TÀI LIỆU KỸ THUẬT SẤY - FREEZE DRYING (Nguyễn Tấn Dũng - Trường Đại học Sư phạm Kỹ thuật TP.HCM) | Cộng đồng Kỹ thuật cơ điện Việt Nam EBOOKBKMT

Freeze drying is one of the most advanced drying techniques for food preservation. Freeze-dried products generally have excellent quality and maintain most of the nutritional values as compared to raw materials.
This drying technique is not only applied for food technology but is also widely used in other fields such as in pharmaceutical industry to preserve biological substances; in biotechnology to long-term store cells, genes and biological materials; or in cosmetic industry to preserve chemical ingredients without using any preservatives.

This book aims to provide the principles and techniques of modern freeze drying technology. It can be used as an excellent reference for teaching and researching activities in Ho Chi Minh City University of Technology and Education, as well as in other interdisciplinary academic institutes.

This book consists of five chapters including Chapter 1. Overview of Freeze drying; Chapter 2. The physical thermal properties of the moist material affecting the freeze drying process; Chapter 3. Modeling freeze drying process; Chapter 4. Methods for establishing modes of freeze drying technology, and Chapter 5. Calculation, design and manufacture of freeze
drying systems. It can be considered as a beneficial reference book for not only food engineers but also students from chemical, material or biological aspects who demand a comprehensive understanding of freeze drying.

As the first book about freeze drying published in Vietnam, the authors hope to provide a comprehensive study of freeze drying technique to the readers to promote the applications of freeze drying in research as well as in industry. Also, we would like to give all of our respect and gratefulness to colleagues in Ho Chi Minh City University of Technology and Education,
who strongly motivate us to write this book.

Due to the massive knowledge presented in this book, mistakes during the compilation are inevitable. We do hope to receive valuable feedback from readers to refine this book in following editions.

Your feedbacks could be sent to the corresponding author’s email:

tandzung072@hcmute.edu.vn.

Assoc. Prof. Dr. Nguyen Tan Dzung

CONTENTS:

PREFACE

Chapter 1: OVERVIEW OF FREEZE DRYING ..............................19

1.1. Scientific basis for the freeze drying process ...............................19

1.1.1. Definition ...............................................................................19

1.1.2. The phase transition process of water ....................................20

1.1.3. Stages of freeze drying process .............................................23

1.1.3.1. Freezing stage ...........................................................23

1.1.3.2. Freeze drying (Primary drying) ...............................26

1.1.3.3. Low-temperature vacuum drying (Secondary

drying) ....................................................................................28

1.1.4. Nature of the drying process ..................................................28

1.1.5. Equation of the phase transition of water during drying ............28

1.1.6. Sublimation mechanism of frozen ice in moist materials ............29

1.1.6.1. Ice sublimation .........................................................29

1.1.6.2. Crystalline ice in moisturous materials .....................30

1.2. Applying the freeze drying technology .........................................30

1.2.1. Application in pharmaceutical products ................................31

1.2.1.1. Injectable products ....................................................31

1.2.1.2. Oral drugs..................................................................32

1.2.2. Application in food technology ..............................................33

1.2.2.1. Animal-based products..............................................34

1.2.2.2. Plant-based products .................................................36

1.2.2.3. Application in post-harvest technology ....................38

1.2.3. Application in microbiology and enzyme technology ...........40

1.2.3.1. Microbiology.............................................................40

1.2.3.2. Enzyme technology ...................................................41

1.2.4. Application in biotechnology .................................................43

1.2.5. Application in material technology ........................................44

1.2.5.1. Ceramics ...................................................................45

1.2.5.2. Aerogels ....................................................................46

6

1.2.5.3. Other materials ..........................................................46

1.2.6. Application in other technology .............................................46

1.3. The freeze drying equipment system ............................................48

1.3.1. Principle diagram of freeze drying system ............................48

1.3.2. The sublimation chamber .......................................................51

1.3.3. The refrigeration system ........................................................54

1.3.4. The vacuum system................................................................56

1.3.4.1. The condensation-freezing equipment ......................56

1.3.4.2. Vacuum pump ...........................................................58

1.3.5. The automatic control of the freeze drying system ...............62

1.3.5.1. Structure of automatic measurement and control

system ....................................................................................64

1.3.5.2. Automatic control and measurement using computer ..........65

1.3.5.3. Automation of sublimation drying system ................66

1.4. Freeze drying systems used in production ...................................68

1.4.1. Sublimation drying system with separate freezing stage .........68

1.4.2. Sublimation drying system with freezing stage right in

the drying chamber ..........................................................................70

1.4.3. Continuous freeze drying .......................................................74

1.5. Development of freeze drying .......................................................75

1.5.1. International development .....................................................75

1.5.1.1. Freeze drying system from Germany ........................76

1.5.1.2. Freeze drying from the USA .....................................76

1.5.1.3. Freeze drying from Japan ..........................................77

1.5.1.4. Freeze drying from France ........................................78

1.5.1.5. Freeze drying from England .....................................80

1.5.1.6. Freeze drying from New Zealand .............................81

1.5.1.7. Freeze drying from China .........................................82

1.5.2. Local market – Vietnam ........................................................83

1.5.2.1. Freeze dryers DS-1 and DS-2 ...................................84

1.5.2.2. Freeze dryer DS-3 .....................................................84

1.5.2.3. Freeze dryer DS-4 .....................................................86

7

1.5.2.4. Freeze dryer DS-5 .....................................................87

1.5.2.5. Freeze dryer DS-6 .....................................................88

1.5.2.6. Freeze dryer DS-7 .....................................................90

1.5.2.7. Freeze dryer DS-8 .....................................................91

1.5.2.8. Freeze dryer DS-9 .....................................................93

1.5.2.9. Freeze dryer DS-10 ..................................................95

1.5.2.10. Freeze dryer DS-11 ................................................96

1.6. Products from the application of freeze drying in Vietnam .........97

1.6.1. Freeze drying of Penaeus monodon (tiger shrimp) and

Durian ..............................................................................................97

1.6.2. Freeze drying of royal jelly ....................................................98

1.6.3. Freeze drying of oranges, bananas, apples, and carrots .........99

1.6.4. Freeze drying of okra and Gac fruit .....................................100

1.6.5. Freeze drying of squid ........................................................100

1.6.6. Freeze drying of Cordyceps mushroom ...............................101

1.6.7. Freeze drying of dragon fruit and durian .............................101

1.6.8. Freeze drying of avocado and others ...................................102

REFERENCES ....................................................................................104

Chapter 2: THE PHYSICAL THERMAL PROPERTIES OF

THE MOIST MATERIAL AFFECTING THE FREEZE

DRYING PROCESS ...........................................................................113

2.1. Inorganic and organic materials .................................................113

2.2. Absolutely dried and moist materials .........................................114

2.2.1. Absolutely dried materials ...................................................114

2.2.2. Moist materials ....................................................................114

2.3. The properties of water in materials ..........................................115

2.3.1. The important physical thermal properties of water ............115

2.3.2. The water bond in moist materials .......................................118

2.3.3. The crystallization temperature in moist materials ..............119

2.3.4. Adsorption and capillary characteristics ..............................119

2.4. Material classification ..................................................................122

8

2.5. Types of linking bond and the moisture linking bond energy

in moist materials .................................................................................123

2.5.1. The adsorbent bonds ............................................................123

2.5.2. The capillary bonds ..............................................................125

2.5.3. The osmosis bonds ...............................................................126

2.6. Chemical compositions of materials ...........................................127

2.6.1. Water ....................................................................................127

2.6.2. Protein and free amino acids ................................................128

2.6.3. Carbohydrate ........................................................................129

2.6.4. Lipids and free fatty acids ....................................................130

2.6.5. Minerals ...............................................................................131

2.6.6. Vitamins ...............................................................................131

2.6.7. Other macro elements ..........................................................131

2.6.8. Other micro elements ...........................................................131

2.7. The advantages of biological materials ......................................132

2.8. The important physical thermal properties of biological

materials affecting the freezing and freeze drying process ...............132

2.8.1. Viscosity and the relationship between viscosity and

quality of biological materials .......................................................132

2.8.2. Specific heat of biological materials ....................................133

2.8.3. Density of biological materials ............................................136

2.8.4. Thermal conductivity of biological materials ......................139

2.8.5. The thermal diffusivity coefficient of biological materials ........142

2.8.6. The moisture diffusion coefficient of biological materials ........143

2.8.6.1. The moisture diffusion coefficient ..........................143

2.8.6.2. Mathematical model to determine the moisture

diffusion coefficient .............................................................145

REFERENCES ....................................................................................148

Chapter 3: MODELING FREEZE DRYING PROCESS ...............155

3.1. Introduction ..................................................................................155

3.1.1. Pretreatment ........................................................................157

9

3.1.2. Freezing ..............................................................................158

3.1.3. Primary drying ....................................................................161

3.1.4. Secondary drying ................................................................163

3.1.5. Why must we model the freeze drying process? .................165

3.2. Modeling of freezing process ......................................................165

3.2.1. General concepts .................................................................165

3.2.2. The freezing and thawing process of product .....................167

3.2.2.1. The freezing process of product .............................167

3.2.2.2. The thawing process of freezing product ................170

3.2.3. Mathematical models of the freezing process ......................170

3.2.4. The essential physical thermal parameters to calculate

the rate of freezing water inside the product of the freezing

process ...........................................................................................174

3.2.4.1. Latent heat of freezing of water ..............................174

3.2.4.2. Specific heat of product ..........................................174

3.2.4.3. The rate of freezing water inside freezing product ........175

3.2.5. Building the method to determine the rate of freezing

water inside the product of the freezing process ............................176

3.2.5.1. General concepts .....................................................176

3.2.5.2. The equipment to determine the rate of freezing

water inside freezing products ............................................177

3.2.5.3. The equipment to freeze the product sample .........178

3.2.5.4. Building the method to determine the rate of

freezing water of freezing products .....................................179

3.2.6. Building modeling the freezing process to determine

the rate of freezing water inside the product ..................................187

3.2.6.1. Assumptions for the building of the mathematical model ............................................................................187

3.2.6.2. Building and solving the mathematical model

of the freezing process .........................................................188

3.2.7. Thermodynamics of the freezing process ............................193

3.2.7.1. General concepts .....................................................193

10

3.2.7.2. Freezing time estimation methods ..........................194

3.2.8. Changes in product properties during freezing ....................195

3.2.8.1. The crystallization of moisture in the product ........195

3.2.8.2. The relationship between the rate of water freezing and freezing temperature .............................................197

3.2.8.3. Changes in product quality when freezing ............197

3.2.9. Technological factors affecting the freezing process of

products used for freeze drying ......................................................198

3.2.9.1. Ambient temperature of the freezing process .........199

3.2.9.2. Time of freezing process .........................................199

3.2.9.3. Thickness of the product layer ................................200

3.3. Modeling of freeze drying process .............................................200

3.3.1. Mathematical models describing the freeze drying process ......200

3.3.1.1. The moisture diffusion model during freeze drying .......200

3.3.1.2. Models of heat and mass transfer during freeze

drying ...................................................................................202

3.3.2. Building a mathematical model to describe the kinetics

of the freeze drying process ...........................................................203

3.3.2.1. The drying material has a flat sheet shape ..............203

3.3.2.2. The drying material has a cylindrical shape ...........209

3.3.2.3. The drying material has a spherical shape ..............217

3.3.3. Changing of product’s characteristics in freeze drying

process ............................................................................................224

3.3.3.1. Moisture content of the product ..............................224

3.3.3.2. Loss of quality components of the product ...........225

3.3.3.3. The loss of rare biological active ingredients

of the product ......................................................................226

3.3.3.4. Loss of vitamins of the product .............................226

3.3.3.5. Reconstitution of the product ................................227

3.3.3.6. Energy cost of the product .....................................228

3.3.4. Technological factors affecting the freeze drying process .......229

3.3.4.1. Temperature of freeze drying environment ............230

11

3.3.4.2. Pressure of freeze drying environment ...................230

3.3.4.3. Time of freeze drying process ................................231

3.4. Optimization problem in freeze drying technology ..................232

3.4.1. Optimization problem of freezing process for use in

freeze drying .................................................................................232

3.4.2. Optimization problem of freeze drying process ..................233

3.4.3. Optimal plans for freeze drying technology ........................234

3.4.3.1. Basic concepts ........................................................236

3.4.3.2. The utopian plan and the utopian effect .................237

3.4.3.3. Multi-objective optimization by the utopian

point method with S(Z) optimal combination criterion .......239

3.4.3.4. Optimizing the multi-objective functions by the

restricted area method with R(Z) optimal combination

criterion ................................................................................240

3.4.4. Experimental statistical method used in freeze drying ........242

3.5. Superior characteristics of freeze drying products ...................245

REFERENCES ....................................................................................248

Chapter 4: METHODS FOR ESTABLISHING MODES OF

FREEZE DRYING TECHNOLOGY ...............................................259

4.1. Some basic concepts .....................................................................259

4.1.1. Modes of freeze drying technology ....................................259

4.1.2. General method for determining the modes of freeze

drying technology ..........................................................................259

4.2. Determination of the chemical composition and viscosity of

royal jelly .............................................................................................261

4.2.1. Royal jelly ............................................................................261

4.2.2. Determination of chemical composition ..............................262

4.2.2.1. Water .......................................................................263

4.2.2.2. Protein .....................................................................263

4.2.2.3. Glucid .....................................................................265

4.2.2.4. Lipid .......................................................................265

12

4.2.2.5. Minerals ..................................................................266

4.2.2.6. Vitamin ...................................................................266

4.2.2.7. Wax .........................................................................267

4.2.3. Functions of royal jelly for humans .....................................268

4.2.3.1. Nutritional value .....................................................268

4.2.3.2. Pharmaceutical value ..............................................268

4.2.3.3. Cosmetic value .......................................................271

4.2.4. Determination of the viscosity of royal jelly .......................271

4.3. Modeling and optimizing, establishing the mode of technology

for freezing stage for freeze drying.......................................................271

4.3.1. Establishing a mathematical model to determine the

appropriate ratio of frozen water and freezing temperature for

frozen royal jelly ............................................................................273

4.3.1.1. Establishing a mathematical model to determine

the appropriate ratio of frozen water ...................................273

4.3.1.2. Determination of the suitable freezing temperature of royal jelly ..............................................................281

4.3.2. Modeling and optimizing for determining freezing

technology mode of royal jelly used for freeze drying ..................284

4.3.2.1. Establishing and solving an optimization problem

describing the freezing process of royal jelly used for

freeze drying ........................................................................284

4.3.2.2. Determining the mode of freezing technology

of royal jelly in stage 1 for freeze drying ............................295

4.3.2.3. Conclusion ..............................................................296

4.4. Modeling and optimizing to determine appropriate technological parameters of freeze drying process of royal jelly ....................297

4.4.1. Determination of the pressure of the freeze drying medium ........298

4.4.2. Establishment of component objective functions of

multi-objective optimizing problem ..............................................299

4.4.3. Establishment of single-objective optimization problem

describing the process of royal jelly freeze drying .......................305

13

4.4.4. Establishment of multi-objective optimization problem

describing the process of royal jelly freeze drying ........................305

4.4.5. Solving the single-objective optimization problems

describing the process of royal jelly freeze drying ........................306

4.4.6. Solving the multi-objective optimization problem of

royal jelly freeze drying by the restricted area method ..................308

4.4.7. Experimental verification of optimal Pareto roots and

optimal Pareto efficiency of royal jelly freeze drying process ......313

4.4.8. Simulation of experimental mathematical models on 3D

and 2D graphs ................................................................................314

4.5. Determination of physicothermal parameters, description

of kinetics and establishment of the mode of freeze drying technology for royal jelly ............................................................................325

4.5.1. Description of the kinematics of royal jelly freeze drying

process ...........................................................................................325

4.5.1.1. Mathematical model describing the kinematics

of royal jelly freeze drying process .....................................325

4.5.1.2. Determination of physicothermal parameters

royal jelly .............................................................................325

4.5.1.3. Finding the roots of the typical equation ................329

4.5.1.4. Identification of the coefficients of mathematical

models (4.33) .......................................................................330

4.5.1.5. Kinetic description of royal jelly freeze drying

process and compatibility assessment of mathematical

models (4.33) .......................................................................336

4.5.1.6. Thermodynamic graph of royal jelly freeze

drying using the optimal mode ............................................343

4.5.2. Setting the technological mode of freeze drying for

royal jelly .......................................................................................344

4.5.3. Determination of the preservation mode for freeze-dried

royal jelly product and establishment of the technological

procedure ........................................................................................346

14

4.5.3.1. Determination of the preservation mode for

freeze dried royal jelly product ............................................346

4.5.3.2. Establishment of technological procedure for

freeze drying of royal jelly ..................................................350

4.5.3.3. Prospects of applying freeze drying technology

in food processing and preservation in Vietnam..................352

REFERENCES ....................................................................................354

Chapter 5: CALCULATION, DESIGN, AND MANUFACTURE

OF FREEZE DRYING SYSTEMS ...................................................373

5.1. General methods ..........................................................................373

5.1.1. Calculation for the cooling system ......................................373

5.1.1.1. The initially required parameters ............................373

5.1.1.2. Steps for calculating and designing a cooling

system ..................................................................................374

5.1.2. Calculation and design for a freeze drying system ..............374

5.1.2.1. Calculating heat for the sublimation chamber ........374

5.1.2.2. Calculating and designing for the condenser ..........375

5.1.2.3. Calculating for the vacuum system ........................375

5.2. Calculation and design for a self-freeze drying system ............376

5.2.1. Calculating and designing a freezing system integrated

into the sublimation chamber of the freeze drying system ............376

5.2.1.1. Calculating the freezing chamber or sublimation

chamber ..............................................................................376

5.2.1.2. Calculating the cooling load (or capacity) for

the product freezing process before the lyophilization

process .................................................................................380

5.2.1.3. Calculating the cooling load (or capacity) for a

refrigeration process to condensate – freeze moisture

sublimating from dried products ..........................................396

5.2.1.4. Building up the operating principle diagram for

the cooling system in a freeze drying system ......................403

15

5.2.1.5. Calculating and choosing a compressor with the

suitable cooling capacity .....................................................404

5.2.1.6. The total electrical motor power ............................409

5.2.2. Calculation and design of heat exchangers of the product

refrigeration system .......................................................................409

5.2.2.1. Calculation and design of the condenser ................409

5.2.2.2. Calculation and design of an evaporator ................419

5.2.2.3. Calculation and design of a receiver .......................424

5.2.2.4. Calculation of a throttle valve ................................430

5.2.2.5. Calculation of pipes ................................................431

5.2.3. Freeze drying system design calculation .............................433

5.2.3.1. Calculation of freeze drying chamber design .........433

5.2.3.2. Calculation of the ice condenser .............................439

5.2.4. Calculation of the vacuum pump system .............................443

5.2.4.1. Flow capacity of a vacuum pump ...........................443

5.2.4.2. Vacuum pump capacity ...........................................444

5.2.5. Determining the defrost time ...............................................445

5.2.6. Durable testing ability for the freeze drying chamber

and the ice condenser ....................................................................447

5.2.6.1. Stability for the drying process ...............................447

5.2.6.2. Checking the thickness of the freeze drying

chamber and the ice condenser ...........................................450

5.3. Calculation, design of low-temperature vacuum drying system

with heat pump and moisture condensation type ................................451

5.3.1. Required input parameters for calculation, design and

manufacturing ................................................................................451

5.3.1.1. Problem ............................................................................451

5.3.1.2. Requirements of the problem ............................................451

5.3.2. Calculating the size of the drying chamber ..........................455

5.3.2.1. Choosing the design of the drying chamber ...........455

5.3.2.2. Determining the size of the drying chamber ..........455

5.3.2.3. Heat plates ..............................................................458

16

5.3.2.4. Calculating and testing equipment structure

durability ..............................................................................459

5.3.3. Heat calculation for the drying system ................................462

5.3.3.1. Determining the temperature and pressure of

the drying environment ........................................................462

5.3.3.2. Determining the size of the dehumidifier (or

condensation - freezing) ......................................................462

5.3.3.3. Determining the moisture capacity of an ice

condenser evaporated from the drying product ...................464

5.3.3.4. Determining the heating capacity of heat plates .......466

5.3.3.5. Calculating the cooling cycle working for the

refrigeration - heat pump system of the dryer .....................469

5.3.3.6. Determination of the heat transfer surface size

of the freezing condenser .....................................................474

5.3.3.7. Calculation of heat load for refrigeration-heat

pump system ........................................................................475

5.3.3.8. Calculation of capacity of refrigeration compressor for refrigeration-heat pump system .........................476

5.3.3.9. Calculation of the condenser’s cooling capacity

in the refrigeration system and the heat supply capacity

for heat plates inside the vacuum drying chamber in the

drying system .......................................................................478

5.3.3.10. Calculation and design of the internal condenser

(the outdoor unit 1) ..............................................................480

5.3.3.11. Calculation for choosing an external condenser

(the outdoor unit 2) ..............................................................482

5.3.3.12. Heating efficiency of side burner .........................482

5.3.3.13. Calculation of the vacuum pump ..........................483

5.3.3.14. Calculation of heat for the pasteurization process .......484

5.3.3.15. Comparison of low-temperature vacuum drying

system, heat pump type with moisture condensation with

some imported machines having the same productivity ......485

5.3.4. Design of low-temperature vacuum drying system, heat

pump type with moisture condensation .........................................486

5.4. Automatic measurement and control of freeze drying machine,

a low-temperature vacuum drying system, heat pump type with

moisture condensation ..........................................................................505

5.4.1. Design of automatic control system for low-temperature

vacuum dryer, heat pump type with moisture condensation ..........505

5.4.2. Requirement of technology and automatic control a lowtemperature vacuum drying system, heat pump type with moisture condensation ...........................................................................506

5.4.2.1. Requirement of pasteurization regime ...................507

5.4.2.2. Requiring low-temperature vacuum drying mode,

sublimation drying ...............................................................509

5.4.3. The design of the dynamic part of a low-temperature

vacuum drying system has moisture condensation ........................510

5.4.4. Designing the controls of a low-temperature vacuum

drying system with moisture condensation ....................................513

5.4.5. Programing automatic measurement and controlling a

low-temperature vacuum drying system, heat pump type with

moisture condensation ...................................................................528

5.5. Manufacturing and installing the system of freeze drying machine,

a low-temperature vacuum drying system, heat pump type with

moisture condensation ...........................................................................529

5.5.1. Step 1: Technological requirements and input parameters

5.5.2. Step 2: Identifying the required specifications for the

design .............................................................................................530

5.5.3. Step 3: Development of technical profile drawings of

low-temperature vacuum drying system with condensation ..........530

5.5.4. Step 4: Fabrication of the low-temperature vacuum dryer

system with moisture condensation ...............................................530

5.5.5. Step 5: Vacuum drying system installation ..........................530

5.5.6. Step 6: Installation of automatic control systems ................531

18

5.5.7. Step 7: Operating, testing and calibrating the system .......531

5.5.8. Step 8: Vacuum drying of product and evaluation of

the effectiveness .............................................................................532

5.5.9. Fabrication and installation results in a low-temperature

vacuum drying system, heat pump type with moisture condensation .......................................................................................532

REFERENCES ....................................................................................538

APPENDIXES .....................................................................................556

APPENDIX 1 ........................................................................................556

APPENDIX 2 .......................................................................................563

APPENDIX 3 .......................................................................................575

APPENDIX 4 ........................................................................................580

APPENDIX 5 ........................................................................................584

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