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Integration and Optimization of Unit Operations
This page intentionally left blank
Integration and
Optimization of Unit
Operations
Review of Unit Operations from R&D
to Production: Impacts of Upstream and
Downstream Process Decisions

Edited by
Barry A. Perlmutter
President, Perlmutter & Idea Development LLC, Matthews, NC, United States
Elsevier
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The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, United Kingdom
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This book and the individual contributions contained in it are protected under copyright by the Publisher (other
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Typeset by STRAIVE, India

Contents

Contributors xiii 2.8.2 Continuous sterilization 47

About the editor xv 2.8.3 Filter sterilization of liquids 53
Preface xvii 2.8.4 Filter sterilization of air 56
2.9 Heat generation 56
1. Crystallization 2.10 Scale-up 59
Nomenclature 64
Brooke Albin
References 65
1.1 Fundamentals and laboratory scale
process development 1
1.1.1 Crystallizer design basics 1 3. Fermentation and downstream
1.1.2 Crystallizer design tradeoffs 4 processing: Part 2
1.1.3 Upstream variables affecting
Alan Gabelman, Ph.D., P.E.
crystallization 6
1.1.4 Impact on downstream 3.1 Fermenter design 69
operations 7 3.1.1 Fermenters without mechanical
1.2 Pilot scale crystallization studies 8 mixers 73
1.2.1 Objectives for a pilot plant 8 3.2 Fermenter instrumentation, control and
1.2.2 Scale-up criteria 9 operation 75
1.3 Commercialization of crystallization 3.2.1 Temperature 77
processes 10 3.2.2 pH 78
References 11 3.2.3 Dissolved oxygen
concentration 79
2. Fermentation and downstream 3.2.4 Mixer speed 80
processing: Part 1 3.2.5 Pressure 80
3.2.6 Gas flow rate 81
Alan Gabelman, Ph.D., P.E.
3.2.7 Liquid flow rate 82
2.1 Introduction 13 3.2.8 Foam 83
2.2 Microbiology and biochemistry 3.2.9 Exit gas composition 85
basics 13 3.2.10 Level 86
2.3 Fermentation media and 3.2.11 Substrate concentration 87
environment 21 3.2.12 Power input 88
2.4 Growth kinetics and substrate 3.2.13 Redox potential 89
utilization 24 3.3 Continuous culture 89
2.5 From vial to production fermenter 27 3.4 Downstream processing 93
2.6 Oxygen transfer and utilization 29 3.4.1 Monosodium glutamate 94
2.7 Mixing in aerobic fermentation 3.4.2 Phenethyl alcohol 100
vessels 37 3.5 Concluding remarks 108
2.8 Sterilization 43 Nomenclature 108
2.8.1 Batch sterilization 46 References 109

v
vi Contents

4. Liquid filtration 6.4.2 General operation 141

6.4.3 Safety interlocks 142
Jose M. Sentmanat
6.4.4 Out of balance monitor 142
4.1 Do you need a filter? 113 6.4.5 Plough parked 142
4.2 Lab testing before you choose the 6.5 Final remarks 142
filter 113
4.3 Choosing the filter 116
4.3.1 Plate and frame filter press 116
7. Dryers
4.3.2 Filter presses 116 Hongben Zhou
4.3.3 Plate filters 117
7.1 Purpose of drying 145
4.3.4 Pressure leaf type filter 117
7.2 Dispersed solid-liquid system 145
4.3.5 Nutsche filter 118
7.3 Drying processes 147
4.3.6 Polishing filter 118
7.4 Convective drying with hot gas 147
4.4 The ABCs of liquid filtration 118
7.5 Conductive and radiative drying 150
4.5 The mechanics of liquid filtration 119
7.6 Evaporation of liquid from a solid
4.5.1 Precoat 119
packing 151
4.5.2 Filtration 120
7.7 Drying facilities 153
4.5.3 Cleaning 120
7.7.1 Grain-sunning ground 153
4.5.4 Standby 121
7.7.2 Tray dryer 154
4.6 Troubleshooting 121
7.7.3 Belt dryer 156
4.7 The filter cake 121
7.7.4 Rotary dryer (kiln) 156
4.8 Preventative maintenance program 122
7.7.5 Fixed bed dryer 159
Further reading 123
7.7.6 Fluidized bed dryer 161
7.7.7 Pneumatic conveyor as dryer 162
5. Cake-building filter technologies 7.7.8 Spray dryer 165
Jose M. Sentmanat and Barry A. Perlmutter 7.7.9 Impact mill as dryer 166
7.7.10 Rotating vessel dryer 168
5.1 Batch processing of filter cakes 125
7.7.11 Plate dryer 168
5.2 Contained filter presses for cake
7.7.12 Roller dryer 170
washing, dewatering, and drying 126
7.7.13 Screw conveyor as dryer 170
5.3 Nutsche filter and filter dryers 127
7.7.14 Agitated mixer as dryer 171
5.4 Continuous processing of filter cakes 128
7.8 Troubleshooting 174
5.4.1 Vacuum belt filters 128
7.8.1 Heat transfer 174
5.4.2 Horizontal vacuum belt filters 129
7.8.2 Level of vacuum 175
5.4.3 Rotary vacuum drum filters 131
7.8.3 Formation of agglomerates and
5.4.4 Rotary pressure filter 131
crust 175
5.4.5 Pressurized vacuum drum
References 176
filter 131

6. Centrifugation 8. Pressure filter dryer

Badrie Luckiram, BSc, MSc, CEng, MIChemE Badrie Luckiram, BSc, MSc, CEng, MIChemE
6.1 Centrifuge choice and analysis of 8.1 General considerations of using a
available equipment 133 pressure filter dryer 177
6.1.1 Horizontal basket centrifuges 135 8.1.1 Pharma-specific
6.1.2 Vertical basket centrifuges 135 considerations 178
6.2 Typical centrifuge operation 138 8.2 Principles of the pressure filter
6.3 Technical considerations of equipment dryer 179
selection 138 8.3 Filter choice and analysis of available
6.3.1 Design basis document 138 equipment 182
6.4 Other considerations of centrifuge 8.3.1 Selection of filter dryer type 182
operation 141 8.4 Technical considerations of equipment
6.4.1 Centrifuge inerting 141 selection 183
 Contents vii

8.5 General operation of a pressure filter 10.1.2 Identify key automation systems
dryer 183 and technology 219
8.5.1 GMP issues and cleaning 189 10.1.3 Identify advanced control
8.5.2 Filter safety interlocks 189 schemes 220
8.5.3 Operational issues 190 10.1.4 Estimate system size 221
8.6 Final remarks 190 10.1.5 Site planning overall
philosophy 221
9. Process automation systems 10.2 Front end engineering design 226
10.2.1 Basic automation
Nick Harbud
requirements 226
9.1 Process automation in production 10.2.2 Advanced process control 226
facilities 191 10.2.3 The MAC, and why you should
9.2 Process control system use one 226
(continuous process) 191 10.2.4 Other automation systems 227
9.2.1 Controlling the process 191 10.2.5 Functional safety 228
9.2.2 Operating the plant 193 10.2.6 Change management for
9.2.3 Integrating automation process automation 228
systems 194 10.3 Delivery phase, detailed engineering,
9.2.4 Enterprise interfaces 195 and procurement 229
9.2.5 Types of process control 10.3.1 Process automation design
system 195 documentation 229
9.3 Process control systems 10.3.2 Automation system design
(batch process) 197 and software configuration 230
9.4 Safety instrumented systems 201 10.3.3 Factory acceptance testing 230
9.4.1 Identifying the hazards 203 10.3.4 Shipment and site
9.4.2 Assessing the risks 203 preservation 231
9.4.3 High integrity pressure protection 10.4 Installation and commissioning 231
systems 205 10.4.1 Manpower plan 231
9.4.4 Cybersecurity risk assessment 206 10.4.2 Infrastructure and overheads
9.4.5 Validation and proving 206 plan 232
9.5 Alarm management systems 207 10.4.3 PAS media plan 233
9.6 Machinery protection 209 10.4.4 PAS change management
9.6.1 Vibration monitoring system 209 plan 233
9.6.2 Compressor and turbine control 10.4.5 PAS security plan 233
systems 209 10.4.6 PAS integration plan 233
9.7 Measurement, and other fun things to 10.4.7 PAS maintenance plan 234
do with instruments 212 10.4.8 PAS user administration
9.7.1 Diagnostics—Is it working? 213 plan 234
9.7.2 Control in the field 214 10.4.9 PAS turnover plan 235
9.7.3 The growth of digital 10.5 Automation system operation and
communications protocols 214 obsolescence 235
9.7.4 HART 214 10.5.1 Hardware maintenance
9.7.5 Fieldbus 215 and obsolescence 235
9.7.6 Ditching the wires 216 10.5.2 Software maintenance and
9.7.7 Instrument asset management change 235
systems (IAMS) 217 10.5.3 Disaster recovery 236
9.8 The effect of technology on process 10.6 Conclusion 237
automation 217

10. Process automation life cycles 11. Process automation platforms

Nick Harbud Mike Williams
10.1 Planning for process automation 219 11.1 Background 239
10.1.1 Operations and maintenance 11.2 Staffing of a manufacturing facility 239
philosophy 219 11.3 Finding the balance 240
viii Contents

11.4 The new paradigm of autonomous 12.10.2 The new way: Break the
operations 240 paradigm 269
11.5 Upgrading the level of automation 245 12.10.3 What was saved? 270
11.6 Where to start when considering 12.10.4 In conclusion: Every
investment in higher levels of perspective matters 271
autonomy 246 12.11 Final remarks 271
11.7 Conclusions 247 References 271
Further reading 271
12. Mixing and blending
13. Process development and
Stephanie Shira integration by mathematical
12.1 Introduction: Why mixing modeling and simulation tools
matters 249 Nima Yazdanpanah
12.2 Upstream considerations 249
12.2.1 Before the shafts 250 13.1 Fundamentals and workflow 273
12.2.2 The first shaft 250 13.2 The steps for building a mathematical
12.2.3 Distributive vs dispersive model 275
mixing 253 13.3 Steady-state and dynamic
12.3 The second shaft 254 simulations 277
12.3.1 High speed dispersion and low 13.4 Process simulation for
speed scraping: The traditional optimization 277
dual-shaft mixer 254 13.4.1 Construction of the optimization
12.3.2 More intense dispersion problem and its
(double the shafts, quadruple components 279
the blades of a traditional 13.5 Process development workflow for
disperser): The dual-shaft continuous manufacturing 280
disperser 255 13.5.1 Process integration and steady-
12.3.3 Dual-shaft disperser case study state simulation 281
and performance review 258 13.5.2 Dynamic process modeling
12.4 The third shaft 258 and control 283
12.5 Additional mixer design 13.6 Correlation between CQAs, CPPs,
considerations 258 CMAs 286
12.6 Rheology considerations 260 References 292
12.7 Overmixing is just as bad as
undermixing: Know the finishing 14. Process safety
point 261
Kaushik Basak
12.7.1 Kitchen connection 261
12.7.2 Case study: “Pancake lumps” 14.1 Lab-scale operations 293
on the production floor 261 14.1.1 Safety and hazards 293
12.7.3 Compensating behaviors result 14.1.2 Key issues for lab-scale
from inadequate products 262 operation 294
12.8 Reliable scale-up 262 14.2 Pilot plant operations 297
12.8.1 Hydraulic ram discharge 14.2.1 Safety and hazards 297
press 263 14.2.2 Key issues for pilot plant
12.9 Mechanical aspects and operations 299
troubleshooting 264 14.2.3 Pilot plant sizing, issues,
12.9.1 Blade health 264 decisions, and trade-offs 301
12.9.2 Understanding shear (rates and 14.3 Production scale operations 303
flow regimes) 265 14.3.1 Safety and hazards 303
12.10 Case study: Why push toward 14.3.2 Key issues for production scale
efficiency? 266 operation 304
12.10.1 The old way: Paradigm 266 References 305
 Contents ix

15. Process commissioning 16.6.5 Coupling environmental and

process chemistry 333
Badrie Luckiram, BSc, MSc, CEng, MIChemE
16.6.6 Environmental emissions
15.1 Commissioning 307 records and HAZOP studies 333
15.2 Competency 307 16.7 Systems integration of plant
15.3 Checks prior to the start of operations within eco-industrial
commissioning 308 parks 334
15.4 Commissioning protocols 308 16.8 Conclusions 337
15.5 Specific process engineering Acknowledgments 337
responsibilities 309 References 337
15.6 Handover of the plant to the user 309
15.7 Overall recommendations for process 17. From idea to 1 million ton year
engineers 310
commercial plant
Appendix: Example Commissioning
Protocol for a new Hydrochloric Acid Joep Font Freide
Tanker Offloading Pump 310
17.1 The framework 339
17.2 The execution 341
16. Holistic process integration and 17.2.1 Concept and laboratory
optimization: Large-scale hybrid stage 341
process applications 17.2.2 Micro reactor stage 341
17.2.3 Pilot plant stage 342
Ugur Tuzun 17.2.4 Demonstration plant stage 343
16.1 Introduction 317 17.3 At last: Safety first 344
16.2 Life cycles of generic activities for
large-scale bulk chemicals 18. Scale-up challenges: Examples
production 318 from refining and catalysis
16.3 Systems integration design for
specialty products manufacture and Kaushik Basak
sales 321 18.1 Challenges in refining scale-up 345
16.4 Gated process development with 18.2 Challenges in catalyst scale-up 348
digital interlinks 321 18.3 Decision gate for catalyst scale-up 349
16.5 Digital control life cycles of integrated References 350
large-scale production plants 327
16.5.1 Configuring
communications 327 19. Scale-up challenges: Wastewater
16.5.2 Multivariable devices Kaushik Basak
communication 328
16.5.3 Loop converters 328 19.1 Challenges in wastewater
16.5.4 Multiplexers 328 treatment 351
16.6 Environmental impact monitoring References 353
and control 329
16.6.1 Green process applications in 20. Hemp/biomass process steps
process industries 330
Jay Van der Vlugt
16.6.2 Industrial emissions control
strategies using digital 20.1 Hemp cultivation overview 355
platforms 330 20.2 Extraction 356
16.6.3 Digital environmental sensor 20.2.1 Ethanol 356
technologies 330 20.2.2 Gaseous hydrocarbon
16.6.4 Digital platform construction extraction 357
for multivariate process and 20.2.3 Liquid hydrocarbon
environmental datasets 331 extraction 358
x Contents

20.2.4 Subcritical and supercritical 21.3 Making cost-of-manufacturing

carbon dioxide 359 estimates during the early stages of a
20.2.5 Cosolvent injection 360 project 387
20.2.6 Solvent-less processes 360 21.3.1 Identifying variable and fixed
20.2.7 Dry sifting 360 costs 387
20.2.8 Cold water (kief) extraction 361 21.3.2 Variable costs 388
20.2.9 Distillation 362 21.3.3 Fixed costs 392
20.3 Innovations and other extraction 21.4 Putting the costs together: Example
technologies 364 problems 397
20.3.1 Ultrasonic processing 364 21.5 Handling uncertainties during early
20.3.2 Hybrid microwave 365 project stages 399
20.3.3 Targeted cannabinoid salt 21.6 Combining costs with revenues to
precipitation 365 compute economic indicators 405
20.3.4 Winterization-purification 367 21.6.1 Introduction to economic
20.3.5 Organic solvent indicators 405
nanofiltration 367 21.6.2 There are only two key
20.4 Cannabinoid isolation 368 questions 405
20.4.1 Decarboxylation 370 21.6.3 Risk and reward: Is there any
20.5 Conclusions 370 data? 405
20.5.1 Hazardous installation 21.6.4 Financial indicators:
requirements 370 Definitions 405
20.5.2 Contamination and other 21.6.5 Internal rate of return (IRR) or
process issues 371 discounted cash flow percent
References 372 (DCF%) 406
21.6.6 Final summary 409
21. Techno-economic analyses References 411

Ron Leng and John Anderson

22. Project management
21.1 Introduction 373
Venkata Ramanujam and Bob Barnes
21.1.1 Uses of a techno economic
assessment 373 22.1 Introduction 413
21.1.2 Decision making 374 22.2 The project engineering process 413
21.2 Technology assessment 376 22.2.1 Integrating course work in
21.2.1 Definition of new chemical process
technology 376 engineering 415
21.2.2 Feasibility: The first screen 377 22.3 Predictive tools 418
21.2.3 Technology scalability to 22.4 Industries served by process
full-scale manufacturing 377 engineers 419
21.2.4 Technical success 22.5 Process plant components 419
parameters 377 22.6 Process safety and process engineering
21.2.5 Types of technology risk 378 work flow 420
21.2.6 Risk management plan 379 22.7 Putting it all together with practical
21.2.7 Licensed technology 382 knowledge 421
21.2.8 Investment in a start-up 22.7.1 Selecting the site or living with
technology 383 the selection handed to you 421
21.2.9 Duplication of existing 22.7.2 Site issues 423
technology: A caution 383 22.7.3 Common concerns: Funding,
21.2.10 Types of projects 383 control of site 424
21.2.11 Types of process 22.7.4 Community issues: Tax
technology 384 incentives, sales tax, resources,
21.2.12 Batch vs. continuous and workforce supply 425
mode 385 22.8 Engineering: In-house resources and
21.2.13 Technology package 386 EPC firms 425
 Contents xi

22.8.1 Forming the team 425 22.9.5 Piping 429

22.8.2 Selecting the engineering, 22.9.6 Power distribution 429
procurement, and construction 22.9.7 Control networking and field
(EPC) firm 425 instruments 430
22.8.3 The all-important P&ID 22.9.8 Project controls: Schedule
development 426 and budget 430
22.8.4 Controls and control room 22.9.9 Operator training 430
concerns 426 22.9.10 Commissioning, qualification
22.8.5 QA/QC needs 426 batches and testing and
22.8.6 Facilities and equipment for start-up 431
operations and
maintenance 427
22.8.7 Hazard analysis: Is it required or 23. Decommissioning
just a good practice 427
Barry A. Perlmutter
22.8.8 Project management 427
22.8.9 Scheduling 427 23.1 Options for decommissioning 433
22.9 Project execution 428 23.2 How to begin decommissioning 433
22.9.1 Organization and 23.2.1 Decontamination 433
planning 428 23.2.2 Final steps of the
22.9.2 Sitework and utility supply 428 decommissioning project 436
22.9.3 Foundations and steel
erection 428
22.9.4 Setting equipment 429 Index 437
This page intentionally left blank
Contributors
Numbers in parentheses indicate the pages on which the authors’
contributions begin.
Brooke Albin (1), Research & Development, MATRIC
(Mid-Atlantic Technology, Research & Innovation
Center), South Charleston, WV, United States
John Anderson (373), Engineering & Process Sciences,
Dow Chemical, Midland, MI, United States
Bob Barnes (413), Project & Process Consultant, Prova-
tions LLC, Gregory, TX, United States
Kaushik Basak (293, 345, 351), Principal Engineer
(SMPO), Shell plc., Shell Technology Centre,
Bangalore, India
Joep Font Freide (339), FFTechnology, Guildford, United
Kingdom
Alan Gabelman, Ph.D., P.E. (13, 69), Gabelman Process
Solutions, LLC, West Chester, OH, United States
Nick Harbud (191, 219), C.Eng., F.I.Chem.E., Newbury,
United Kingdom
Ron Leng (373), Engineering & Process Science, Dow
Chemical, Midland, MI, United States
Badrie Luckiram, BSc, MSc, CEng, MIChemE (133,
177, 307), Pharmaceutical & Process Engineer, London,
United Kingdom
Barry A. Perlmutter (125, 433), Perlmutter & Idea Devel-
opment LLC, Matthews, NC, United States
Venkata Ramanujam (413), McDermott Inc., Houston,
TX, United States
Jose M. Sentmanat (113, 125), Liquid Filtration Specialist,
LLC, Conroe, TX, United States
Stephanie Shira (249), Myers Mixers, Cudahy, CA, United
States
Ugur Tuzun (317), Churchill College, University of
Cambridge, Cambridge, United Kingdom
Jay Van der Vlugt (355), Cannabinoid Sciences, Nectar
Health Sciences Inc., Victoria, BC, Canada
Mike Williams (239), Process Automation, ARC
Advisory, Dedham, MA, United States
Nima Yazdanpanah (273), Engineering and Development,
Procegence, Chevy Chase, MD, United States
Hongben Zhou (145), BHS-Sonthofen Process Tech-
nology GmbH & Co. KG, Herrsching, Germany
xiii
This page intentionally left blank
About the editor

Barry A. Perlmutter is President of Perlmutter & Idea Development LLC (P&ID). He has 40 years of technical engi-
neering and business marketing experience in solid-liquid separation, filtration, centrifugation, and process drying. His
skills focus on process solutions, innovation strategy, and business development and market expansion. Barry has published
and presented worldwide and is responsible for introducing many European technologies into the marketplace. He is an
author of Elsevier’s Solid-Liquid Filtration - Practical Guides in Chemical Engineering handbook and a new e-book
Framework for Selecting Automated Solid-Liquid Filtration Technologies for Clarification Applications.
Barry began his career with the US Environmental Protection Agency and then entered the world of solid-liquid sep-
aration at Pall Corporation. For 11 years, he continued at Rosenmund Inc. as VP of Engineering and Sales including Comber
and Guedu Dryers and Ferrum Centrifuges. From the process industries, Barry joined Process Efficiency Products, now part
of Amiad USA, as a Director of Marketing and Sales for the manufacturing of filtration, separation and adsorption
technologies for cooling tower and HVAC water, process fluids, and water and wastewater treatment. He then became
President & Managing Director of BHS-Filtration Inc. (BHS-Sonthofen Inc.) where he grew the filtration, drying, mixing,
and recycling business of BHS for more than 20 years including the integration of AVA GmbH dryers. His current
company, P&ID, allows Barry to provide consulting services for process and project development with operating
companies and business development, marketing, and sales strategies for process technology suppliers.
He received his BS degree in Chemistry from Albany State (NY) University, MS degree from the School of Engineering
at Washington University, St. Louis, and an MBA from the University of Illinois, Chicago.

xv
This page intentionally left blank
Preface

Over my career of 40 years in the process industry, writing has always been a passion for me. It represents an opportunity to
convey concepts, ideas, and technical information in a manner that makes sense to the audience. While I never had any
formalized journalism or writing training, this skill somehow developed on its own through my continuing learning,
reading, and speaking/presenting on the topics of solid-liquid separation, centrifugation, drying, and other process
equipment and technologies as well as business development and innovation. This work has spanned over 40 countries
on 6 continents.
I began writing when I was a young Environmental Scientist with the US Environmental Protection Agency (USEPA).
During those years, I issued Code of Federal Register rules and justifications, approved, of course, by the Branch Manager
and eventually the Regional Administrator. Several of my reports are still available should you be eager to read “EPA 905/
5-81-002: Economic Impact of Implementing VOC Group II Rules in Ohio” or “EPA 905/9-82-005: Air Quality Non-
Attainment Areas in Region 5.”
From the USEPA, I joined Pall Corporation and continued my writing in their marketing group where I issued my first
filtration paper in 1982, WER 5300—Principles of Filtration. This paper had to be approved by Dr. Pall before it was issued.
My writing continued, and one of my tag lines was “like the Sheriff in the Wild West, my role is to bring order from chaos in
the filtration industry.”
My technical and marketing application articles—more than 150 to date—culminated in 2015 with the publication of
my first book for Elsevier, the handbook of Solid-Liquid Filtration. Part of Elsevier’s Practical Guides in Chemical Engi-
neering, where each book provides a focused introductory view on a single subject, the Handbook required almost 1 year to
write. The fun and challenge of that task have further been rewarded with year-to-date sales of more than 900 copies.
Now here we are at the current book, Integration and Optimization of Unit Process Operations. On the strength of the
handbook’s market acceptance, Elsevier asked me to propose a second book. They suggested that based upon my
experience, I edit a book unique to the chemical process industry (CPI). I welcomed the opportunity.
The problem in the marketplace, as I see it, is the type of engineers trained. In the early 1970s, companies wanted staff
with an “I-shaped” skill level. Someone with “I-shaped” skills has a deep (vertical) expertise in one area and practically no
experience or knowledge in other areas. This person is typically known as a specialist. In the 1980s, the industry wanted
“T-shaped” professionals. The vertical bar on the T represents strong knowledge in a specific discipline. The horizontal bar
represents a wide (horizontal) yet shallow knowledge in other areas. This allows the person to be able to collaborate across
other disciplines and acquire new skills or knowledge. Now, however, with the rapid proliferation of technological
advances and the cross-disciplinary nature of work, we need “Key-shaped” engineers who have several areas of expertise
with varying degrees of depth. This book addresses this need.
First, what this book is not is another textbook for designing equipment and technology. There are many references,
university courses, etc., for this work and teaching the “nuts and bolts” of pumps, heat exchangers, distillation towers,
thermodynamics, etc.
This book takes a different approach to share up-to-date and practical information on chemical unit operations from the
R&D stage to scale-up and demonstration to commercialization and optimization. At each stage, the information presented
differs as the technology and issues faced at the lab scale change in commercialization and optimization. This book takes a
broader view and encourages a “Key-shaped” approach to chemical engineering.
As the chemical industry changes and becomes more integrated worldwide, information exchange is needed. This
exchange must include not only principles of operation, but also practical knowledge transfer. This book addresses
this need.
Engineers must be able to ask questions of I-shaped and T-shaped professionals to develop creative solutions. This book
addresses the needs of engineers who want to increase their skill levels in various disciplines so that they can develop,
commercialize, and optimize processes.

xvii
xviii Preface

Some theory is included to provide the necessary background of the specific unit operation, but as stated previously, this
is not the main emphasis. Each chapter discusses practical aspects and illustrates the impacts of upstream process decisions
on downstream operations. Chapters also include troubleshooting at each process stage and suggest questions to ask to
develop creative solutions to process problems.
The engineer using this book will be able to take the content and apply it to the task at hand. For example, if you are
working on a process and need information on electrical and controls, you will find this. If you are a new project manager,
you will find a chapter on how to develop a project from beginning to final acceptance and start-up. Whether you are a start-
up or producing millions of tons/year, you will find the necessary guidance. I hope that this will be your “go-to book” along
the way as you grow and expand your skills and career.
The organization of the chapters follows that of a chemical operating company no matter the size of the operation. It
begins with crystallization and fermentation. Then, there are discussions of the process equipment followed by automation,
mixing and blending, process modeling and safety, and commissioning. We then discuss optimization, project man-
agement, techno-economic analysis, and “putting it all together.” The book concludes with a chapter on decommissioning
which is important, as processes change, products change, and the market itself changes.
Two more topics in the book deserve a separate mention. First, there is a chapter on hemp, cannabis, CBD or canna-
bidiols, and biomass. This is a new and flourishing industry, and many of the readers of this book may be drawn into this
process area. Finally, we discuss sustainability and holistic integration and optimization of chemical processes and con-
sumer product manufacturing. This chapter explores the impacts of environmental, socio-ecological, and economic issues
on decision making requiring the application of holistic systems modeling in process and product design to evaluate the
related consequences.
Finally, the text, as you will see, varies from chapter to chapter, as all contributing authors come from differing back-
grounds and experiences. This, I believe, it one of the greatest strengths of this book. Besides the United States, we have
authors from India, Germany, United Kingdom, Ireland, Netherlands, and Canada. Their experience encompasses process
engineers, technology suppliers, plant managers, academia, governmental agencies, consultants, and start-up to Fortune
500 companies. Each author brings a unique approach to problem solving and plant operations. An approach and expertise
they have so graciously taken the time to share.
As one author commented: “We, as a community, really have a responsibility to help and support younger engineers
and/or people who are thinking of going into the profession. We particularly need to mentor people from non-traditional
backgrounds who just need some encouragement and support, otherwise there is the danger of them becoming discouraged
and falling away from the profession. We need diversity in this profession.”
This book embraces that diversity. Thank you to all the authors who spent time researching and writing to contribute
your chapters. You are the backbone of this book. I have enjoyed working with you and truly hope that our paths will
cross again.
Thanking everyone I’ve worked with over my 40 years for their guidance, influence, help, and assistance would take a
book itself. As I reflect on my career and the many worldwide friends that I have had the pleasure of meeting over all these
years, I am truly grateful to each one of you. Let me say that the word “friends” in my mind are colleagues, customers,
competitors, suppliers, publishers, editors, and many others who have helped me to succeed. I have been fortunate through
hard work, long hours, and a personal goal of making each and every one of our contacts an informative and productive
experience to build many long-lasting relationships and, more importantly, invaluable friendships over all these years. It
has been these relationships that keep me striving to give back to our engineering community.
A heartfelt thank you also to my parents, my wife Michelle, and my family, friends, trainers, and yogis for supporting me
all these years and being part of my life. You all have heard the stories, and while you may not have fully understood all, you
have been there for me forever. Thank you, thank you, and thank you again.
I now must give one final thanks to Jenn Goddu who started with me in 2014 as my technical associate, editor, friend,
and all-around writer as I publish, blog, post, and tweet. Her skills are completely beyond reproach.
And, to the readers of this book, I hope that the information from the experiences of the contributing authors will help
you to succeed in your careers and personal growth. Thank you.

Barry A. Perlmutter, Editor

Perlmutter & Idea Development LLC, Matthews, NC, United States
Chapter 1

Crystallization
Brooke Albin
Research & Development, MATRIC (Mid-Atlantic Technology, Research & Innovation Center), South Charleston, WV, United States

Crystallizer process design requires attention to many varied factors. This chapter discusses fundamentals and laboratory
scale process development, pilot scale crystallization studies, and commercialization of crystallization processes to provide
an overview of the considerations in this area of solids processing.

1.1 Fundamentals and laboratory scale process development

The design of an industrial crystallization unit depends greatly on the characteristics of the feed supplied from the upstream
process and has direct consequences for downstream operations. For this reason, both narrow and broad perspectives are
needed to ensure a design that will be implemented successfully. The crystallizer operation must be robust within the entire
range of operating conditions it is subjected to. For example, if upstream concentration varies, the crystallizer must be able
to respond to that in some way in order to continue to operate smoothly and not cause upsets downstream.
The design of a crystallizer starts in the laboratory. The lab setting offers maximum flexibility for making changes to
design, adjusting conditions, and closely observing behavior of the system. Laboratory crystallizer equipment is often con-
structed of glass, which provides a significant advantage in early stages of process development when much can be learned
by visual inspection. Nucleation, crystal growth, agitation, slurry thickness, and tendency for fouling can all be studied
in situ. Ranges for operating conditions can start to be approximated often within the first few tests, and many items of
concern can be identified at this stage so proper design considerations can be made.

1.1.1 Crystallizer design basics

Crystallization is achieved by exploiting differences in solubility of components in a solution. It can be a useful method for
separating components or purifying a particular material. It is often used for recovering a solid product of high purity, but in
some cases, the objective is to remove solid impurities from a liquid stream. In either case, the separation occurs when
supersaturation is generated to solidify one component in pure form. This process is governed by the physical properties
of the components in the solution. A phase diagram is the ideal starting point for developing any crystallization process.
A phase diagram for a typical binary eutectic system is shown in Fig. 1.1. It shows the solid-liquid equilibrium data
(solubility curves) for each of the major components in solution. This provides important information regarding the con-
ditions required for crystallizing the desired component, and it establishes the limits of what crystallization can achieve in
terms of yield (recovery). For a solution of a given concentration, the diagram indicates the temperature at which crystal-
lization will begin. If temperature is lowered further, more solids will form, leaving a less concentrated liquid (mother
liquor) behind. The theoretical yield can be determined by performing a material balance that accounts for the starting
concentration of the solution and ending concentration of the mother liquor at a given set of conditions. The eutectic indi-
cates the point at which both components will crystallize and separation cannot be achieved. This represents the conditions
at which the maximum theoretical yield can be attained.
Consider the example in Fig. 1.1, which assumes a feed solution containing 80 wt% of component A. Pure crystals of
component A will start to form as the solution is cooled to 0°C. Crystals of component A will continue to form as tem-
perature is lowered until the solution is cooled to its eutectic point at
40°C. At this point, both A and B will crystallize,
producing a solid phase that contains a 2:1 ratio of B:A.
Phase diagrams can sometimes be found in the literature, but it is preferred that solubility data are generated experi-
mentally to ensure they are representative. This especially applies to feeds that contain greater than 1%–2% of impurities or
have more than two components, since the physical properties are more likely to be affected (Bamforth, 1965).

Integration and Optimization of Unit Operations. https://doi.org/10.1016/B978-0-12-823502-7.00022-0

Copyright © 2022 Elsevier Inc. All rights reserved. 1
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