FEED TANK SPRAY DRYER - AMBIENT AIR - AVAILABLE WASTE HEAT CON BUSTI ON1-1MR - E =AV AIR C OO LING HEATER A IR PRODLE COLL Ec TOR ❑ .CYCLONE.SCRUBDER B BAOFILTER c ELECTROSTATIC PRECIPITATOR DRIED PRODUCT S ILO TO CHEMICAL REFINING TO FLASH SMELTER COMPACTOR (FLAKER I OR REW ET TING TO NON-DUSTING PRODUCT TO REVERBERATORY SMELTER Figure 14.18. Flow diagram for spray drying flotation concentrates. 535 14.7.1. Sulphide Ores (Copper, Nickel, Molybdenum, Tin) The flow diagram for the spray drying of sulphide flotation concentrates is shown in figure 14.18. Concentrates up to 70 % solids by weight are dried to a product of moisture content required for reverberatory smelting, flash smelting or chemical refining. Inlet drying air temperatures up to 1830°F (1000°C) are used in the spray dryer. Direct air heaters are employed. Where available, waste heat can act as a supplementary heat source, thus minimizing fuel requirements of the heater. The drying air is passed to the spray drying chamber via a central air disperser, the outlet of which is just beneath the atomizer. The central air disperser is a most effective design to handle very high air temperatures, and provide optimum spray—air contact for rapid moisture evaporation from the spray. The concentrate is gravity fed to the atomizer. Direct feed with automatic flow control at a diaphragm valve is also applicable. The exhaust air temperature from the drying chamber is controlled to a value set by the desired dried product moisture content. The spray drying system causes no measureable loss of sulphur. Primary product discharge takes place at the base of the drying chamber. Powder fines are recovered from the exhaust air in mechanical separators. On large dryers, electrostatic precipitators are installed. When cyclones are favoured, the exhaust air is scrubbed after the cyclone. The scrubber water can be recirculated via a settling tank to increase the solid content. The scrubber water is returned to the thickener, from which solids pass back into the dryer system. Operation of one of the first spray dryers on sulphide ores has been described in the literature (46). Two spray dryers each 30 ft (9 m) in diameter are reported producing 45 tons of dry concentrate per hour from a 65 % solids feed (figure 14.19). The feed is atomized by a 9 in (225 mm) wear resistant atomizer wheel rotating at 8400 rev/min. Potential applications of the above process include many minerals at present being processed by froth flotation. These minerals include lead, zinc, manganese, tungsten and silver ores. 14.7.2. Iron Ores Spray drying is becoming applied to iron flotation concentrates, replacing the conventional processing of vacuum filter and rotary dryer. Spray drying systems enable more economic and effective use of binders, and produce a superior product for pelletizing. A co-current flow spray dryer with rotary atomizer is used. The layout is similar to figure 14.18. The dried product is belt conveyed to pelletizing and sintering equipment. The underflow from the thickener can be pumped directly to the spray dryer at 72-75 % solids, or first mixed with vacuum filter cake to increase solids to 80 %. _Bentonite and limestone are added (if required) to the slurry. The binder, when added to a liquid base is normally more active than when 536 APPLICATIONS OF SPRAY DRYING IN INDUSTRY Figure 14.19, Twin spray dryer complex in Western Australia, producing bone dry nickel- concentrate. (Direct heater to right of drying chambers. Cyclones, scrubber to left of drying chambers.) (By courtesy of Niro Atomizer.) dry mixed (i.e. in the conventional process). This means savings in binder requirements. Based upon a unit weight of dry concentrate for pelletizing, binder requirements for the spray drying system can be up to 50 % lower than for the conventional system. The conventional system requires 0.31.0 % bentonite, 2% limestone addition, and dry mixing in a 'mullet.' mixer. The concentrate is dried to 5 % moisture in the spray dryer then pelletized and sintered to bone dry in a travelling grate kiln. The final product is homogeneous and completely free of 'mini-balls'. Recirculation of under/ oversize from the pelletizer is avoided. This compares favourably with the conventional process where the concentrate leaves the rotary dryer at 7 % moisture, then 2 % water is added as a fine spray prior to pelletizing. A large recirculation of fines from the pelletizer often occurs. The spray dried concentrate of 5 % moisture is optimum for pelletizing. By achieving a product of good pelletizing characteristics at a moisture APPLICATIONS IN THE CHEMICAL INDUSTRY 537 content lower than in the conventional process, the spray drying system enables reduction of the evaporative load on the sintering equipment. 14.7.3. Cryolite Cryolite is sodium aluminium fluoride (Na 3 A1F 6 ) and as a white mineral is found mainly in Greenland with lesser deposits in the Ural mountains and Colorado. It is used in the aluminium, enamel, glass and welding electrode industries. Crude cryolite has many impurities, the most important being quartz, siderite, galena, chalcopyrite, fluorspar, zinc blende and hagemannite. The removal of impurities is carried out in four stages. The mineral is crushed and the known impurities are often sorted out by hand. Ferrous materials are removed by magnetic separators. The next stages are selective grinding and screening. The hard quartz resists grinding and hence is removed during screening. The ground cryolite is further separated from the impurities by flotation techniques. The ground cryolite and accompanying minerals pass to flotation cells, where through aeration and reagent addition, one or more of the impure minerals float to the cell surface for removal with the bubbles and foam. The flotation process is repeated several times, until only the cryolite and fluorspar remain. A final reagent dosage effects the separation of the flotation cell and is removed. The cryolite suspension is spray dried and packed in bags as 94-98 % pure cryolite. Co-current flow dryers with rotary atomizers are used. The flow diagram is similar to figure 14.18. Cryolite lowers the melting point of aluminium oxide from 4000-1750°F (2200-950°C), thus enabling aluminium smelting to use standard furnaces. Although synthetic cryolite is widely used nowadays in the aluminium industry, there is still strong opinion within the industry that the natural product is indispensable especially during start-up of smelting furnaces. The natural product is the more stable and more reliable. Other uses of powder cryolite fines are in fluxes, and as filling material for grinding wheels. 14.8/14.9. General Inorganic and Organic Chemicals The vast majority of inorganic and organic chemicals that have a solid form at atmospheric conditions can be obtained from fluid feeds in suspended particle processing equipment involving an atomization chamber. Equipment design is so flexible that subject to the feed being atomized satisfactorily diverse product properties can be handled, whether it be in open, semiclosed or closed cycle dryers, spray reactors or spray coolers. The list of products given in table 13.1 cannot be considered complete. New products from day to day are being test dried successfully to increase the range of product applications. 538 APPLICATIONS OF SPRAY DRYING IN INDUSTRY 14.8. Inorganic Chemicals Inorganic chemicals fall into the following categories. 1. Aluminates 2. Arsenic compounds 3. Carbonates, Bicarbonates 4. Chlorides 5. Chlorites, Hypochlorites 6. Chromates 7. Cyanides 8. Fluorides 9. Fluorosilicates 10. Hydroxides 11. Manganates 12. Nitrates 13. Oxides 14. Phosphates 15. Silicates 16. Sulphates, Sulphides, Sulphites, Thiosulphates 17. Uranates 18. Zirconates 14.9. Organic Chemicals Some applications have already been discussed in previous sections where products in the form of dyestuffs, plastics, rubbers, resins, pesticides are mentioned. Carbohydrates and organic pharmaceuticals fall into the food and biochemical fields and are mentioned in chapters 15 and 16. Organic products form three main categories. 1. Organic acids which include amine acids, salicyclic acid, citric and maleic acids, ascorbic acid. 2. Organic salts which include phthalates, stearates, salicylates, benzoates, butyrates, gluconates, lactates, sacharates, sorbates and many others. 3. Nitrogen containing compounds, which include hydrazine, chloramines, ureas. 14.10. New and/or Specialized Applications in the Chemical Industry The products described below are given individual attention due to their special relation to suspended particle process systems that involve a chamber with an atomizer. APPLICATIONS IN THE CHEMICAL INDUSTRY 539 The products selected are Abrasives, require special atomizing and handling equipment Catalysts, require meeting strict specifications of particle size and shape Cement, a new field of application Metal powders, a new field of application Sodium carbonate, an example of spray reaction Sodium hydroxide, an example of spray cooling Titanium tetrachloride, an example of spray purification. The first four products involve the chamber as a dryer. The final three products are examples of utilizing spray drying equipment in the other suspended particle processing of spray reaction, cooling and purification. 14.10.1. Abrasives Coarse and fine grits for abrasive materials can be manufactured by spray drying grit suspensions. Abrasives require grits of narrow particle size to conform with international standards. Grit is subjected to a series of washing operations, where a suspension of finer and finer grit sizes is obtained from successive washing. The suspension can be formed into slurries by sedimentation techniques and then spray dried to give a dried product of uniform moisture and narrow size distribution. The spray drying operation is one of high temperature with inlet temperatures of the order 1000°F (550°C) and outlet temperatures 350-390°F (175-200°C). The feed slurries are particularly abrasive and require wear resistant atomizer wheels (as in figure 6.26). Use of low pressure nozzles with boron carbide inserts has also been reported (230) but monthly insert replacements were necessary. Silicon carbide is a typical abrasive that is spray dried. 14.10.2. Catalysts Spray drying is established as an important stage in the preparation of catalysts. The choice of atomizers, atomizer operation and drying chamber design enables the specific powder qualities for catalyst effectiveness to be readily obtained, whether coarse granules or fine powders are required. Spray dried products consist of free flowing spherical particles of constant bulk density, constant residual moisture, and fixed size distribution. These physical properties render the product well suited for subsequent fluid-bed processing or dry pressing into catalyst pellets. Solutions, slurries, gels or pastes of catalysts and catalyst carriers can be dried to products of closely controlled characteristics. Where the catalyst is dispersed in a toxic or inflammable solvent closed-cycle spray drying is applied. Spray dried catalysts form three important categories (a) catalysts for inorganic reactions, e.g. ammonia, hydrogen, sulphuric acid synthesis, carbon—oxygen reaction, (b) catalysts for oil and gas refining, e.g. cracking, 540 APPLICATIONS OF SPRAY DRYING IN INDUSTRY reforming, desulphurization, and (c) catalysts for organic reactions, e.g. hydration, dehydration, oxidation, polymerization and condensation. It is impossible to generalize catalyst drying as catalyst requirements are so varied. Invariably co-current or mixed flow dryers are used. Atomizer wheels, pressure nozzle or two-fluid nozzle atomization is selected after particle size requirement. Inlet temperature can be high (1110°F, 600°C) or relatively low. The development of wear resistant atomizer wheels has established rotary atomizers as the preferred atomization technique. The spray drying of silica-alumina petroleum cracking catalysts has been described by Shearon (316). General catalyst manufacture involving spray drying has been reported by Placek (317). 14.10.3. Cement The spray drying of cement slurry is an example of one of the latest applications in the heavy inorganic chemical industry although its potential has long been recognized (318). Spray drying has been incorporated in cement manufacture in two ways. (a) Modifying existing facilities to increase production (semi-wet process). (b) Rationalizing new cement plant designs (dry process). In (a) the addition of a spray dryer to an existing kiln increases the kiln capacity and improves overall heat economy. In (b) the kiln length can be substantially reduced per given cement clinker output. With a spray dryer attachment a kiln operates only as a calciner. In the conventional wet process of cement manufacture, limestone and clay are homogenized to form a 60% solids aqueous slurry. The slurry is introduced into a rotary kiln and contacted with hot combustion gases in a counter-current flow. Clinker is produced from the kiln, after the slurry has undergone three stages ; (i) moisture evaporation, (ii) vaporization of some solid components (e.g. alkalis), and (iii) calcining. The clinker passes to rotary cooling, ball milling and gypsum addition. The kiln exhaust gases pass to powder—air separation equipment for recovery of fines and alkali fraction. A spray dryer can be incorporated with the kiln, so that the kiln receives powder as well as slurry, or just powder alone. Introduction of powder increases the heat economy and output per given kiln size. In the semi-wet process applied to existing plant, figure 14.20(a), exhaust gases from the kiln are ducted to a spray drying chamber at 575-660°F (300-350°C), into which cement slurry is sprayed. The slurry is pumped to a clay/limestone/water homogenizing tank as a 60 % solids content feed and mixed with powder fines to raise solids content to a maximum 70 %. The slurry, now a paste, is atomized by a rotary atomizer with a wear resistant wheel. Nozzles can also be used (50 % solid) with effective feed filtering although anti-abrasive parts replacement is more frequent. Spray APPLICATIONS IN THE CHEMICAL INDUSTRY 541 slurry 2 130)150 C - 300350 . 0 alkali powder raw materials slurry cement gypsum max 70% TS a. b. raw mot erlots Figure 14.20. Flow diagram for manufacture of cement utilizing spray drying. (a) Semi-wet process. (b) Dry process. 1. Kiln. 2. Spray dryer. 3. Cyclone. 4. Electrostatic precipitator. 5. Homogenizer (mixer). 6. Rotary cooler. 7. Ball mill. dried powder falls as a bone dry product from the chamber base and is introduced back into the kiln towards the firing end of the kiln. Exhaust gases leaving the spray dryer pass to powder separator equipment. Cyclones, bag filters, scrubbers and electrostatic precipitators can be used. Cyclones are recommended to remove the coarse fines, with a multi-stage electrostatic precipitator to cover the finer fines and alkali content. The outlet temperature of gases from the spray dryer is adjusted to give a bone dry product 542 APPLICATIONS OF SPRAY DRYING IN. INDUSTRY and meet the needs of the fines recovery equipment. Where electrostatic precipitators are utilized outlet temperature ranges between 260-300°F (130-150°C). Powder from the cyclone and the first electrostatic precipitator recovery stage is mixed with cement slurry to form a 70 % maximum pastelike feed. The high alkali content fines are discarded, being used for fertilizer additives or land fill. The capacity of the kiln is increased by reducing the evaporative load. More 'efficient utilization of heat in the gases leaving the kiln leads to improved operating economy. In the dry process (figure 14.20(b)), only powder is passed to the kiln. This means that when designing a new plant the kiln associated with the spray dryer will be only 70 % of the length required for the wet process if the kiln were to operate under conventional wet process operation. Marked reduction in costs are possible by incorporating a spray dryer. The dry process differs from the semi-wet process since the kiln acts only as a calciner. Exhaust gases leaving the kiln are much higher leading to a more economic spray drying operation. Slurry from the homogenizing tank (60 % solids ( max. 70 %)) is pumped to a rotary atomizer (wear resistant wheel). Bone dry powder leaves the chamber. Powder recovered from the exhaust air in the cyclones and electrostatic precipitator is mixed with the chamber powder (except alkali fraction from electrostatic precipitator) and passed back to the kiln. Clinker from the kiln is cooled, ground in a ball mill and gypsum added prior to storage. 14.10.4. Metal Powders The formation of metal powders by spraying melts which are spray cooled is a new and interesting development in the field of metallurgy (319) (492). Powders can be compacted to give metal pieces improved quality. With steel powders, properties unattainable before are acquired. High speed tools do not suffer from segregation. They have very fine and uniform grain size, and high dimensional stability during heat treatment. By powdercompacting techniques, casting operations become obsolete. The scope of metal powders is immense, especially as hydrometallurgical methods are being more and more applied for extracting methods from ores, and the final product is in powder form. A steelmaking process to include the production of steel powder has been recently reported (1970) (319). Based in Sweden, the steel is melted in a high frequency furnace. The molten steel is tapped to a tundish located at the top of a spray cooling tower (30 ft (9 m) in height). The molten steel flows to two-fluid nozzles. The steel particles cool on falling through an argon atmosphere to prevent oxidation. The powder (mean size 500 micron) freely flows from the tower base to capsules ready for compaction. Compaction is first carried out at 4000 atm at ambient temperature followed by APPLICATIONS IN THE CHEMICAL INDUSTRY 543 100 atm at 2000°F (1100°C) in argon. The compacted steel billet is ready for forging or rolling in the conventional way. 14.10.5. Sodium Carbonate Sodium carbonate can be produced in a spray drying chamber used as a spray reactor (figure 0.2) (493): Interest has been growing in this process during recent years since sodium carbonate is being used in increasing amounts in detergents (replacing phosphates), and caustic soda (the starting material) is becoming more and more available as a by-product in the manufacture of chlorine by electrolysis. Liquid caustic soda (35-50 % concentration) is sprayed into a hot gas atmosphere (1110°F, 600°C) containing carbon dioxide. The caustic soda spray reacts with the carbon dioxide to form sodium carbonate. 2NaOH + CO, = Na 2 CO 3 + H 2 O The CO, rich gas can be low sulphur content combustion gases. To achieve as complete a conversion as possible the CO, content in the hot gas should not be less than about 14 % wt. Waste gases from steam boilers where fuel combustion is stoichiometric are applicable. If waste CO, is available it can be used following heating to 1110°F (600°C). Solids recovered from the chamber contain 99 % Na 2 CO 3 or better, 0-1 % NaOH and traces of Na 2 SO 4 . The moisture content is approximately 0.1 %, and bulk density 0.6 &m'. Standard spray dryer layouts are used with nozzle or rotary atomization. Vapour and combustion gases are exhausted via cyclones. Atomization is controlled to produce a granular dried product (100-300 micron). 14.10.6. Sodium Hydroxide Sodium hydroxide in pellet form is manufactured by the spray cooling process. Sodium hydroxide melt at 660°F (350°C) is atomized by low pressure nozzles to give a coarse atomization (500-1500 micron) in a mixed flow (fountain layout) or counter-current flow cooling chamber. Ambient air is introduced into the chamber. The temperature of the exhaust air is of the order 330-350°F (165-175°C) well above the critical 230°F (110°C) level. The latent heat of fusion is 126 BTU/lb (70 Kcal/kg). The product is deliquescent and requires special handling. Gravity flow feed systems are generally adopted. 14.10.7. Titanium Tetrachloride In the manufacture of titanium tetrachloride, a spray dryer is operated as a spray purifier. During the f;' - anium ore heat treatment, a gaseous mixture containing TiC1 4 , CO, CO 2 ' 2 , HCl and inerts is evolved. This mixture passes to a spray chamber at 1830°F (1000°C). Impure liquid titanium tetrachloride (impurities of iron, vanadium chlorides, etc. can reach 20 %) 544 APPLICATIONS OF SPRAY DRYING IN INDUSTRY is sprayed into the hot ingoing gases. Vaneless (plate-type) discs, rotating at low speeds (VT = 200-300 ft/sec, 60-90 m/sec) are used as atomizers. Vaned wheels are not suitable due to erosion effects on the vanes due to i mpure feeds. Nozzles are less suitable as the impurities tend to block the nozzle internal passages. The atomized sprays are relatively coarse with vaneless disc atomization, but the large droplets are readily evaporated as the liquid feed has a low latent heat of vaporization (A = 72 BTU/lb, 40 Kcal/kg). A 500 micron droplet evaporates in less than 1 second. Small diameter chambers can thus handle high feed rates. The titanium tetrachloride enriched gaseous mixture leaves the chamber and passes to condensers for tetrachloride recovery. An amount of solid material originating from the impurities in the liquid feed is recovered from the chamber base. 15 Applications in the Food Industry 15.1. Milk Products and Eggs 15.1.1. Milk Products Raw materials derived from milk are shown in figure 15.1. They are utilized in the milk powder industry to produce products that can be listed as follows : Skim milk Coffee/tea whitener Whole milk Cheese Whey Ice cream mix Fat enriched milk Butter Sodium caseinate Buttermilk Baby food Skim milk, whole milk, whey and fat enriched milk are still the most i mportant from the aspect of quantities spray dried. However, current trends show increased drying of caseinate, for use in luncheon meat, sausages and similar products, while also finding a market in special diets for those having difficulties in acquiring the daily protein requirement through normal diet. There is also increasing interest in spray dried baby foods and beverage whiteners. Spray dried cheese is widely used in the powdered soup and biscuit industries. Cream powder is an important raw material in ice cream mix, and can be successfully spray dried in spite of powders having a fat solids content between 48-70 %. Dairy products having fat contents up to 82 % have been spray dried, namely butter. Spray dried buttermilk is used as an ingredient in animal feedstuffs. The rapid growth of the milk powder industry during the last decade has evolved through the diversity of specialized purposes for which such powder can now be utilized. However, this widening range of applications has also been accompanied by the increased demand for milk powder of more 546 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE FOOD INDUSTRY stringent specifications. Recent research papers published from the milk industry have, therefore, been concerned with the definition of stable powder forms most suitable for specific production applications. These theoretical studies have been accompanied by development of processing techniques for high tonnage production of premium grade powder having special physical properties. C BUTTER BUTTER MILK 'N. Churning t 1 C SKIM MILK ) Coagulation —+ CHEESE Precipitation CASEIN WHOLE MILK Processing Solution 1C- CASEINATE R0CESSE ❑ CHEESE ) Evaporation Crystallization Separation MILK SUGAR MOTHER LIQUOR Figure 15.1. Products derived from milk. Dairies with spray dryer installations handling over a million kilograms of milk per day are nowadays by no means unique (321). Large capacity spray dryers are used, and this has led to more economic spray drying of milk. Use of inlet hot-air temperatures up to 750°F (400°C) is possible with secondary cool air introduced lower in the chamber. Without cool air, 480°F (250°C) temperature appears maximum, but lower temperatures are 547 usually used to obtain optimum powder quality. Milk is never dried with its original moisture content, but evaporated to concentrations of 45-52 % prior to spray drying. Concentration is carried out due to economics, as i about ten times cheaper in a modern evaporator than in water evaporation is a spray dryer. Furthermore a concentrate effects spray dried product quality in a positive way. A further area of high capacity drying is whey. Whey powder from fresh whey is well used in the foodstuff industry, as ingredients in powdered soups, cake mixes, baby foods. However, it is the processing of raw whey (quarg or cottage cheese whey) that has increased overall whey drying capacities. With the vast quantities produced, the pollution problem its discharge creates is a problem that must be tackled and spray drying is one possible solution. Apart from products dried in high capacities, there is a range of specialized products. Diet powder preparations, for example, can contain the daily human needs of protein, vitamins and calories. Other convenience food products are ice-cream powder, milk-cocoa powder, cake mixes and even custard powder. Spray dried milk products are redissolved or dry mixed when utilized. The important powder characteristics are flowability, wettability, sinkability, dispersability and solubility, Skim milk is dusty when in ordinary spray dried form, but recent developments in skim milk powder agglomeration have overcome these problems. Whole milk powder, with its high fat content demands quick solubility and powder flowability, and this has been accomplished by addition of additives, e.g. lecithin. Spray dried whey powder is very hygroscopic in ordinary form, but modern processing techniques are now able to produce non-caking, non-hygroscopic varieties. Drying of milk products has been reviewed recently by Noyes (322), Minifie (323), Shebler (244), Crossley (324), Hynd (489), Knipshildt (490), Antonsen (518) and Pisecky (506). (a) Skim Milk There are several ways of spray drying skim milk (329). Each is adapted to meet specified physical characteristics of powder, i.e. varying grades of agglomerated (instant) powder. Three main methods involve (a) a spray dryer with pneumatic conveying system (basic system), (b) a spray dryer with vibrated cooling bed, (c) a spray dryer with vibrated after-dryer and cooler (straight-through system). Vibrated after-dryers and coolers operating on the fluid-bed principle are hereafter termed vibro-fluidizers. Common to all methods is a skim milk concentrate of 45-52 % solids feed to the dryer, use of indirect gas/oil heaters or steam heaters. Skim milk powder contains approx. 4 % moisture. (i) Ordinary Skim Milk Powder. Ordinary skim milk powder is produced on a plant layout shown in figure 15.2(a). This is in fact the basic layout, with a 548 APPLICATIONS IN THE FOOD INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY AIR OUT ALR OUT AIR HEATER after-cooler ( vibro-fluidizer} FE D SYSTEM b. ATOHEZER Alk FeED offerdryer C. aftercooler vibro-fluidiier P R RCt TC auU Figure 15.2. Spray dryer layouts for dairy products. (a) Layout with pneumatic cooling system (basic). (b) Layout with cooling bed system (aftercooler, vibro-fluidizer). (c) Layout with straightthrough instantizer system (after dryer-cooler, vibro-fluidizer). pneumatic conveying system. Drying air is introduced at the top of the chamber around a rotary atomizer. The majority of powder leaves the conical chamber base, while entrained powder passes to the main cyclones (or bag filters). The chamber and cyclone powders are mixed and cooled in a pneumatic conveying system prior to bagging-off Skim milk powder 549 produced in such a plant consists of small single particles and is very dusty. Dissolving is difficult as the powder lumps. A typical microphoto of the powder is shown in figure 15.3(a). The high content of small particles gives the powder its dustiness, poor wettability and dispersibility, but high bulk density. The properties of ordinary skim milk powder are given in table 15.1. Nozzle atomization can be used in the basic layout. The drying chamber may differ from that shown in figure 15.2(a) as nozzles also fit in vertical towers and horizontal co-current chambers (box dryers). Pressure nozzles, similar to those shown in figure 6.33 atomize 40-50 % concentrate at pressures of 170-200 atm. Usually nozzle powder has a higher bulk density than powder from rotary atomizers. Ten nozzles are often incorporated to produce 1500 kg/hr of dry powder. However, such nozzle duplication, likely abrasion and maintenance of high pressure pumps often make the rotary atomizer the preferred technique. Skim milk powder produced from a rotary atomizer (atomizer wheel, figure 6.24(b)) can have 15-35 % occluded air, while nozzle powder has 7-13 %. Powders have a mean particle size of about 60 micron. Atomizer wheel powder can closely approach nozzle powder through increase in feed concentrate, by controlling feed temperature prior to atomization, and adjustment of atomizer speed to produce a mean particle size in the optimum range. Surface tension can affect occluded air content by its influence on particle rupture and ballooning during drying. The protein content and the state of the protein has marked influence on surface tension. The physical structure of dried milk is given by King (327) (328). (iii) Instant Skim Milk Powders. The dissolving of milk powder in water features a rather complicated mechanism. Each individual particle has initially to be wetted, then sink into the liquid in order to be finally dissolved. For a mass of particles there is the problem of dispersing them through the liquid. For skim milk powder the wettability and rate of solubility of each individual particle are very high, but when a large number of particles is present lumping occurs. Each lump is surrounded by a semi-impervious layer of milk solids, which delays the penetration of water into the dry powder within the lump. This lump formation is the reason for the poor dispersibility of an ordinary milk powder. Powder properties that are of importance for the reconstitution process can be summarized as follows : 1. Wettability. This is the ability of a milk powder particle to adsorb water on its surface, i.e. to be wetted. It is through this solids-water contact that the reconstitution process commences. 2. Sinkability. This is the ability of milk powder to sink down into the water after it has been wetted. 550 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE FOOD INDUSTRY (a) 3. Dispersibility. This is the ability of milk powder to be distributed throughout the water. This means the ability of the lumps or agglomerates to fall apart. 4. Solubility. This term is used for, two different properties : (a) The rate of dissolving. (b) The total solubility (expressed, for example, as the solubility index). During the 'instantizing' process the original single particles of the raw product (usually skim milk powder or as another food powder preparation) are transformed into porous agglomerates. When these porous agglomerates come into contact with the Water, water quickly enters the pores to wet the particles. Subsequently, the particles sink below into the water, disperse, and finally dissolve. Agglomeration alters the physical state of the powder to such an extent that the rate of wetting, sinking, and dispersing is so increased that reconstitution occurs very quickly. The powder is instant, and dissolves readily in cold water. The alteration of the physical powder conditions from single particles to agglomerates also means alteration of properties other than instant properties. For instance, there is a considerable drop in bulk density, also thermo-stability is effected. Instant milks for use in coffee and tea form an extensive market for agglomerated products, and high thermo-stability is often demanded. High thermo-stability prevents coagulation when instant milk powder is added to hot, slightly acid liquids containing tannin. However, there are markets that require a low-heat skim milk powder without 'cooked' flavour for reconstitution purposes. The basic layout (figure 15.2(a)) can be adapted to produce agglomerated powder. Agglomerated powder can be produced by incorporating a cooling bed system at the base of the chamber. Powder of 'superior' instant properties can be produced by so-called 'straight-through instant process', a special development of the vibro-fluidizer for after-drying and cooling. The vibrofluidizer is mounted at the base of the chamber. Powders produced by the cooling bed and straight-through systems exhibit instant properties. These systems produce powder in a single process directly from fresh milk and thus depend upon regular milk supplies. For processing that does not rely on milk supplies and can be operated year round, stored skim milk powder is instantized by a separate rewetting process. Rewetting gives a considerably higher degree of agglomeration . and therefore has even better instant properties than 'straight-through' powder. Four stages are involved in the rewetting process. 1. Powder is wetted with water, either in the liquid or vapour phase. The surface of the particles is uniformly wetted. 2. Wetted powder is retained in the chamber for moisture stability. The residence time is sufficient for the moist clusters to settle out at the base of the chamber. . (c) (d) Figure 15.3. Forms of spray dried skim milk powder. (a) Ordinary skim milk powder, layout figure 15.2(a). (b) Dustless skim milk powder, layout figure 15.2(b). (c) Instant skim milk powder, layout figure 15.2(c). (d) Prime rewet instant skim milk powder, layout figure 15,4. (By courtesy of Niro Atomizer.) 551 552 APPLICATIONS IN THE FOOD INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY 3. The clusters are dried, reducing the moisture content to the desired level, and cooled in a vibro-fluidizer. 4. The clusters are screened. Equipment for rewetting is termed re-wet instantizer. The re-wet instantizer forms a separate plant layout, and is not an attachment to a spray dryer. It can operate in conjunction with the spray dryer, up-grading ordinary spray dried powder. . Dustless Skim Milk Powder from Spray Dryer with Cooling Bed System. The layout is given in figure 15.2(b). The drying chamber is as in the basic layout but here the fines formed during production are returned to the atomization zone for agglomeration with the evaporating spray. Dried particles pass out of the chamber into a cooling bed (vibro-fluidizer) for powder cooling, transport and classification. The air velocity in the cooling bed is high enough to separate off the fines for return to the atomization zone, but is low enough to prevent formation of extra fines through agglomerate breakage. The powder leaving the cooling bed possesses a low dustiness and improved dispersibility. The cooling bed is used for both fat and non-fat products. A microphoto of skim milk powder produced on this layout is shown in figure 15.3(b). The extent of agglomeration can be seen typified by the presence of particle-adherence of small to large, and very low content of fines. Instant Skim Milk Powder from Spray Dryer with Straight-through Instantizer System. The plant layout is shown in figure 15.2(c). Instant powder is obtained by agglomeration in two separate stages. The initial agglomeration of fines is carried out in the atomizing zone, amidst the evaporating spray. Further agglomeration occurs within the drying chamber. The spray dryer is operated to maintain a slightly increased powder moisture content at the dryer outlet. Under these conditions the powder possesses stickiness properties which readily promote agglomeration through self-adhesion of particles. The moist warm powder passes out of the chamber base into the vibro-fluidizer for completion of drying and subsequent cooling. A microphoto of skim milk powder produced on this layout is shown in figure 15.3(c). The granular characteristics of the powder are evident. It has a coarser particle size (mean 300-400 micron) than powder from the cooling bed system. It, therefore, possesses a higher degree of wettability and dispersibility. The properties of powders produced on a dryer with pneumatic conveying system (ordinary) and straight-through system (instant) are summarized in table 15.1. Prime instant Skim Milk from Rewetting Skim Milk Powder. An improved instant product results from a further processing of powder produced on a spray dryer with pneumatic conveying system. The skim milk powder is rewetted in a vertical agglomerating tube, then dryed and cooled. 553 Table 15.1. Properties of Ordinary and Instant Milk Powders (Typical Figures) Whole milk Ordinary Moisture content 2.3 Bulk density 0.62 Solubility index 0.1 Wettability more than 10 hr Dispersibility* Skim milk Instant Ordinary Instant Rewet 2.6 0.59 0.1 40 min 46.3 g 3•8 0.64 0.1 More than I hr 4.3 0.55 0.1 10 sec 48.4g 4.0-4.5 0.28 0•I 3-6 sec >49g * Standards for Grades of Dry Milks (including Methods of Analysis, Bulletin 916), A.D.M.I., Chicago, 1965. t Mohr, W., Milchwissenschaft, 15, 215 (1960). The vertical agglomerating tube layout incorporates a surface agglomeration procedure. Surface agglomeration is accomplished by treating powder with steam or warm moist air. The surface of the individual dry particles will be wetted by condensation, thus creating the required stickiness. If contact between powder and air takes place, for instance in a vortex, agglomerates are formed. This procedure is the most suitable for skim milk, as pure milk solids require considerable mechanical impact if large porous agglomerates are demanded. The equipment is shown in figure 15.4. The powder is fed from a silo into a vertical agglomeration tube into which warm humid air is introduced simultaneously. The surface of each particle becomes moist and sticky. The particles form agglomerates of required size. The agglomerates pass into a small chamber and are contacted with drying air. The surface of the agglomerates are cooled in a vibro-fluidizer mounted at the chamber base. The dried agglomerates pass to a sieving unit from which the product is discharged with the desired particle size limits. Fines collected from the sieve are returned to the agglomerating process together with fines from the drying chamber and vibro-fluidizer. A microphoto of skim milk powder produced on a rewet instantizer is shown in figure 15.3(d). The product consists of big porous agglomerates. It is this structure which gives the product excellent instant properties. The product is also non-dusty, due to absence of fines, which gives the powder the additional advantage of having a low bulk density ( 0.3 g/cm 3 ). (For other properties, see table 15.1.) (b) Whole Milk Whole milk can be spray dried in dryers used for producing ordinary skim milk powder. A layout as shown in figure 15.2(a) is applicable or preferably the cooling bed system figure 15.2(b). The powder gains in flowability due to 554 A APPLICATIONS OF SPRAY DRYING IN INDUSTRY PPLICATIONS IN THE FOOD INDUSTRY 5 55 atomizer{ for citernistive arrangement} Gif L0 EPod INC .i .. E AIR HEATER PAOOLMT out COOLING MA Figure 154 Rewet instantizer (shown with agglomerating tube mounted), a low content of free fat resulting from the more lenient mechanical handling in the vibro-fluidizer than in the pneumatic conveying system. The fat content renders the whole milk powder particles sticky and therefore electric hammers operate at the chamber wall to prevent deposit formation. Rotary or nozzle atomization is used. Atomizer wheels with curved vanes (figure 6.24(b)) rotate at peripheral speeds between 400-500 ft/sec (120-150 m/sec). Centrifugal pressure nozzles (figure 6.33) operate in the range 100-140 atm. Whole milk concentrate of 40-50 % solids is usually dried with inlet hot air temperatures, 340-390°F (170-200°C). The final powder contains 2.5 % moisture. Whole milk powder can be instantized by the straight-through process (figure 15.2(c)) followed by lecithin addition (506). Agglomeration of whole milk powder improves its dispersibility but not its wettability. This is caused by the content of free fat in the powder which, even if in minute quantities is sufficient on migration to the surface of each particle, to render the particle water repellent (hydrophobic). The migration of fat can be prevented by physical means, i.e. the addition of small quantities of surface active agents, e.g. lecithin. Lecithin improves the wettability making the powder instant in cold water. The use of lecithin to improve on instant properties has been known for some years, but in most countries the use of additives to milk powders is not permitted. However, the International Dairy Federation has Figure 15.5. Spray dryer with vitro-fluidizer for instant skim milk, whole milk, milk replacer, ice-cream mix, cheese, cream powders. (By courtesy of Niro Atomizer.) 556 APPLICATIONS OF SPRAY DRYING IN INDUSTRY recently dealt with this problem and recommends the addition of lecithin to fat-containing milk powders (515). (c) Whey Whey has been known for decades as a product of high nutritive value, but until recently it has been considered a troublesome by-product, the majority of which has been discharged as effluent to river courses. The application of spray drying to whey and the development of markets using whey powder as ingredients in foodstuffs for human and animal consumption has transformed the dairy and cheese-making industries. There are two main groups of whey : Sweet Whey. This is also termed cheese whey and is produced during cheese making, when rennet is used. Sweet whey forms a very large family of products. Their compositions may vary only slightly but their properties are very different. The pH-value of sweet whey can range between 5.2-6.7. Sour Whey. This can be acid whey, quarg or cottage cheese whey and sour sweet whey. Acid whey, also known as casein whey, orginates from the manufacture of casein by means of lactic acid and hydrochloric acid. The origin of quarg or cottage cheese whey is self-explanatory. Lactic acid created through natural fermentation gives the whey a high acidity. The pH value of these types of whey is normally about 4.6. If insufficient care is given to the cheese whey, it becomes more sour by continued natural fermentation. Such a process is of course undesirable so that soured (not sour) whey cannot be considered a natural product. All types of whey can be spray dried. Each, however, requires its own handling techniques. Layouts for spray dried whey can vary from the very simple to the sophisticated. Generally speaking, sweet (cheese) whey is easier to dry than acid whey. The main operations used for the manufacture of whey powder are as follows : preheating—concentration—precrystallization—spray drying—after-crystallization—after-drying in a vibro-fluidizer (accompanied by a final crystallization) cooling in a pneumatic cooling system—cooling in a vibro-fluidizer (512). These operations are combined in various ways to handle the different types of whey. In all there are five important processing layouts involving spray drying. Four involve crystallization. (1) Spray Drying without Crystallization Treatment (Ordinary Whey Powder). Processing consists of a preheating, concentration, spray drying and pneumatic cooling (figure 15.6(a)). The spray dryer features a standard pneumatic conveying system similar to that shown in figure 15.2(a) for skim and whole milk powders. Nozzle atomization is vertical or horizontal (box) drying chambers can also be used. Pressure nozzles operate around 200 atm. APPLICATIONS IN THE FOOD INDUSTRY 557 Process Diagram for Ordinary Whey Powder FRESH WHEY 6% T.S. (a) Pre-heating Concentration 50 % T.S. Spray-drying 96 % T.S. Cooling of powder Bagging-off ORDINARY WHEY POWDER Process Diagram for Non-caking Whey Powder 6 % T.S. FRESH WHEY (b) Pre-heating Concentration 50 % T.S. Precrystallization Spray-drying 86% T.S. After-crystallization Fluid-bed drying 96% T.S. Cooling of powd6r Bagging-off NON-CAKING WHEY POWDER Figure 15.6. Processing stages in the spray drying of whey. Ordinary whey powder obtained by this process is very fine, dusty, hygroscopic and therefore caking. Hygroscopicity and caking are influenced by the type of whey and by local climatic conditions. The hygroscopicity, caking and all the problems associated with the stickiness of ordinary whey powder is mainly due to lactose being present in an amorphous glassy state. In the spray drying of milk products, lactose is in an amorphous state and is not stable in atmospheric air of normal humidity. The only form of lactose that is stable to humidity is a-lactose monohydrate. Since the lactose content of whey powder contains more than 70 % of the total solids in comparison with 30 % in whole milk the problem of the lactose content in whey powder is more severe. However, since the solubility of lactose is 17 g/100 cm' H 2 O at 20°C, it is easy to guide the drying process in such a way that a great part of 558 APPLICATIONS OF SPRAY DRYING IN INDUSTRY the lactose can be transformed to the stable ce-lactose monohydrate form during the drying process. (ii) Spray Drying including Crystalline Treatment. Spray drying with precrystallization. The basic process layout (figure 15.6(a)) is modified by conducting a precrystallization before spray drying. During the precrystallization process, it is easy to keep ideal conditions for crystallization. Viscosity of the concentrate is reasonably low, temperatures may be exactly adjusted and controlled, displacing of used solution from the surface of crystals may be accelerated by agitation, and the required amount of suitable crystals of lactose may be ensured by proper seeding. Furthermore, there is normally time enough for the precrystallization process so that it is no problem to reach the theoretical degree of crystallization at this stage. Crystallization of all lactose cannot be achieved in one stage and the product obtained shows only a slight improvement in the undesirable properties of hygroscopicity, caking tendencies and dustiness. Spray drying with cooling bed system. The process stages consist of preheating, concentration, precrystallization, spray drying, and cooling in a vibrofluidizer. When compared with the product described above the product from the cooling bed system is again improved. The process has the advantage of recycling fines and the resulting agglomeration reduces the dustiness of the final powder. The spray dryer layout resembles figures 15.2(b) and 15.5. Spray dryer with after drying cooling system. This process is more sophisticated, consisting of preheating, concentration, precrystallization, spray drying, after-drying and cooling in a vibro-fluidizer. The product made by this process is non-caking and being agglomerates is dustless and free flowing. The agglomerates tenti to be small and thus the bulk density is relatively high. The spray dryer layout resembles figure 15.2(c). Whey concentrate is of the order 50 % T.S. The low temperature process (non caking whey powder). This process consists of all operations as in the process above, plus further operations of aftercrystallization that takes place following spray drying (figure 15.6(b)). The drying process is guided in such a way that in addition to the 70-75 % of the lactose which can be crystallized in the whey concentrate prior to spray drying, the remaining lactose can also be converted to the stable crystalline form. This process has the advantage of being suitable for both sweet cheese and acid wheys. The spray dryer is operated to give a 12-14 % moist powder from the chamber. This is achieved by using a low outlet drying temperature. Within the moist powder the lactose is still in a state of solution and thus can migrate to the surface of the lactose crystal and crystallize there. The crystalline time needed is achieved by holding the moist powder on a conveyor belt (figure 15.7) mounted at the base of the drying chamber. Powder falls from the APPLICATIONS IN THE FOOD INDUSTRY 559 - - Figure 15.7. Spray dryer producing non-caking whey powder (after-crystallization carried out on conveyor band), (By courtesy of Niro Atomizer.) 560 APPLICATIONS IN THE FOOD INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY belt into a vibro-fluidizer (after drying-cooling) for completion of crystallization and drying. Non-caking whey powder has the following properties. It is non-caking and since the hygroscopicity is a minimum the powder is completely stable in storage. (A non-hygroscopic product does not exist since even if all the lactose is crystallized the salts and proteins possess some hygroscopicity.) The powder leaves the chamber as large agglomerates and it is possible to keep this structure when carrying out the drying process in the mechanically lenient way of the vibro-fluidizer. The product leaving the vibro-fluidizer is both dustless and instant. The large agglomerates give a low bulk density. Choice of whey process. The choice of process depends upon the type of whey available, intended market for the whey powder and plant location. The ability to handle sweet whey and yet produce a non-caking product enables use of a more simpler layout than if sour whey must be processed. If the dried powder is intended for dry powder mixes, fiowability is essential and the process must be equipped with crystallization and cooling stages to ensure this property is obtained. Local climate should also be considered. If the climate is too humid, it is advisable to use a process that produces a less hygroscopic product having low caking tendencies (d) Fat Enriched Milk (Milk Replacer) Fat enriched milk is a replacement for whole milk in which the butter fat has been replaced by a cheaper animal or vegetable fat. In recent years there has been increasing interest in utilizing skim milk powder enriched with animal and/or vegetable fats for feeding of calves, pigs, lambs and other domestic animals. •For calves it has been used for both breeding and fattening. A special powder composition is used in each case. A number of products have been manufactured. Feeding trials with these products have shown that they can be used successfully and economically as whole milk substitutes, particularly in the case of rearing veal calves. The first products of this type were manufactured by simple mixing of the ingredients. This method is still used, but gives numerous problems as the entire fat content is in the state of free fat (directly extractable by organic solvent), which adversely effects both the digestibility and shelf life of the product. The process usually applied today is an emulsifying of the fat in the skim milk. In this way, the fat is protected by the milk solids and does not show the disadvantages mentioned above. In general the melted fat is mixed with preconcentrated skim milk. The mixture is homogenized prior to spray drying. Fat enriched skim milk feed for calves usually contains 15-20 % fat. The fat content of the reconstituted milk will thus be 2-3 %. The composition of . 561 the marketed fodder varies a great deal according to the purpose of animal feeding. A calf fodder, for example, is 15-20 1. Fat 50-80 2. Skim milk solid (milk solids non-fat, MSNF) 0-30 3. Dextrose, lactose, possibly whey solids 4. Emulsifying agents (lecithin, mono-glycerides, succro0-2 glycerides, etc.) 0-7 5. Flour 6. Minerals (chlorides, phosphates, bicarbonates of Ca, Na, Mg, Cu) 0-0.5 % 0-0.5 7. Vitamins A, D, E (B, C) trace 8. Antibiotics (terramycin, aureomycin) Powder Production by Spray Drying an Emulsion of Skim Milk Concentrate and Fat. The method produces the so-called premix. A premix contains up to 60 % fat in the total solids content. This is much higher than is desired in the finished fodder mixture. Normally a lower fat content mix is produced by dry mixing to meet the strict quality specifications. A higher fat content cannot meet such standards. Pasteurized skim milk with a titratable acidity below 0.19 % lactic acid is concentrated to 42-45 %. The exact concentrate solids content depends upon the amount of fat to be added later in the process. Skim milk leaves the evaporator at about 110°F (45°C) and is preheated to 150-160°F (6570°C). Fat is then added. Fat must be of first class quality with free fatty acid content less than 0.4 % (as oleic acid) and a very low content of impurities and water. Prior to use the fat is stored at temperatures not exceeding 120°F (50°C). Antioxidants are generally added (13utylhydroxytoluene (BHT), Nardihydroguajaretic acid (NDGA)). If emulsifiers are required, they are added_ at this stage. Lecithin and monoglycerides are usually used. Fat is then heated to the same temperature as the milk concentrate. Appropriate amounts of skim milk concentrate and fat are mixed while undergoing stirring. The ratio between fat and skim milk concentrate is selected so that the fat content in the powder obtained from the spray drying plant lies between 40 and 50 %. The mixing of fat and skim milk concentrate can be carried out either batchwise or continuously. The mixture is homogenized prior to spray drying. The purpose of homogenizing is to divide the fat globules and make them more easily digestible for the animals. The aim is a maximum size of fat globule (3 micron) and a minimum of 90 % less than 1 micron. Homogenizing causes an increase in viscosity and care must be taken to prevent formation of too viscous a feed which will later cause atomization and poor drying conditions. Emulsifiers can reduce viscosity increase, but excess use can cause deposit formation in the spray drying chamber. 562 APPLICATIONS IN THE FOOD INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY Batch mixing is performed volumetrically but continuous mixing is mostly adopted nowadays, Milk concentrate and melted fat are delivered from the evaporator and melted fat tank storage. The milk and fat are best supplied by a triple piston pump. One piston supplies milk, the second fat, and the third emulsifier (if required). The proportioning between fat and skim milk concentrate can be adjusted by changing the stroke of each piston. The milk and fat is pumped into a combinator for product heating and mixing, and then to the homogenizer, which also acts as the feed pump to the spray dryer. A co-current flow spray dryer with a conical chamber base is used. Chambers having flat or slightly conical bases are not suitable as the product is warm and sticky. Use of scrapers create lumps and free fat formation. Inlet drying air temperature is usually in the range 320-390°F (160-200°C). A cooling vibro-fluidizer is mounted at the base of the drying chamber. Ambient or refrigerated air is used. Powder from the cyclones is transported by a vibrated conveyor to the vibro-fluidizer. The cooled powder is sieved before packing. Before marketing, the spray dried powder (i.e. premix) is blended with other powders and additives, e.g. skim milk powder, whey powder, vitamins, antibiotics (antidiarrhoeatics). The blend depends upon the purpose to which it is intended, i.e. feeding of calves, pigs, or lambs. The content of fat in the final product is normally between 15 and 28 Z. In many countries, the authorities request the addition of a tracer in order to provide against abuse, and to prevent the product from being introduced onto the market as ordinary whole milk powder. (e) Sodium Caseinate The preparation of sodium caseinate feed for spray drying can be from either fresh wet casein curd or dried casein (491). The liquifaction of casein in alkali is performed by either batchwise or (more recently) continuous methods. In the batchwise method, casein, water and alkali are fed to a heated vessel equipped with an agitator. The contents of the vessel is pumped through a colloid mill and back to the vessel. The process usually takes 1-4 hr per batch. In the continuous method, wet curd (produced continuously) is the raw material. The curd is mixed with water to give the proper solid content, then passed through a colloid mill and mixer. The mixer is also supplied by sodium hydroxide and steam (figure 15.8). On leaving the mixer, the mixture composition is controlled continuously by pH, temperature and viscosity measuring equipment. The sodium caseinate solution has a high viscosity and this usually limits solids content in the feed to the spray dryer to 22-25 Z. This low solids content leads to a low bulk density product (^ 0.3 g/cm 3 ) with a high occluded air content. To increase the bulk density and reduce occluded air, the spray dryer is operated at the highest feed solids the rotary atomizer can handle, and powder leaves 563 WATER SODI UM C AS El NA T E POWDER 1. Feed pump 2. Mixing aggregate 3. Mill 4. Mixer 5. Dosification pump 6. PH meter controller 7. Temperature controller 8. Viscosity meter controller 9. Intermediate tank 10. Feed pump 11. Spray dryer 12. Flash dryer 13. Pneumatic cooling section Figure 15.8. Flow diagram for the production of spray dried sodium caseinate. the chamber moist. An after-drying is required, and this is accomplished in a flash dryer. Heated filtered air enters the horizontal vortex section tangentially, picks up the moist powder and passes into the vertical section. Moisture removal is completed and the powder is recovered in cyclones for normal pneumatic conveying to bagging-off. Pneumatic conveying cools the powder. Powder recovered from the exhaust spray dryer air is returned to the central part of the flash dryer. Sodium caseinate produced in this manner has a powder density of 0.45-0.50 g/cm 3 . Uses of sodium caseinate include luncheon meats and sausages, coffee/tea whitener, diet foods and other special foodstuffs. 564 APPLICATIONS OF SPRAY DRYING IN INDUSTRY (f) Baby Foods Dried milk based baby foods, that closely resemble breast milk when reconstituted are sold extensively nowadays. The dried powder is prepared for packing by spray drying. Preconcentrated skim milk is mixed with mineral and vitamin. additives and certain animal or vegetable fats in strictly controlled proportions. Carbohydrates and whey proteins are also used. The fat chosen is more easily dealt with by the limited digestive power of a new born baby or young infant than the fats present in normal cows milk. The mixture is pasteurized carefully, and spray dried. The powder is often packaged in tins under ultra-violet light to maintain a low bacteria count. Long shelf life is obtained by packing in an inert atmosphere of nitrogen. Baby foods can be instantized using the straight-through or rewet systems. The rewet system differs slightly from the layout shown in figure 15.4. A rotary atomizer replaces the agglomerating tube. The powder is sprayed with a fine mist of water or solution of required additive. Powder is moistened to 8-10 % prior to entering the vibro-fluidizer. This form of wetting gives droplet agglomeration of powder. The agglomeration process is not so forceful as surface agglomeration, and smaller agglomerates are formed. (g) CoffeelTea Whiteners Whiteners for addition to coffee and tea are widely used as a cream substitute of excellent keeping quality. Based upon sodium caseinate, corn syrup, vegetable fat, emulsifying agent, potassium phosphate and sodium silicoaluminate, the feed can be handled using straightforward spray drying procedures. Whiteners can be instantized successfully using a straightthrough system or by rewetting (involving droplet agglomeration). (h) Cheese Melted processed cheese is normally used in spray drying. Formally only cheeses with imperfect structure were used but nowadays demand for cheese powder is such that cheeses are produced solely for spray drying. There are no particular difficulties in spray drying cheese. The cheeses are crushed and mixed with water to form a smooth cream. This is atomized (atomizer wheel) in a dryer with a conical chamber base. There are limited chamber wall deposits due to the high fat content in the cheese. Inlet air temperatures are of the order 350°F (175°C). Low outlet temperatures are used for maximum retention of flavour. Cheese powders cannot be handled successfully in a pneumatic conveying system, and a cooling bed is preferred at the chamber base. For dryers in residential areas, deodorizing equipment (active carbon) is required to treat the 'exhaust air. Alternatively a semiclosed cycle system can be adopted where part of the exhaust air is used as combustion air in an indirect air heater. Passage through the heater destroys the odour in the exhaust air. APPLICATIONS IN THE FOOD INDUSTRY 565 (i) Ice-cream Mix Ice-cream is essentially a frozen aqueous emulsion of fat, dairy and non-dairy solids, sugar, flavourings, stabilizers and colours. Dairy ice-cream mixes include butter fat, skim milk solids, sucrose or corn syrup solids as main ingredients. Vegetable fat replaces butter fat, and sodium caseinate replaces skim milk solids in non-dairy ice-cream. Moisture contents are 1-2 %. Ice-cream mixes are difficult to spray dry due to high contents of sugar (up to 30 %). It is usual to dry the mix with only part of the sugar in the liquid feed. The remaining sugar is added after drying by dry mixing. Special equipment is available to handle the total sugar content. The remaining sugar is added to the dryer via a fines-return system. The straightthrough instantizer process is then used. The ice-cream mix is obtained as a dustless, non-caking powder. (j) High Fat Powder for Bakery Use (also Butter) The drying of products containing 60-80 % fat requires overcoming the problem of easy rupture of the fat protective membrane (usually protein), that leads to fat release. This rupture is prevented by minimizing the mechanical handling of the powder, especially while still warm, or increasing the melting point of the fat. Conditions of lenient handling are obtained by incorporating a cooling bed system at the base of the chamber. Alternatively the air in the base of the drying chamber is cooled by secondary air to prevent melting of chamber powder, and solidifying particle surfaces prior to mechanical handling. Where cyclones are used as a powder collector, cool air is often introduced prior to the cyclones to prevent product melting. The cyclone powder has a quality inferior to that of the chamber powder. Increasing the melting point of many vegetable and animal fats is practiced, but for a product such as butter this is not practicable due to loss of flavour and the strict specifications of what butter may contain. Studies on spray drying of high fat food products has been reported by Amundson (330). (k) Buttermilk Spray drying sweet and acid buttermilk overcomes the problem of disposing any excess that is not consumed in liquid form. Buttermilk cannot be discharged due to effluent problems, or be mixed with skim milk due to coagulation. Spray dried powder can be used as an ingredient in animal feeds. Sweet buttermilk presents no difficulties in spray drying. Dryers for skim milk are used. Buttermilk is concentrated to 45-50 % and dried in cocurrent flow dryers with pneumatic powder conveying. The moisture content of the powder is around 4 %. Acid buttermilk presents no difficulties in spray drying but preconcentration requires special attention. The buttermilk acidity (due to addition of lactic acid bacteria starter during butter-making) is in the range 4.5 and coagulation 566 APPLICATIONS OF SPRAY DRYING IN INDUSTRY APPLICATIONS IN THE FOOD INDUSTRY of casein occurs. The buttermilk viscosity is high and there is danger of scorching on the heat surfaces of the evaporator. Buttermilk and concentrate temperatures are kept low (134.5-136°F, 57-58°C). There must be no high temperatures in the first effect of the evaporator, or pasteurization. The circulation in the first and second effects is carried out as lower temperatures result in low capacities. Ordinary evaporators concentrate to 25 %. Special types with a de-gassing stage concentrate to 36 %. The concentrate is highly viscous and is pumped (110°F, 43°C) to the spray dryer. (Skim milk dryer designs are applicable.) Inlet drying temperatures are in the range 350-375°F (175-190°C). Light deposits occur in the chamber, but use of low outlet temperatures prevents discolouration. The powder on packing is cream coloured and consists of small particles. The moisture content is held around 4 %. The tapped bulk density is 0.77-0.83 g/cm. 3 15.1.2. Eggs Whole egg, egg yolk and white (albumen) are spray dried commercially (513). Although egg white and egg yolk powders have very different characteristics, spray dryers of similar designs can handle both types successfully. However, for cleaning purposes, it is recommended to have a dryer for each product group, e.g. one for whites and one for whole eggs/yolks. The flow diagram for processing eggs is shown in figure 15.9. Eggs are supplied from cold storage (40-60°F, 5-15°C) unpacked and weighed. F RH ENTATIDN TANKS DUALITY CONTROL FRESH EGGS W OLE EGG CANDLING STABILIZING BREAKING STORAGE HOMOGENIZING SPOILED AND . BROKEN EGGS COOLING or HE AT IN G SPRAY DRYING HOLDING TANK HOLDING TANK FE ED TANK PASTEURIZER EGG POWDER Figure 15.9. Piocessing diagram for production of egg powders. 567 Rotten eggs are removed by candling. Dirty eggs are removed to a washing machine equipped with detergent sprays, then fan dried and returned to the candling machine. The eggs are broken. This is often done by hand, as the operation is easy. Presence of an operator allows a further chance to remove any rotten eggs that failed to be detected during candling. If the egg whites and yolks are to be separated, a cup and ring device facilitates separation. A skilled operator can break 500-800 eggs per hour. In spite of this high rate fully automatic breaking and separating machines have been developed and are established in the industry. Up to 18 000 eggs per hour can be handled per machine when separating whites from yolks or when breaking without separation. All egg shells contain small amounts of whites, and this is recovered by centrifuging the shells. For processing egg whites, efficient separation of whites from yolks is of great importance as no yolk must contaminate the whites. Even a small amount of yolk oil in albumen greatly reduces the whipping quality. Nevertheless modern machines are able to achieve limits of not more than 0.02 % yolk oil in egg white, and this is acceptable. In the production of whole egg/egg yolk powder, whole eggs/egg yolk are homogenized, filtered to remove chalazae, membranes and any shell, and pasteurized. Pasteurization (normally 147-151°F, 64-66°C, holding time 2-4 min) ensures the desired microbiological requirements that are usually a total count less than 100 000 col/g absence of B. Coli and Salmonella. For whole egg especially, pasteurization conditions are precisely chosen and maintained to obtain desired powder characteristics without affecting baking performance. Whole eggs (solids content 25-27 %) or egg yolk (solids content 45-48 %) are fed to the spray dryer. Co-current flow dryers with rotary or nozzle atomization are used. The drying air inlet temperatures range between 290-390°F (145-200°C). Powder moisture content is 2-4 %. The powders are conveyed pneumatically in ambient air to the packing area. Powder airborne in the exhaust drying air is recovered in cyclones. For improving the shelf-life of egg powders, a fermentation process can be used to remove glucose. Thus discolouration and development of disagreeable smell during powder storage is avoided by preventing the so-called `Maillard' reaction,. which proceeds between glucose and proteinamino groups. Nevertheless, fermentation is not very common in the production of whole egg and egg yolk powders. On the other hand, it is currently used for egg albumen. Egg albumen is fermented by means of bacteria, yeast or enzyme (glucoseoxidase) to reduce the content of glucose below 0.1 %. The performance and conditions of fermentation vary considerably from factory to factory. This also applies to conditions of pasteurization. Normally stabilizing salts 568 APPLICATIONS IN THE FOOD INDUSTRY APPLICATIONS OF SPRAY DRYING IN INDUSTRY are added to prevent heat damage, and temperatures around 133-138°F (56-59°C) are used for several minutes. Prior to pasteurization, egg albumen is filtered to remove chalazae, and foam created during fermentation. A 1012 % solids feed is spray dried in co-current flow dryers with either rotary or nozzle atomization. Drying air inlet temperatures range between 290390°F (145-200°C). Dried egg albumen contains normally 7-9 % moisture. Pneumatic powder conveying is adopted. Powder airborne in the exhaust drying air is recovered in a battery of high efficient cyclones or bag filter. Egg powders are attractive in appearance and fully soluble. They are packed in plastic bags, plastic lined boxes, tins or cartons. Whole egg/egg yolk powder is much denser than egg white powder. The lightness of egg white powder is due to the low solids content in the feed. Denser powder can be produced if the solids content is increased. Vacuum evaporation can be adopted, but the most promising technique for future egg white drying is the use of reverse osmosis where feeds up to 25 % solids appear attainable. 15.2. Beverages, Flavouring Compounds, Meats, Protein from Vegetable Sources 15.2.1. Beverages (a) Instant Coffee The history of instant coffee powder dates back many decades and the product has been commercially produced during the past fifty years. However, intensive development did not start until some ten years ago, but during this fairly short period, the quality of spray dried coffee has been improved and the product enjoys an extensive consumer market. In the production of instant coffee, process stages of roasting, granulation and extraction proceed spray drying. A typical flow diagram is shown in figure 5.10. The raw coffee on delivery is used immediately or stored in bags. An additional method is to transport the green coffee to.collecting bins and silos. Raw coffee for use in the production of instant coffee is first cleaned to remove wood, leaves and other foreign matter. Cleaning is carried out in a cyclone system and a set of vibrating sieves. Following cleaning the raw coffee passes to silo storage. As various types of coffee are used in manufacture, there is a silo for each type. The basic material for instant coffee production is a green coffee mixture. Blending equipment ensures uniform mixture of the desired blend. The following roasting stage is vital to taste, colour and overall quality of the product. Both continuous and batchwise roasting techniques are fully developed with varying degrees of automation. Full automatic control of mixing and roasting is the usual requirement. Combustion air from gas or fuel burning heaters is used for roasting. Loss in coffee bean weight during roasting is around 14-20 % (dry matter basis). 569 GREEN COFFEE BEANS NOZZLE ATOMIZER ASSEMBLY EXHAUST AIR • FINES TO ATOMIZATION ZONE POWDER TO AIR-CONDITIONED FACI•OND AREA 1. Pneumatic conveyor 2. Cleaner 3. Pneumatic conveyor 4. Silos 5. Blending scale 6. Roaster 7. Cooling screens 8. Stoner 9. Scale 10. Bucket conveyor 11. Silo for roasted beans 12. Magnetic separator 13. Granulator 14. Weighing unit 15. Crane beam 16. Feed hopper SPENT GROUNDS 17. Semi-continuous (batch) extraction battery 18. Continuous extractor 19. Water treatment plant 20. Clarifier 21. Cooler 22. Scale tank 23. Storage tank/feed tank 24. Bulk density regulator 25. High pressure unit for feeding extract to dryer 26. Co-current flow spray dryer (nozzle tower) 27. Cyclones 28. Vibrating cooler 29. Scale 30. Hoppers Figure 15.10. Flow diagram for production on instant coffee powder by spray drying. The roasted product is transported to a silo and afterwards to a granulator. The purpose of grinding is chiefly to obtain a particle size suitable for the subsequent extraction. This particle size may vary for the different types of extraction equipment. Principally, the larger the surface of a given amount of coffee, the faster and/or more thorough will be the extraction. However, this indicates a very small particle size to be desirable, yet a too finely ground 570 APPLICATIONS OF SPRAY DRYING. IN INDUSTRY coffee will pack too tightly and cause mechanical difficulties during extractor operation. Grinding is controlled to produce granulized roasted coffee particles of size between 1000-2000 micron with a very small percentage of 'fines'. The extraction of roasted and ground coffee takes place in three steps; wetting, solubles extraction, and solubles formation by hydrolysis. The particles are first wetted and selectively absorb an amount of water from the extract equal to about double their dry weight. This causes a raise in extract concentration and gases are evolved from the particles. The soluble matter in the particles dissolves and as the concentration of solubles in the surrounding extract is lower than the concentration in the solution within the particle, the solubles diffuse towards the surface. In order to secure the highest efficiency, the mean concentration differences must be kept as high as possible. Hence counter-current extraction principles are used. Any back-mixing in either extract or grounds streams decreases the efficiency. Fluctuations in the speed of the stream