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André B. de Haan, Johan T. Padding
Process Technology
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André B. de Haan, Johan T. Padding

Process
Technology

An Introduction

2nd Edition
Authors
Prof. Dr. Ir. André B. de Haan
Department of Chemical Engineering
Delft University of Technology
Section Transport Phenomena
Van der Maasweg 9
2629 HZ Delft
Netherlands

Prof. Dr. Johan T. Padding

Faculty of Mechanical, Maritime and Materials Engineering
Delft University of Technology
Leeghwaterstraat 39
2628 CB Delft
Netherlands

ISBN 978-3-11-071243-8
e-ISBN (PDF) 978-3-11-071244-5
e-ISBN (EPUB) 978-3-11-071246-9

Library of Congress Control Number: 2021951791

Bibliographic information published by the Deutsche Nationalbibliothek

The Deutsche Nationalbibliothek lists this publication in the Deutsche Nationalbibliografie;
detailed bibliographic data are available on the Internet at http://dnb.dnb.de.

© 2022 Walter de Gruyter GmbH, Berlin/Boston

Cover image: Mimadeo/iStock/Getty Images Plus
Typesetting: Integra Software Services Pvt. Ltd.
Printing and binding: CPI books GmbH, Leck

www.degruyter.com
Preface
Multidisciplinary cooperation is one of the key contributors to successful innovation
and project execution within the current and future process industry. The main chal-
lenge within multidisciplinary teams is communication, which will be much more ef-
fective when possessing basic understanding of each other’s discipline. It is exactly
this reason, enhancing the understanding of process technology by those without a
background in (bio)chemical process engineering, that has motivated us to create
the second edition of this book. The first edition served as the basis for the industrial
course “Introduction into the World of Process Technology,” which has been given for
many years within multiple multinational companies. Participants included chemists
(organic/catalytic/bio/physical/analytical), material technologists, economists, ac-
countants, lawyers and many others working in a position where cooperation and
communication with (bio)chemical process engineers was an essential part of their
job. Since 2020 the course has been revived and is now provided as “Process Technol-
ogy for Non-process Technologists” by the TU Delft Process & Product Technology In-
stitute (www.tudelft.nl/Pro2Tech). Besides small revisions/corrections throughout all
chapters and an update of references for further reading, this second edition now in-
cludes electrochemical conversion, a more complete overview of computational fluid
dynamics approaches and more background on economic evaluation of projects.
The main objective of this book is to provide a general overview of chemical
and biochemical process and product technology. It focuses on the structure and
development of production processes, main technological operations and the most
important aspects of product and process development, including economics. For the
technological operations, the emphasis is on their operating principles, reasons for
application and available industrial equipment. Design calculations and mathematics
have been kept to a minimum required to understand why process technologists and
engineers need certain information. All topics are extensively illustrated by represen-
tative examples.
The book is organized into seven distinct parts. An introduction to the structure
of the chemical industry and (bio)chemical processes is treated in Chapters 1 and 2.
Chapters 3–5 deal with (bio)chemical reaction engineering and reactor technology.
The most frequently applied molecular separation techniques such as distillation,
extraction, absorption, stripping, adsorption and ion exchange are discussed in
Chapters 6–9. The part on mechanical separation technology presents an overview
of the most important techniques for separating heterogeneous mixtures in Chap-
ters 10–12. Technologies relevant for particles and final product manufacturing are
treated in Chapters 13–15. Chapters 16–18 deal with the development, scale-up, de-
sign, engineering and safety of processes. The book concludes with three appendi-
ces in which major industrial processes for the production of base chemicals,
polymers and fine chemicals are described. It should be noted by the reader that the
appendices only represent a small selection of the numerous industrial processes in

https://doi.org/10.1515/9783110712445-202
VI Preface

operation and that the described processes have been selected with a bias on the
companies where the course was lectured. For further reading, an extensive list of
reference books is provided.

André B. de Haan
Johan T. Padding
Contents
Preface V

1 The chemical industry 1

1.1 Introduction 1
1.2 General characteristics of the chemical industry segments 3
1.3 Major raw materials 5
1.4 Production structure of the chemical industry 6

2 The structure of chemical and biochemical process systems 11

2.1 Structure of chemical and biochemical processes 11
2.2 Characteristics of production processes 12
2.2.1 Batch production technology 12
2.2.2 Continuous processes 13
2.3 Unit operations 15
2.3.1 Reactors 16
2.3.2 Recovery, purification and fractionation technologies 18
2.3.3 Product finishing operations 20
2.3.4 Other important process units 22
2.4 Process synthesis 24

3 Principles of chemical reaction engineering 27

3.1 Introduction 27
3.2 Classification of reactions 28
3.3 Rate of chemical reactions 29
3.3.1 Effect of concentration 29
3.3.2 Effect of temperature 30
3.3.3 Chemical equilibria 31
3.4 Catalysis 33
3.4.1 Homogeneous catalysis 33
3.4.2 Heterogeneous catalysis 35
3.5 Conversion, selectivtity and yield 37
3.5.1 Conversion 37
3.5.2 Selectivity and yield 38
3.5.3 Multistep reactions 39
3.6 Basic design equations for model reactors 41
3.6.1 Molar balances 41
3.6.2 The ideal batch reactor 42
3.6.3 The continuous ideal stirred tank reactor 44
3.6.4 Ideal continuous plug flow reactor 45
3.6.5 Cascade of continuous ideal stirred tanks reactors 47
VIII Contents

3.7 Heat effects in model reactors 48

3.7.1 General heat balance 48
3.7.2 Heat balance in a continuous ideal stirred tank reactor 49
3.7.3 Heat balance in a batch reactor 50

4 Chemical reactors and their industrial applications 53

4.1 Introduction 53
4.1.1 Classification of reactors 53
4.1.2 Influence of heat of reaction on reactor type 53
4.2 Stirred tank reactors 54
4.2.1 Description 54
4.2.2 Batch stirred tank reactors 55
4.2.3 Continuous stirred tanks 57
4.2.4 Cascade of stirred tanks 60
4.3 Tubular reactors 61
4.3.1 Introduction 61
4.3.2 Gas-phase reactors 62
4.3.3 Liquid-phase reactors 64
4.4 Loop reactors 65
4.4.1 Continuous loop reactors 66
4.4.2 Buss loop reactor 66
4.5 Bubble columns 68
4.6 Fixed and moving bed reactors 70
4.6.1 Fixed bed reactors 70
4.6.2 Adiabatic fixed bed reactors 71
4.6.3 Fixed bed reactors with supply or removal
of heat 72
4.6.4 Moving bed reactors 74
4.7 Fluidized bed reactors 75
4.7.1 The fluidization principle 76
4.7.2 Fluidization properties of typical bed solids 78
4.7.3 Applications 78
4.8 Electrochemical reactors 82
4.8.1 Basic elements of an electrochemical reactor 82
4.8.2 Design of an electrochemical reactor 83
4.8.3 Applications 85

5 Biochemical reaction technology 87

5.1 Characteristics of biochemical processes 87
5.1.1 Fermentation 88
5.1.2 Enzymatic conversions 93
5.2 Biochemical reaction engineering 96
 Contents IX

5.2.1 Principles 96
5.2.2 Kinetics of biochemical reactions 96
5.2.3 Basic reactor operations 100
5.3 Industrial bioreactors 102
5.3.1 Classification 102
5.3.2 Bioreactors with mechanical mixing 103
5.3.3 Bioreactors with pneumatic mixing 104
5.3.4 Bioreactors for immobilized enzymes and cells 106

6 Evaporative separations 109

6.1 Evaporative separation 109
6.1.1 Introduction 109
6.1.2 Vapor-liquid equilibria 110
6.1.3 Separation by single-stage partial evaporation 113
6.2 Multistage distillation 115
6.2.1 Distillation cascades 115
6.2.2 Column distillation 116
6.2.3 Feasible distillation conditions 118
6.2.4 Basic design calculations 119
6.2.5 Energy requirements 122
6.2.6 Batch distillation 123
6.2.7 Continuous separation of multiple products 125
6.2.8 Enhanced distillation techniques 125
6.3 Distillation equipment 127
6.3.1 Basic functions 127
6.3.2 Tray columns 128
6.3.3 Packed columns 132
6.3.4 Criteria for column selection 137
6.4 Polymer devolatilization 137
6.4.1 Introduction 137
6.4.2 Basic mechanisms 138
6.4.3 Multistage operation and devolatilization aids 140
6.4.4 Devolatilization equipment 141

7 Extraction and leaching 147

7.1 Liquid-liquid extraction 147
7.1.1 Introduction 147
7.1.2 Liquid-liquid equilibria 149
7.1.3 Solvent selection 151
7.1.4 Extraction schemes 152
7.2 Industrial liquid-liquid extractors 154
7.2.1 Mixer settlers 154
X Contents

7.2.2 Mechanically agitated columns 155

7.2.3 Unagitated and pulsed columns 155
7.2.4 Centrifugal extractors 157
7.2.5 Selection of an extractor 158
7.3 Leaching 159
7.3.1 Mechanism and process of leaching 160
7.3.2 Solid-liquid extractors 161
7.4 Supercritical extraction 165
7.4.1 Introduction 165
7.4.2 Properties of supercritical fluids 166
7.4.3 Processes and applications 167

8 Absorption and stripping 173

8.1 Introduction 173
8.2 The aim of absorption 175
8.3 General design approach 176
8.3.1 Gas solubilities 177
8.3.2 Minimum absorbent flow 179
8.3.3 Number of equilibrium stages 179
8.4 Basic characteristics of absorbers 180
8.5 Industrial contactors 181
8.5.1 Packed columns 182
8.5.2 Tray columns 183
8.5.3 Spray towers 185
8.5.4 Bubble columns 186

9 Adsorption and ion exchange 189

9.1 Introduction 189
9.2 Adsorption fundamentals 191
9.2.1 Industrial adsorbents 191
9.2.2 Adsorption equilibrium 194
9.2.3 Adsorption kinetics 196
9.2.4 Fixed bed adsorption 198
9.3 Basic adsorption cycles 200
9.3.1 Temperature swing 201
9.3.2 Pressure swing 202
9.3.3 Inert and displacement purge cycles 203
9.4 Principles of ion exchange 204
9.4.1 Ion exchange resins 204
9.4.2 Equilibria and selectivity 205
9.5 Ion exchange processes 207
 Contents XI

10 Solid-liquid separation 211

10.1 Introduction 211
10.2 Gravity sedimentation 215
10.2.1 Sedimentation mechanisms 216
10.2.2 Rate of sedimentation 217
10.2.3 Design of continuous sedimentation tanks 220
10.2.4 Gravity sedimentation equipment 221
10.3 Centrifugal sedimentation 223
10.3.1 Particle velocity in a centrifugal field 223
10.3.2 Sedimenting centrifuges 223
10.3.3 Bowl centrifuge separation capability 226
10.3.4 Hydrocyclones 227
10.4 Filtration fundamentals 229
10.4.1 Flow through packed beds 229
10.4.2 Cake filtration 231
10.4.3 Constant pressure and constant rate filtration 232
10.5 Filtration equipment 233
10.5.1 Continuous large-scale vacuum filters 234
10.5.2 Batch vacuum filters 235
10.5.3 Pressure filters 236
10.6 Filter media 239
10.7 Centrifugal filtration 240
10.8 Deep bed filtration 242

11 Particle removal from gases 245

11.1 Introduction 245
11.1.1 Separation mechanisms 245
11.2 Collecting efficiency 246
11.3 Gravitational separators 248
11.4 Cyclones 251
11.5 Electrostatic precipitation 253
11.5.1 Principles 253
11.5.2 Equipment and collecting efficiency 255
11.6 Particle interception mechanisms 257
11.7 Dry impingement separators 259
11.7.1 Deep bed filtration 260
11.7.2 Surface filters 261
11.7.3 Lamellar plate separators 262
11.8 Wet scrubbers 263
XII Contents

12 Membrane separations 269

12.1 Introduction 269
12.2 Principles 272
12.2.1 Membranes 272
12.2.2 Modules 274
12.2.3 Flux, permeability and selectivity 276
12.2.4 Concentration polarization and fouling 278
12.2.5 System design and cascades 280
12.3 Membrane filtration processes 282
12.3.1 Microfiltration 282
12.3.2 Ultrafiltration 283
12.3.3 Reverse osmosis and nanofiltration 284
12.4 Solubility-driven processes 286
12.4.1 Gas and vapor permeation 286
12.4.2 Pervaporation 288
12.5 Electrodialysis 290

13 Crystallization and precipitation 293

13.1 Introduction 293
13.2 Fundamentals 295
13.2.1 Solid-Liquid equilibria 296
13.2.2 Supersaturation and metastability 297
13.2.3 Nucleation 298
13.2.4 Crystal growth 300
13.2.5 Effects of impurities 302
13.3 Crystal characteristics 302
13.3.1 Morphology 303
13.3.2 Crystal size distribution 304
13.3.3 Size control 304
13.4 Types of solution crystallizers 305
13.4.1 Basic operations 305
13.4.2 Cooling crystallizers 306
13.4.3 Evaporating and vacuum crystallizers 307
13.4.4 Continuous crystallizers 308
13.5 Crystallizer modeling and design 309
13.5.1 Basic yield calculations 310
13.5.2 Population balances 312
13.5.3 The well-mixed MSMPR crystallizer 314
13.6 Precipitation 314
13.7 Melt crystallization 315
 Contents XIII

14 Solids finishing technologies 321

14.1 Overview 321
14.2 Drying 322
14.2.1 Classification of drying operations 323
14.2.2 Drying mechanisms 324
14.2.3 Direct heat dryers 327
14.2.4 Contact dryers 331
14.2.5 Other drying methods 335
14.3 Size reduction 336
14.3.1 Particle breakage 337
14.3.2 Methods and selection criteria for size reduction 339
14.3.3 Size reduction equipment 341
14.4 Size enlargement 345
14.4.1 Agglomeration principles 346
14.4.2 Methods of size enlargement 348
14.4.3 Growth/tumble agglomeration 348
14.4.4 Pressure agglomeration 350
14.4.5 Other agglomeration techniques 352
14.5 Conveying 353
14.5.1 Transportation systems 353
14.5.2 Mechanical conveyors 354
14.5.3 Pneumatic conveying 358

15 Product technology 363

15.1 Cheese coating technology 363
15.1.1 Cheese production 363
15.1.2 Coatings 364
15.1.3 Application techniques 364
15.2 Enzyme formulation 367
15.2.1 Introduction 367
15.2.2 Glucose isomerase immobilization 368
15.2.3 Detergent enzymes 370
15.2.4 Application research 373
15.3 Compounding 375
15.3.1 Introduction 375
15.3.2 Compound formulation 376
15.3.3 Additives 378
15.3.4 Polymer mixing mechanisms 381
15.3.5 Compounding equipment 383
15.4 Polymer processing 387
15.4.1 Extrusion processes 388
15.4.2 Injection and blow molding 389
XIV Contents

15.4.3 Melt and gel spinning 392

15.4.4 Film production techniques 394
15.4.5 Thermoforming 398
15.4.6 Foam extrusion 399

16 Development, scale-up and engineering 401

16.1 Introduction 401
16.1.1 General aspects of scaling up 401
16.1.2 Ways of scaling up 402
16.2 Development and scale-up in the bulk chemical
industry 403
16.2.1 Basic course of process development 403
16.2.2 Laboratory and bench scale research 406
16.2.3 Pilot plant research and demonstration plants 408
16.2.4 Feasibility evaluation 410
16.3 Engineering and construction 412
16.3.1 Introduction 412
16.3.2 Conceptual engineering 414
16.3.3 Basic engineering 415
16.3.4 Detailed engineering, procurement and construction 417
16.4 Development and scale-up of fine chemical processes 421
16.4.1 Differences between bulk and fine chemical industry 421
16.4.2 Fine chemical process development 421
16.4.3 Scale-Up challenges in multipurpose plants 423
16.4.4 Future developments 424

17 Hydrodynamic aspects of scale-up 427

17.1 Introduction 427
17.2 Hydrodynamic flows in process equipment 428
17.2.1 Single-phase flows 428
17.2.2 Multiphase flows 429
17.2.3 Flows in mixers and stirrers 430
17.2.4 Flows in bubble columns 438
17.2.5 Flows in fluidized beds 440
17.3 Scale-up 440
17.3.1 Dimensional, similarity and regime analysis 441
17.3.2 Important dimensionless numbers for mixing vessels 442
17.3.3 Important dimensionless numbers for bubble columns 443
17.3.4 Important dimensionless numbers for fluidized beds 445
17.4 Computational fluid dynamics (CFD) 446
 Contents XV

17.4.1 Types of CFD simulations 446

17.4.2 Basic principles of CFD 449
17.4.3 Applications 452

18 Process safety 455

18.1 Safety problems in chemical plants 455
18.2 Development, design and construction of safe plants 456
18.2.1 Introduction 456
18.2.2 Safety assessment 457
18.2.3 Structure of safety studies 459
18.3 Identification of hazardous properties of substances 461
18.3.1 Pure components 461
18.3.2 Exothermic chemical reactions 464
18.4 Inherently safer plant design 466
18.4.1 The concept and its benefits 466
18.4.2 The road to friendlier plants 467

A Base chemicals 471

A.1 Ammonia 471
A.1.1 General description 471
A.1.2 Desulfurization 471
A.1.3 Primary and secondary reforming 471
A.1.4 Shift conversion 473
A.1.5 Carbon dioxide removal 474
A.1.6 Final purification 474
A.1.7 Ammonia syntheses and recovery 475
A.2 Inorganic acids 476
A.2.1 Nitric acid 476
A.2.2 Sulfuric acid 478
A.3 Ammonia-based products 480
A.3.1 Caprolactam 480
A.3.2 Acrylonitrile 483
A.3.3 Urea 484
A.3.4 Melamine 486
A.4 Naphtha cracking 488
A.4.1 Basic principles 488
A.4.2 Hot section 489
A.4.3 Cold section 491
A.4.4 Coke formation 492
A.5 Oxidation processes 492
A.5.1 Toluene oxidation 493
A.5.2 Cyclohexane oxidation 495
XVI Contents

A.5.3 n-Butane oxidation 496

A.6 Fischer-Tropsch 498
A.6.1 Synthesis gas production 499
A.6.2 Fischer-Tropsch synthesis 501
A.7 Industrial electrochemical processes 505
A.7.1 Chlorine gas production 505
A.7.2 Hydrogen peroxide production 507
A.7.3 Adiponitrile production 508

B Polymer manufacturing 511

B.1 Polyethylene 511
B.1.1 High-pressure process 511
B.1.2 Solution polymerization 512
B.1.3 Slurry process 513
B.1.4 Gas-phase process 515
B.2 Polypropylene 517
B.2.1 Gas-phase process 517
B.2.2 Slurry process 520
B.3 EPDM 522
B.4 Polyamides 525
B.4.1 Introduction 525
B.4.2 Nylon 6 525
B.4.3 Nylon 4,6 526
B.5 Saturated and unsaturated polyesters 528
B.5.1 Saturated polyesters 528
B.5.2 Unsaturated polyesters 531
B.5.3 Powder coatings 532

C Life science products 533

C.1 Benzaldehyde-based products 533
C.1.1 Amino acids 533
C.1.2 Cinnamon aldehyde and cinnamyl alcohol 535
C.1.3 Benzyl alcohol 537
C.2 α-Picoline 537
C.3 Aspartame 540
C.4 Penicillin 541
C.5 Synthetic antibiotics 545
C.5.1 Introduction 545
C.5.2 Cephalosporins 546
C.5.3 Amoxillins 548
 Contents XVII

C.6 Glyoxylic acid 549

C.7 Food additives 551
C.7.1 Quinine 552
C.7.2 Enzymes 552

References and further reading 555

Index 565
1 The chemical industry

1.1 Introduction

The industry that applies the knowledge of chemical behavior is generally called the
chemical process industry. Chemical reactions and separation of compounds are
used to obtain products with desired properties. In reality, the chemical industry is a
set of related industries with many diverse functions and products. Some of these dif-
ferent areas, divided into three general classes of products, are listed in Fig. 1.1:
1. Industrial chemicals and monomers such as acids, alkalis, salts, chlorine,
ammonia, ethylene, propylene, caprolactam, acrylonitrile, industrial gases and
other organic chemicals.
2. Polymers and end chemicals to be used in further manufacture such as syn-
thetic resins, plastics, fibers, elastomers, dyes and pigments.
3. Finished chemical products for consumer applications as architectural paints,
drugs, cosmetics and soaps or to be used as materials or supplies in other indus-
tries such as industrial paints, adhesives, fertilizers and explosives.

Figure 1.1 emphasizes that certain raw materials are used to prepare key chemicals,
monomers and intermediates that may be sold independently or used directly in ad-
ditional steps to give various polymers and end chemicals. These in turn can be for-
mulated and fabricated into chemical products, which can sometimes be modified
into finished products. Hence, the term chemicals and allied products accurately
represents this diversity as well as the flow of materials and products from raw
sources to finished formulations. Although the division is approximate, about 60%
of the chemical industry manufactures industrial products that are further modi-
fied, whereas 40% of their products are sold directly to the consumer. Clearly, the
chemical industry is part of the manufacturing industry and within this it plays a
central part even though it is by no means the largest part of the manufacturing
sector. Its key position arises from the fact that almost all the other parts of the
manufacturing sector utilize its products.
The three major segments of the chemical industry depicted in Fig. 1.2 are related
to commodities, fine chemicals and specialty chemicals. The substances repre-
senting these segments exhibit an increasing complexity in molecular architecture.
In the business column starting from fossil fuels and culminating in the application
products, fine chemicals take a position with their special characteristics between the
commodities or base chemicals such as toluene, acetic acid, acetone, and methanol
and specialty chemicals or desired products for various markets. Fine chemicals are
sold on the basis of their chemical composition for use as intermediates in the pro-
duction of other materials. They are often needed in relatively small quantities and

https://doi.org/10.1515/9783110712445-001
 2

Chemical raw Chemicals Polymers Formulated Finished

materials Monomers End chemicals chemical products
products

“Allied” industries

Basic Organic Plastics Textiles Pharmaceuticals

Petrochemicals industrial Resins Rubber Soap and
chemicals processes detergents
Sulfur Elastomers
Industrial Photographic Cosmetics
Salt Synthetic
gases chemicals
1 The chemical industry

Paints, varnishes

Fig. 1.1: Chemical process industry.

Phosphate rock fibers
Inorganics Water and and lacquers
Minerals Dyes
Ammonia waste-treating Inks
Others Pigments
Perfume, flavor Adhesives
Surfactants
chemicals Pesticides
Functional Fertilizers
fluids
Consumer and
Carbon other industrial
60% Industrial products products specialties
Explosives
Propellants
Fabricated
plastics

40% Consumer products

 1.2 General characteristics of the chemical industry segments 3

high purity for only one or a few end uses. Product applications can be found in phar-
maceutical (50%), agrochemicals (20%) flavors and fragrances (5%), food additives
(5%) and various other industries (20%). Specialty chemicals are purchased because
of their effect rather than composition. There is some overlap in the definitions of
fine and specialty chemicals. The worldwide market in fine chemicals is estimated to
be approximately $100 billion in sales, compared to $1,000 billion for the commodity
segment. With respect to the financial turnover (sales), the specialty chemicals indus-
try is as large as the bulk chemical industry.

Basic Active
Raw Building Basic Consumer
feed ingre-
materials blocks products products
stocks dients

Oil Nafta Ethylene Polyethylene Plastic bags

Natural Propylene Acrylonitrile Polypropylene Car parts
gas Ammonia Caprolactam Nylon6 Carpet fiber
Air Toluene Benzaldehyde Phenylglycine Cephalexine
Butane Maleic Glyoxylic acid Aspartame Candarel
Anhydride Z-ASP
Beats Glucose Penicillin 6-APA Amoxillin

Commodity chemicals

Fine chemicals

Specialty chemicals

More complexity in molecular architecture

Fig. 1.2: Business column segmentation.

1.2 General characteristics of the chemical industry segments

The major sectors of the chemical industry are categorized on the basis of end prod-
uct uses in Fig. 1.3. Going from commodities, through fine chemicals to specialty
chemicals the products become higher priced, have a higher added value, a lower
volume and generally a shorter life cycle than the products closer to the fossil fuels
in the value chain. Within the chemical process industries, batch processing is fo-
cused on the fine and specialty chemicals sectors, while continuous processing is
dominant in bulk chemicals production. The scale of operations ranges from quite
small plants (a few tons per year) in the fine chemical area to the giants (100–1,000
thousand tons per year) of the petrochemical sector. Today, a typical base petro-
chemical plant is designed to produce enormous quantities (100–600 ktons/year)
4 1 The chemical industry

of a single product and operate 24 h a day all the year round. They are used to
make key intermediates, which are turned into a very wide range of products by
further processing. Clearly, such large and sophisticated plants require a very high
capital investment and are characterized by high investment versus low labor com-
ponents in the cost of manufacture. The investment per worker in a base petro-
chemicals olefins plant may well exceed a quarter of a million dollars. Although
these plants take full advantage of the economy of scale effect, the losses due to
running under design capacity can be extremely high if the balance between pro-
duction capacity and market demand is disturbed. This is particularly evident when
the economy is depressed, and the chemical industry’s business tends to follow the
cyclical pattern of the economy with periods of full activity followed by those of
very low activity.

Commodities: Fine chemicals: Specialties:

• Product life cycle Long (>30 yrs) Average(10-20 yrs) Short(<10 yrs)
• Product spectrum Narrow Broad Very Broad
• Product volume >> 10.000 t/yr < 10.000 t/yr Variable
• Product price < $ 5/kg > $ 10/kg Variable
• Product
differentiation None Low High

• Added value Small High High

• R&D focus Process Process Product

improvement development development

• Technology Continuous Batch & Batch &

Continuous Continuous

Fig. 1.3: The three main segments of the chemical industry.

It is important to keep in mind that, although most of the discussion about the
chemical industry tends to revolve around the multinational giants, the industry is
very diverse and includes many small-sized companies as well. There is a similar
diversity in the sizes of chemical plants. Batch type plants are used for the manufac-
ture of relatively small amounts of fine and specialty chemicals, typically up to 100
tons per annum. They are therefore not dedicated to producing just a single product
but are multipurpose and may be used to produce a number of different chemicals
each year. In this part of the chemical industry the investment level may not exceed
the order of 25,000 dollars per worker.
The research and development carried out in industry can be divided into prod-
uct development, process development, process improvement and application devel-
opment. The nature of research and development carried out varies significantly
 1.3 Major raw materials 5

across the various sectors of the chemical industry. In the commodity chemicals sec-
tor, most of the R&D expenditure will be devoted to process improvement. Process
improvement relates to processes, which are already operating. It may be due to
problems arisen and hindering or stopping production. More commonly, however,
process improvement will be directed at improving the profitability of the process.
Improving the quality of the product, by process modification, may lead to new
markets for the product. In recent years, the most important process improvement
activity has been to reduce the environmental impact of the processes. At the
other end of the scale lie the specialty chemicals. Here there are immense and
continuous efforts undertaken to discover and develop new products, which exert
the desired, specific effect. As such, the main focus in this sector is on new prod-
uct development such as pharmaceuticals, agrochemicals and antioxidant addi-
tives. Process development absorbs considerable resources in the fine chemicals
industry, in part because of the shorter life cycles of fine chemicals as compared
to commodities. It covers developing new manufacturing processes for new as
well as existing products. The push for the latter may originate from the availabil-
ity of new technology or change in the availability and/or cost of raw materials.
Process development for a new product depends on things such as the scale on
which it is to be manufactured, the by-products formed and required purity.

1.3 Major raw materials

Inorganic chemicals are derived from many different sources. In contrast, the pro-
duction of organic chemicals is almost entirely based on two raw material sources,
crude oil and natural gas. At present, more than 90% (by tonnage) of all commer-
cially important organic chemicals are produced from crude oil and natural gas via
a multitude of petrochemical processes. Compared to crude oil, natural gas is less
versatile because carbon–carbon bonds have to be built up. Apart from crude oil
and natural gas, other raw materials are used on a smaller scale such as fatty oils,
starch, sugar and molasses, wood and straw.
The inorganic chemical industry is based on a large variety of minerals, air
and water. Minerals are converted into products like building materials and pig-
ments. There is, however, a group of raw materials from which a limited number of
rather important inorganic intermediates is made. Perhaps the most notable exam-
ple is sulfur. Substantial quantities of sulfur are also removed and recovered from
natural gas and crude oil. Over 80% of all sulfur is converted into sulfuric acid, and
approximately half of this is then used in fertilizer manufacture. Sulfuric acid is the
most important chemical of all in tonnage terms. Other important examples are air,
the source of oxygen and nitrogen, and sodium chloride, the starting material for
caustic soda and chlorine.
6 1 The chemical industry

Fig. 1.4: Product family tree of the chemical

industry.

1.4 Production structure of the chemical industry

As indicated, the chemical industry is concerned with converting raw materials, such
as crude oil, firstly into chemical intermediates and then into a tremendous variety
of other chemical products. In an earlier period of the chemical industry’s develop-
ment, chemical companies were generally production oriented, exploiting a process
to produce a chemical and then selling it in rapidly expanding markets. As the indus-
try has grown, there has been a strong tendency toward integration, both forward
and backward. If today’s production structure of the chemical industry is examined,
it is seen that there are only a few hundred major basic products and intermediates
that are produced on a scale of at least a few thousand to several million tons per
annum worldwide. This relatively small group of key products, which are in turn pro-
duced from only about ten raw materials, forms a stable foundation on which the
many branches of refining chemistry (dyes, pharmaceuticals, etc.), with their many
thousands of often only short-lived end products are based. This has resulted in the
well-known family tree, schematically depicted in Fig. 1.4, which can also be regarded
as being synonymous with an integrated production system, with synergies that are
often of critical importance for success.
A special characteristic of the major basic products and intermediates is their
longevity. They are statistically so well protected by their large number of second-
ary products and their wide range of possible uses that they are hardly affected by
 Polypropylene plant
Polypropylene Garden furniture,
carpets, bumpers,
Propylene bottles
Rubber plant
Window profiles,
Rubbers bumpers, cooling water
hoses
Cracker LD Polyethylene plant
Naphtha Ethylene LD Polyethylene Packaging materials,
extrusion coatings

HD Polyethylene plant
HD Polyethylene Household articles as
crates, buckets etc.

Butane Slurry polyethylene plant

Propylene Strong fiber, artificial
UH Polyethylene hips, bullet proof vests,
tennis rackets

Fig. 1.5: Production chain for naphtha to polymers.

Butadiene plant MTBE plant
Butadiene MTBE Lead replacer in petrol

Styrene plant
Dashboards, helmets,
ABS plant
LEGO, household
Styrene ABS equipment housings

Ammonia Acrylonitrile Nylon4,6 plant Air bags, engineering

Nylon4,6 plastic
ACN plant Diamino butane

DAB plant
1.4 Production structure of the chemical industry

Adipic acid
7
8 1 The chemical industry

the continuous changes in the range of products on sale. Unlike many end prod-
ucts, which are replaced by better ones in the course of time, they do not them-
selves have a so-called life cycle. However, the processes for producing them are
subject to change. This is initiated by new technical possibilities and advances
opened up by research but also dictated by the current raw material situation. Here,
it is not the individual chemical product, but the production process or technology
which has a life cycle.
The relations between raw materials, intermediates, semimanufactured prod-
ucts and finished products are complex. For the chemical industry, cracking of
naphtha and gas oil is an important operation to produce raw materials, such as
ethylene, propylene and benzene. These are then used as raw materials for further
processing as shown in the product tree depicted in Fig. 1.5. The polymers sector
is the major user of petrochemical intermediates and consumes almost half of the
total output of produced organic intermediates. It covers plastics, synthetic fibers,
rubbers, elastomers and adhesives. Ammonia and fertilizers is a sector in which it
has been difficult to achieve a balance between capacity and demand. In tonnage
terms, it is one of the most important sectors based on the Haber process for ammo-
nia. As shown in Fig. 1.6, a large variety of products are starting with ammonia as
the basic intermediate. Based on a combination of petrochemical intermediates and
natural raw materials such as glucose the fine chemicals sector (Fig. 1.7) produces
an amazingly wide range of products for an even wider range of applications.
Along with pharmaceuticals, agrochemicals is a very profitable area because the
demand for its products is unaffected by the world’s economy and therefore re-
mains high even during recessions. This contrasts with the situation for most other
sectors of the chemical industry. The product trees presented here are especially
useful in the development of new processes and products.
 Cracker ACN plant
Propylene
Acrylonitrile Acrylic fibers,
clothes

α-Picoline plant
α-Picoline
2-Vinylpyridine

Phenol plant Caprolactam plant

Caprolactam
Phenol Nylon6, carpets

Urea
Air Tropical fertilizer
Urea plant Melamine plant
Urea Melamine Kitchen application,
Ammonia cups, plates etc.
Dolomite
KAS plant
Nitric acid plant
Natural gas KAS KAS fertilizer
Nitric acid
Fertilizer
Mixed fertilizers

Fig. 1.6: Production chain from ammonia to chemical products and fertilizers.
Phosphate NP & NPK fertilizers
1.4 Production structure of the chemical industry
9
 Penicillin
10

fermentation β-Lactam plant

7-ADCA
Glucose Pen G,V Cefalexine
Antibiotic

6-APA

Ampicilline Antibiotic
Toluene oxidation

Toluene Benzoic acid

Food & flavor
Derivatisation plant
Benzaldehyde Benzaldehyde derivatives
1 The chemical industry

Food additive

D-PG
Amino acid plant
amide
Benzaldehyde Aspartame plant
Phenyl alanine
Aspartame
Sweetener

Z-ASP plant
Benzyl alcohol
Z-ASP

Butane oxidation
Fumaric acid Maleic anhydride
Butane Monomer (SMA,
Resins), agro-
Ozonolysis plant chemicals

Fig. 1.7: Production chain for glucose, toluene and butane to fine chemicals.
Glyoxylic acid
Pharmaceutical
products
2 The structure of chemical and biochemical
process systems

2.1 Structure of chemical and biochemical processes

The route along which a raw material is converted to products is a logical coupling
of interconnected operations: the process (Fig. 2.1). At least one of the process
units is the chemical reactor in which chemical conversion takes place. In principle,
every chemical reaction shows incomplete conversion and often the formation of
by-products. Furthermore, auxiliary materials are often used, which must be sepa-
rated in another process step.

Bleed
Recycle

Product(s)
Feed Product
Pretreatment Conversion recovery & Product
purification finishing
Side
product(s)

Fig. 2.1: General representation of a process.

Raw materials are generally impure, have the wrong physical form or even consist
of mixtures of different compounds. Process units preceding the reactor prepare the
feed with mechanical operations such as crushing or grinding, followed by physi-
cal treatments such as mixing, heating and evaporating. Operations succeeding the
reactor treat the converted mass to recover and purify the product to the desired
specification, generally utilizing a series of separation steps. Hence, in most cases,
a plant contains a large number of separation steps, of which the investment typi-
cally accounts for 50–70% of the total plant investments. Unconverted feed compo-
nents and auxiliary chemicals will generally be recycled after further purification in
the recycle section. Often a part of the recycle is bled to avoid build-up of contami-
nants that are difficult to remove. Final product treatment consists usually of me-
chanical operations such as drying, granulation and packing.
Besides the desired product, usually several waste streams are produced, which
must be brought into an acceptable condition before leaving the plant. Ideally, only
air and water are emitted. After combining all process steps and streams, a compli-
cated network results.

https://doi.org/10.1515/9783110712445-002
12 2 The structure of chemical and biochemical process systems

2.2 Characteristics of production processes

The practical way a product is prepared on a laboratory scale is in many ways different
from the way it is done on an industrial scale. The main reasons for this are the huge
differences in the amount of material that has to be processed. On a laboratory scale,
one is usually satisfied with amounts that are sufficient for analytical purposes. Indus-
trial production concerns the production of amounts that can vary from 1,000 kg/year
up to over 1,000,000,000 kg/year for a single plant. It is clear that such large amounts
should have significant effects on the way a production process is designed.

2.2.1 Batch production technology

Batch processing has been a part of man’s activities throughout history and is still
used most of the time on a laboratory scale. Batch processes are used to manufac-
ture many of the products required for modern life. Within the chemical process in-
dustries, batch processing is focused on the fine and specialty chemicals sectors,
while continuous processing is dominant in commodity chemicals production.
A batch process is one in which a series of operations are carried out over a period
of time on a separate, identifiable item or parcel of material. It is different from a con-
tinuous process, during which all operations occur at the same time and the material
being processed is not divided into identifiable portions. This definition of batch proc-
essing includes what has been called semibatch production, during which material is
added continuously to a batch over some period. The sequence of events copies the
sequence developed in the laboratory, but in larger-size vessels and batches. The raw
materials are purified, perhaps by distillation or adsorption, and stored. Reactants are
then pumped or poured into a reaction vessel. The agitation intensity, the rate of heat-
ing and/or cooling and the rates of flow of other reactants or catalysts are controlled in
such a manner that the reaction proceeds as planned. When the reaction is completed,
the reactant mass is removed to a separation system. The desired products are sepa-
rated from unreacted feed materials and undesired byproducts. The reactants are usu-
ally recycled for use in the next batch. This is schematically represented in Fig. 2.2.
Batch processing is typically applied for small-volume products and in cases
where the fundamental mechanisms of the reaction are not well known. This issue of
robustness to incomplete knowledge is of extreme importance for the production of
fine chemicals in a multipurpose environment. Batch processes often use complex
chemistry of which substantially less is known than a typical continuous process. The
cost of evaluating kinetics and physical parameters to the accuracy required to use
standard chemical engineering design methods would be far too high. However, such
detailed analysis is seldom necessary. It is usually sufficient to know how long an
operation will take and even that need not be known to excessive accuracy. The use
of rules of thumb for scale-up based on identification of the rate-controlling process
 2.2 Characteristics of production processes 13

Fig. 2.2: Schematic representation of a batch process operation.

is a common way of assessing the time taken for an operation on the full scale. Dis-
crepancies between the expected and actual times for each operation tend to average
out over the many operations that constitute a single batch. Thus, the impact of inac-
curate knowledge is much less serious than for a continuous process whose overall
productivity is limited by the capacity of whichever unit has lowest throughput.
Besides robustness, batch production plants offer us the second advantage of
extreme flexibility. In general, the plant used, typically employing stirred vessels
of either stainless or glass-lined steel of 1–50 m3 in volume, is easily modified for
use on new products. Such equipment is very versatile and can be used to blend
reactants, heat them to reaction temperature, carry out the reaction, cool, distil off
solvent and crystallize the product. In a continuous process, each operation would
be carried out in a separate unit.
Small-scale processes and processes in which solids occur are likely to be
batch. Numerous chemical process industries retain batch processing as their pri-
mary method of manufacture. Many of these continue to be made batch wise be-
cause quality is more important than price. The product has traditionally been
made so, or the industry is not large or technically sophisticated enough to operate
successfully in a continuous mode. Typical products manufactured by batch pro-
cesses include pharmaceuticals, agrochemicals, dyestuffs, photosensitive materi-
als, food additives, perfumes, vitamins and pigments.

2.2.2 Continuous processes

For large production capacities where the process reaction mechanism is better
known and reaction rates are not too slow, continuous processing is often possible.
14 2 The structure of chemical and biochemical process systems

Here, the raw materials are prepared and fed to the reactor continuously. The reactor
system is sized so that the materials reside in it long enough at the reaction condi-
tions to achieve the desired extent of reaction. The reaction system may be a single
vessel or a number of reactor vessels in series, each operating at different conditions.
The product leaves the reaction zone continuously and passes to a sequence of sepa-
ration steps where the desired products are obtained in continuous streams. Un-
reacted feed materials are obtained in other streams and continuously returned to
the reactor. Any by-products are also removed.

Gaseous waste

Air pollution
control
Raw
material
Feed Product X
A
purifier purifier
for A

Initial Product X
Reactor product
separation
Product Y
Raw
material
B Feed
purifier Product Y
for B purifier

Waste product
purifier

Liquid/solid waste

Fig. 2.3: Typical continuous process plant.

Figure 2.3 shows a possible configuration for a typical continuous process plant.
Two raw materials are fed to a reactor after each is purified. The reactor effluent is
separated in three separation steps, and all waste streams are treated before release
to the environment. Product X might be the main product desired and product Y a
salable by-product. Ideally, such a process operates under steady-state condi-
tions, that is, a stable operating condition where none of the process parameters
(temperature, pressure, process stream composition, flow rate, etc.) vary with time.
In any real process, there will be a period of adjustment as the plant is started or
stopped, and there will be disturbances as the process operates. The process con-
trol system attempts to minimize the effects of these process upsets.
 2.3 Unit operations 15

In a plant operating under steady-state conditions, variables are different from

point to point along the process path. But if you were to take a photograph of the
control panel, where an array of instruments records the process conditions at all
the crucial points in the process, you would see no differences between a picture
taken at 8 a.m. and one taken at 8 p.m. Some basically continuous processes have
components, for example, dryers, filters and ion exchange beds that operate cycli-
cally. These units must be taken off-stream periodically for regeneration. The period
of on-stream operation may be several hours to several days.
Most large-scale processes operate continuously, especially ones in which gases
and low-viscosity liquids are handled. Petroleum refining, the manufacture of bulk
chemicals and industrial gas manufacturing are typical examples.

Fig. 2.4: Flowchart of an atmospheric crude oil distillation train.

2.3 Unit operations

Despite the very large number of chemical processes and products, there are only a mod-
est number of different kinds of chemical process steps. This has allowed an economical
method of organizing the field of chemical engineering into manageable segments.
These segments are called unit operations and have been defined on two principles:
16 2 The structure of chemical and biochemical process systems

(1) Although the number of individual processes is great, each one can be broken
down into a series of operations that appear in process after process.
(2) The individual operations are based on the same scientific principles. For
example, in most processes, solids and fluids must be moved, heat or other
forms of energy must be transferred from one substance to another, and tasks
like drying, size reduction, distillation and evaporation must be performed.

Most of the unit operations are used to conduct the primarily physical steps of prepar-
ing the reactants, separating and purifying the products, recycling unconverted reac-
tants and controlling the energy transfer into or out of the chemical reactor. Typical
examples are operations such as distillation, evaporation, liquid–liquid extraction, fil-
tration, drying, heat exchange, mixing, classification, crystallization and adsorption.
When a process step involves a chemical change, it is sometimes called a unit pro-
cess, or, more appropriately, a chemical reaction step.
The consequence of this way of thinking is that a process designer regards a
plant first and foremost as a collection of operations connected by a network of
pipes. It requires a certain amount of thinking in systems to design a process opti-
mally. The resulting network is called a flowchart. Such a flowchart generally con-
tains the mass and energy balances for all the operations. As illustrated in Fig. 2.4,
a flowchart can be quite complicated, the more so since every unit process can be
regarded as a subsystem.
Because the unit operations are a branch of engineering, they are based on
both science and experience. Each process step can be carried out in a variety of
equipment types. Theory and practice must combine to yield designs for equipment
that can be fabricated, assembled, operated and maintained. Usually the apparatus
selected is chosen because it has some particular advantage in light of the properties
of the materials being processed or the goal of the process step.

2.3.1 Reactors

The reactor in which the chemical reaction takes place occupies a central position in
the chemical process. In size and appearance, it may often seem to be one of the
least impressive items of equipment, but its demands and performance are usually
the most important factors in the design of the whole plant. The reactor provides the
volume necessary for the reaction and holds the amount of catalyst required for the
reaction. When a new chemical process is being developed, at least some indication
of the performance of the reactor is needed before any economic assessment of the
project as a whole can be made. An essential factor in this economic assessment is
the formation of unwanted by-products, which directly affect the operating costs of
the process. In most cases, the design of the reactor has a great effect on the amount
of by-products formed and therefore the size of the separation equipment required.
 2.3 Unit operations 17

Reactant
Coolant
inlet Product
inlet
outlet

(a) (b)
Coolant
outlet

Coolant Reactant
inlet inlet

Reactant
inlet Catalyst
Steam or
cooling
water
Product
outlet

Coolant (c) Product (d)

outlet outlet

Fig. 2.5: Various common reactor types: (a) agitated batch reactor, (b) continuous stirred tank
reactor, (c) tubular reactor and (d) multitubular packed bed reactor.

The design of a reactor and its mode of operation can thus have profound repercus-
sions on the remainder of the plant.
Figure 2.5 shows several common types of reactors. The agitated batch reactor
shown in (a) is an extremely common device. The jacket can be used to heat or cool
the reactor, typically with steam or cooling water. The vessel may be built with
thick walls so that the reactions can take place under pressure. There may be vari-
ous ports for feed addition and product withdrawal. In many cases, baffles are used
on the inside to prevent vortexing of the liquid and to improve mixing. Normal con-
struction materials include glass-lined steel, stainless steel, carbon steel and vari-
ous corrosion-resistant alloys. Internal cooling coils are sometimes used to provide
additional heating or cooling capacity.
Sketch (b) shows a continuous stirred tank reactor. This is essentially identi-
cal to the agitated batch reactor but is operated continuously. Thus, feed and prod-
uct are continuously added and removed. Obviously, it is not possible to operate
this reactor in a way that every fluid molecule stays in for the same length of time.
Fairly intense agitation is usually employed to keep the reactor content uniform.
However, the degree of mixing decreases as the size of reactor increases.
18 2 The structure of chemical and biochemical process systems

The tubular reactor shown in (c) is the most common type of reactor for reac-
tions where large amounts of heat have to be supplied or removed. This can be
achieved by burners or a heating/cooling fluid on the outside of the tubes. The tu-
bular reactor is also widely used for highly exothermic solid-catalyzed reactions as
multitubular packed bed reactor (d).

2.3.2 Recovery, purification and fractionation technologies

Separation processes constitute more than half of the total equipment investment
for the chemical and fuel industries. They are also widely used in pharmaceutical
and food industries, mineral processing industry and a variety of other industries.
Separation processes may have a number of purposes, which can be loosely catego-
rized as follows:
– Recovery or concentration: increasing the desired substance concentration in
a solution, usually by removal of a substantial fraction of solvent
– Purification: removal of impurities from the final product
– Fractionation: separation of desired substances from one another

Separating the desired product or products from the reaction mixture is often a
complex and therefore expensive process. During the chemical and biochemical
conversion, mixtures are generated that contain many different components includ-
ing the product, undesired side products, unconverted raw materials, solvents, cat-
alysts and so on. All these components can exist in different states: gas, liquid or
solid. When all components are present in the same state, the mixture is called ho-
mogeneous. Typical examples are gas mixtures (air = oxygen + nitrogen + carbon
dioxide) or liquid mixtures (sugar in water, ammonia in water, petrol, naphtha). If
the components are present in different states the mixture is called heterogeneous.
Solid–liquid mixtures (melting ice, water–sand slurries), solid–gas mixtures (dust
in air) and liquid–gas mixtures (droplets in air, bubbles in water) are typical exam-
ples of heterogeneous mixtures.
The separation of homogeneous mixtures and the separation of heterogeneous
mixtures require totally different techniques and separation principles. Separation
technologies for homogeneous mixtures are used to separate on a molecular basis
and therefore referred to as molecular separations. Technologies for heteroge-
neous mixtures are usually called mechanical separations because they are based
on mechanical principles.

2.3.2.1 Molecular separations

Homogeneous mixtures with a molecularly dispersed distribution of individual
components can only be separated with a molecular separation process. In these
 2.3 Unit operations 19

processes, mass and often heat is exchanged between at least two phases of differ-
ent composition. The phases are the mixture phase(s) and a selective auxiliary
phase. This auxiliary phase is generated the introduction of an energy separating
agent such as heat and refrigeration or by means of a mass separating agent such
as a solvent, adsorbent or ion exchange resin. The separating agent serves to create
the second phase and thereby form the required driving forces, concentration and
temperature gradients. An overview of the main molecular separation technologies,
their separation principle and used separation agent is given in Tab. 2.1.

Tab. 2.1: Overview of main molecular separation technologies.

Separation principle Phase contact Separation agent Technology

Difference in volatility Gas–liquid Heat transfer Evaporation

Distillation
Azeotropic distillation

Solvent and heat transfer Extractive distillation

Liquid absorbent Gas absorption

Stripping gas Stripping

Liquid–solid Heat transfer Drying

Difference in solubility Liquid–liquid Solvent Liquid–liquid extraction

Solid–liquid Solid–liquid extraction

Solid–liquid Leaching

Difference in solubility or Solid–liquid Heat transfer Crystallization

melting point

Difference in adsorbability Gas–solid Solid adsorbent Gas adsorption

Liquid–solid Liquid adsorption

Difference in permeability Liquid, vapor Membrane Membranes

and/or solubility

2.3.2.2 Mechanical separations

The separation of heterogeneous mixtures is usually accomplished by exerting
forces on the mixture that has to be separated. These forces move the components
that comprise the mixture in such a way that a separation is obtained. Different
forces are used in the different mechanical separation technologies:
– Gravity
– Centrifugal
– Impingement
20 2 The structure of chemical and biochemical process systems

– Electrostatic
– Magnetic

Many commercial separation operations also combine these separation principles,

sometimes in the same apparatus or otherwise in different pieces of equipment in
series. An overview of the different mechanical separation technologies and their
basic separation principles is given in Tab. 2.2.

Tab. 2.2: Overview of the main mechanical separation technologies and their application areas.

Technology Separating Application area

principle
Solid–solid Liquid–solid Gas–solid Gas–liquid Liquid–liquid

Sorting Gravity X

Classifiers X

Sieves X

Settlers X X

Filtration Pressure X

Presses X

Centrifuges Centrifugal X X

Cyclones X X X X

Fabric filters Impingement X X

Wet scrubbers X X

Electrostatic X
precipitators

2.3.3 Product finishing operations

In recent decades, the chemical industry has moved away from commodity chem-
icals toward products of higher added value such as specialty chemicals and con-
sumer products. These materials are often complex multiphase materials such as
pharmaceutical tablets and creams, cosmetic creams and lotions, ceramic and plas-
tic products, ice cream and margarine, industrial paints and adhesives, fertilizer
granules and so on. The quality and properties of these products is no longer deter-
mined solely by the concentrations achieved in the separation operations. End con-
sumers generally judge products according to their end-use properties, such as
taste, smell, feel and handling properties rather than their chemical composition.
These end-use properties are typically linked to chemical and biological stability,
 2.3 Unit operations 21

degradability, chemical, biological and therapeutic activity, aptitude to dissolution,

mechanical, rheological, electrical, thermal, optical, magnetic characteristics for
solids and solid particles together with size, shape color, touch, handling, cohe-
sion, friability, rugosity, tastes, succulence, esthetics, sensory properties and so on.

Formulation Manufacturing

Microstructure

Product properties

Fig. 2.6: Influence of formulation and processing on product properties.

An important characteristic of these industrial products is that they all possess a sig-
nificant microstructure which is, as illustrated in Fig. 2.6, very dependent upon the
product formulation (recipe) as well as the manufacturing conditions (technologies,
process). Product finishing technologies are concerned with physical or physico-
chemical principals, which add value to a product. Typical engineered products are:
– Structured solids such as catalyst carriers and coated pharmaceuticals. A cata-
lyst carrier must be of a given shape and must have a defined porosity and inner
surface with a given pore size distribution. Coated pharmaceutic granules may
have an improved taste and often release their active ingredients in a controlled
and retarded way.
– Particulate solid systems concern crystalline, polymeric or amorphous solids
that represent over 60% of all products that chemical companies sell to their
customers. Examples are fertilizers which have to be stored without caking and
which have to be handled and applied without dust formation. Other solid sys-
tems are some pharmaceuticals and vitamins which have to be specially formu-
lated to guarantee their bioavailability. These materials need to have a clearly
defined physical shape in order to meet the designed and the desired quality
standards.
– Emulsions, colloids, dispersions, suspensions, sprays, gels and foams con-
cern complex media for which rheology and interfacial phenomena play a major
role. Also involved are the so-called soft solids, systems which have a detectable
yield stress, such as ceramic pastes, foods or drilling muds.

The main characteristics of product finishing technologies are that quite different
unit operations are used, involving less reaction and separation tasks and more struc-
turing and stabilization tasks. Structuring processes are the opposite of separation
processes. Man-made structured products use assembly, structuring or texturizing
22 2 The structure of chemical and biochemical process systems

processes, for example, crystallization and emulsification processes (e.g., margarines,

mayonnaises, ice creams, paints and detergents), foaming (e.g., insulating materials,
shaving cream and whipped creams), precipitation, granulation, agglomeration, dry-
ing, extrusion, compression, prilling, shaping, micronization, dough making and
baking. The end product is often a complex microstructure of dispersed phases held
together by binding forces and a continuous phase. The product microstructure leads to
the desired product functionality in use. Stabilization processes are the opposite of
transformation processes. Two major processes can be identified. The first, encapsula-
tion, provides a barrier between two reacting species. For instance, to preserve the integ-
rity of the ingredients or accomplish intelligent functions such as controlled reactivity or
programmed release of active components that may be obtained by multiple layer coat-
ings. The second, to combat spoilage, is rather typical for the food industry and pharma-
ceutical products. Naturally structured foods often use preservation or stabilization
processes in which the main aim is to eliminate microbial, enzymatic or chemical spoil-
age of the raw materials, which are usually food tissues (fish, meat and vegetables).

Fig. 2.7: Schematic of a single pass countercurrent shell-and-tube heat exchanger.

2.3.4 Other important process units

In addition to purification and reaction, chemical processes usually include steps

to heat or cool process streams and devices to move fluids. Heating and cooling de-
vices include furnaces, air coolers and heat exchangers. Furnaces and air coolers
are familiar from your experiences with automobile radiators, household furnaces,
refrigerators and air conditioning units. Fluid-to-fluid heat exchangers are not so
familiar, but they are very common in chemical processes. The most common of
these heat exchangers, the shell-and-tube heat exchanger, is shown in Fig. 2.7. In
this unit, one fluid flows through the shell over the outside surfaces of the tubes.
Baffles are usually used to increase the velocity of the fluid passing through the
 2.3 Unit operations 23

shell. A second fluid enters the tubes, flowing through them in parallel in one or
more passes. As it flows through the exchanger, the cold fluid is heated by heat
transferred through the tube walls. At the same time, the hot fluid is cooled. The
figure shows inlet and exit nozzles for two fluid streams. These streams could be
gas or liquid and could change phase within the heat exchanger.
Fluid motion in chemical processing is generally produced by pumps or, if
gases are being moved, by blowers and compressors. The most common type of
pump is the centrifugal pump shown in Fig. 2.8a. Liquid flows into this pump and
is accelerated into high-speed circular motion by the vanes of the pump impeller.
The liquid exits into the pump volute, where it slows down, converting at least part
of the kinetic energy into pressure. Because of the mechanism of its operation, the
performance of this pump is sensitive to the pressure that it develops. The higher
the pressure rise across the pump, the lower the pump capacity is. Thus, the pres-
sure that the pump produces will decrease as the throughput through the pump is
increased. Pump efficiency also depends on flow rate. The other common type of
liquid pump is a positive displacement pump illustrated in Fig. 2.8b. Capacity is
directly related to the volume swept out by a piston operating in a cylinder or to the
frequency with which a gear tooth enters the cavity between other like teeth. Pres-
sure rise has much less of an effect on the capacity of positive displacement pumps.

Outlet

High
pressure
Discharge

Casing
Vanes

Low
pressure
Suction
Impeller Inlet

(a) (b)

Fig. 2.8: Schematic of a (a) centrifugal and (b) positive displacement pump.

Gas compressors operate on the same principle as do liquid pumps but usually
handle larger volumes and operate at higher speeds. Since large amounts of work
24 2 The structure of chemical and biochemical process systems

are used to compress gases, cooling is usually needed during and after compres-
sion. Reciprocating, centrifugal and axial-flow compressors are commonly used in
the chemical process industries. Figure 2.9 shows a schematic of a double piston
gas compressor which are used in the high-pressure polyethylene process for the
compression of ethylene in multiple stages up to pressures of 3,000 bar with cooling
in between the stages.

Inlet Inlet

Discharge Discharge

Fig. 2.9: Schematic of a double piston compressor.

2.4 Process synthesis

The development of a commercial product from a laboratory chemical involves the tal-
ents and efforts of many people. At the laboratory stage, the market potential of the
product is estimated. The physical and chemical properties of the chemicals involved in
the process are then determined, and the conditions under which the product can be
produced in the laboratory are explored. But a long and complex effort still remains.
There are times when an engineer is called upon to devise a plausible process
long before all of the development effort has taken place. Perhaps a decision
whether to invest in the development effort is required. If a tentative process can be
suggested, the cost and difficulty of the development of the process can be esti-
mated. Also, a rough estimate of the cost of the product can be calculated, and the
size of the market can be forecasted. Like most economic forecasts, these guessti-
mates are subject to an enormous amount of uncertainty. Accordingly, many tech-
nically and economically sound processes and products have been shipwrecked on
the rocks of poor marketing forecasts.
The development of a process scheme involves coming up with that configura-
tion of processing steps that efficiently and safely produces the desired product. An
enormous amount of art, skill, intuition and innovation goes into developing the
processing scheme. Literally millions of designs are possible. One of the tasks of a
 2.4 Process synthesis 25

process engineer is to choose from these possibilities, taking into account the many
conditions set by product markets, geographical location of the plant, the social sit-
uation, legal regulations and so on. This is not only important in choosing among
existing processes but also in developing new processes. This process synthesis
step is where vast amounts of money can be made or lost and where a good, inno-
vative chemical engineer can be worth his or her weight in gold.
These activities are not merely a straightforward application of the scientific disci-
plines on which chemical technology is based (chemistry, physical transport processes,
unit operations and reactor design). It is necessary to select relevant knowledge from
these fields, combine different aspects and interpret these quantitatively. This means
integration of knowledge from various fields of science. With such complicated systems
as chemical processes, some of the questions will inevitably be answered in a semi-
quantitative or even qualitative way. Typical questions that must be answered as the
engineer conceives and develops a process to make a marketable product:
1. What reaction steps are required to get the product?
2. What is the best type and size of reactor to use, and what are the optimum reactor
operating conditions (temperature, pressure, agitation, catalyst concentration etc.)?
3. What is the optimum reactor conversion, and how does it affect the design and
operation of the downstream separation steps? The optimization must incorpo-
rate the entire plant.
4. Will the catalyst degrade or be poisoned?
5. What side reactions occur? What will the likely by-products be? What effect
will they have on yield and performance?
6. What are the best raw materials? Air, water, petroleum, natural gas, coal, min-
erals and agricultural products are the basic raw materials. However, a host of
semiprocessed intermediates may also be used.
7. How can the raw materials be brought to conditions suitable for the reaction?
Usually, several purification steps are needed, as well as heating and compress-
ing to the appropriate conditions.
8. How can the products and by-products be separated and purified to meet mar-
ket specifications?
9. Should cooling water be used, or should air-cooling be considered?
10. Are any of the materials used, produced or present in the process toxic or carci-
nogenic? Are there other health or safety hazards in the process? Is there a po-
tential for hot spots or explosions in the reactor? Should the reactor be shielded
and remotely operated?

All of these questions have several possible answers. Each choice the engineer
makes has technical, economic, social and political repercussions. The engineer is
expected to make prudent and wise choices, and the impact on the environment
must be considered. In many cases, experience is a necessary asset to assist sound
intuition and judgement.
3 Principles of chemical reaction engineering

3.1 Introduction

Design of a chemical reactor is no routine matter, and many alternatives can be

proposed for a process. In searching for the optimum it is not just the cost of the
reactor that must be minimized. One design may have low reactor cost, but the ma-
terials leaving the unit may be such that their treatment requires much higher cost
than the alternative design. Hence, the economics of the overall process must be
considered. Reactor design uses information, knowledge and experience from a va-
riety of areas:
– thermodynamics
– chemical kinetics
– fluid mechanics
– heat transfer
– mass transfer
– mechanical engineering
– economics

Chemical reaction engineering is the synthesis of all these factors with the aim of
properly designing a chemical reactor. The design of chemical reactors is probably
the one activity which is unique to chemical engineering, and it is probably this
function more than anything else which justifies the existence of chemical engi-
neering as a distinct branch of engineering.
In reactor design, we want to know what size and type of reactor and method
of operation are best for a given job. To establish the actual behavior of a reactor for
a certain application, two major basic questions have to be answered:
– What changes can we expect to occur?
– How fast will these changes take place?

The first question concerns the thermodynamics, the second the various rate pro-
cesses (chemical kinetics, heat transfer, etc.). Tying these all together and trying to
determine how these processes are interrelated can be an extremely difficult prob-
lem. Since this is far beyond the scope of this course, the content of this chapter is
limited to the most essential basics and some simple situations that provide a basis
to discuss and appreciate the work of chemical reaction engineers.

https://doi.org/10.1515/9783110712445-003
28 3 Principles of chemical reaction engineering

3.2 Classification of reactions

There are many ways of classifying chemical reactions, see Table 3.1. In chemical reac-
tion engineering, probably the most useful scheme is the breakdown according to the
number and types of phases involved, the big division being between homogeneous
and heterogeneous systems. A reaction is homogeneous if it takes place in one phase
alone. A reaction is heterogeneous if it requires the presence of at least two phases to
proceed at the rate that it does. It does not matter whether the reaction takes place in
one, two or more phases, or at an interface, or whether the reactants and products are
distributed among the phases or are all contained within a single phase. All that counts
is that at least two phases are necessary for the reaction to proceed as it does.
Sometimes this classification is not clear-cut as with a large class of biological
reactions, the enzyme substrate reactions. Since enzymes themselves are highly
complicated large-molecular-weight proteins of colloidal size, enzyme-containing
solutions represent a gray area between homogeneous and heterogeneous systems.
Other examples for which the distinction is not sharp are the very rapid chemical
reactions, such as the burning gas flame where large nonhomogeneity in composi-
tion and temperature may exist.
Cutting across this classification is the catalytic reaction whose rate is altered
by materials that are neither reactants nor products. These foreign materials, called
catalysts, need not be present in large amounts. Catalysts act somehow as go-
betweens, either hindering or accelerating the reaction process while being modi-
fied relatively slowly if at all.

Tab. 3.1: Classification of chemical reactions useful in reactor design.

Noncatalytic Catalytic

Homogeneous Most gas-phase reactions Most liquid-phase reactions

Fast reactions such as burning of Reactions in colloidal systems

a flame
Heterogeneous Enzyme and microbial reactions

Burning of coal Ammonia synthesis

Roasting of ores Oxidation of ammonia to produce
nitric acid
Attack of solids by acids
Incineration of waste Cracking of crude oil
Reduction of iron ore to iron and steel Electrochemical production of
hydrogen and chlorine
 3.3 Rate of chemical reactions 29

3.3 Rate of chemical reactions

For the application of material balances to chemical reaction engineering problems

an expression is required for the chemical reaction rate. The reaction rate of a com-
ponent is defined as the number of moles produced or consumed per unit time and
per unit volume. From this definition, it follows that the chemical reaction rate is
negative for reactants and positive for products. In many cases, A and B are used
as symbols for a reactant and P is the symbol for a product. In the reaction equation:

νA A + νB B ! ν P P (3:1)

νA, νB and νP are stoichiometric coefficients for the respective components A, B

and P. These stoichiometric coefficients relate the relative reaction rates of the indi-
vidual components:
νA νA
ð− RAÞ = ð− RBÞ = ðRPÞ (3:2)
νB νP

It should be noted that the chemical reaction rate only reflects the chemical kinetics
of the system. The reaction rate generally depends on the composition of the reac-
tion mixture (most importantly the local concentrations of each of the reactants), its
temperature and pressure and the properties of the catalyst.

3.3.1 Effect of concentration

For relatively simple reactions, it is usually postulated that the rate-controlling

mechanism involves the collision or interaction of a single molecule of A with a sin-
gle molecule of B. This means that the reaction rate is proportional to the con-
centration of each of the reactants, since the number of molecular collisions per
unit time is proportional to the amount of molecules of each of the reactants. Such
reactions are called elementary reactions. For example, in the case of a bimolecu-
lar elementary reaction:

A+B ! P (3:3)

the rate of disappearance of reactant A at a given temperature is proportional to the

concentrations CA and CB of both reactants, with a proportionality constant called
the reaction rate constant, kA:

− R A = k A CA CB (3:4)

The order n of a reaction is the power dependence of the reaction rate on the concen-
tration of each reactant. The reaction in the example above is first order in A and first
order in B. For nonelementary reactions, the reaction rate is a result of multiple ele-
mentary reactions, leading in general to a complicated dependence on the reactant
30 3 Principles of chemical reaction engineering

concentrations. In such cases, for a limited range of concentrations, an effective reac-

tion order can still be defined for each reactant. We will show later how the effective
reaction order can be determined experimentally in a batch reactor.

EA

Fig. 3.1: The potential energy curve for a

Reactants Intermediates Products chemical reaction with activation energy EA.

3.3.2 Effect of temperature

The effect of temperature on a chemical reaction is most easily explained by the

transition state theory. Thermodynamics tell us that a chemical reaction will only
proceed when an energetically more favorable situation is obtained. The reaction
pathway toward this more stable situation usually proceeds through the formation
of less stable intermediates by the breakage of chemical bonds, which subsequently
decompose or form new bonds into the thermodynamically more stable products.
This process is schematically represented in Fig. 3.1, where the potential energy of
starting, intermediate and end situation is shown. From Fig. 3.1, it can be seen that
activation energy, EA, has to be provided to allow a chemical reaction to proceed.
In reaction rate expressions, this activation energy is used to separate the influence
of temperature and composition on reaction rate. The actual representation of the
dependence of the reaction rate constant kA on temperature T is done through an
exponential probability function, better known as the Arrhenius relation:


− EA
kA = kA, ∞ exp (3:5)
RT

In this equation, R represents the gas constant (8.3144 J/mol K) and the pre-
exponential factor kA,∞ is called the frequency factor. Although the frequency factor
has a weak dependence on temperature, this is usually ignored because of the over-
whelmingly stronger temperature dependence of the exponential part. For most reac-
tions, the activation energy lies in the range of 40–300 kJ/mol, resulting in an increase
of the reaction rate constant by a factor of 2–50 for a temperature rise of 10 °C.
 3.3 Rate of chemical reactions 31

3.3.3 Chemical equilibria

So far, it has been assumed that the reactions are irreversible. In practice, many
reactions are reversible, meaning that the products can be converted back into the
reactants again:
k1
A+B!P (3:6)
k−1

For an elementary equilibrium reaction, the rate of formation of P by the forward

reaction and its rate of disappearance by the reverse reaction are now given by

RP,forward = k1 CA CB (3:7)

−RP,reverse = k − 1 CP (3:8)

Because at equilibrium there is no net formation of P, the reaction equilibrium

constant, KR, can be obtained from the condition Rp,forward + Rp,reverse = 0:

Cp k1
KR = = (3:9)
CA CB k−1

What this equation shows is that the forward and reverse reaction rates are not in-
dependent, but related through the equilibrium constant. Thermodynamics allows
the calculation of the equilibrium constant from the standard free energies of for-
mation ΔGof of the reacting components. For the considered reaction, this results in
the following relation for the standard free energy of reaction ΔGoR and the reac-
tion equilibrium constant KR:

ΔGoR = ΔGof , P − ΔGof , A − ΔGof , B = −R T ln KR (3:10)

Note that the equilibrium constant KR depends only on temperature and not on
pressure. Using Eq. (3.10) and standard thermodynamic relations, it can be shown
that the temperature dependence of the equilibrium constant is given by the Van ‘t
Hoff equation:

d ln KR Δh0 R
= (3:11)
dT RT 2
Here, Δh0R is the standard enthalpy of reaction, which is the heat of reaction pro-
duced in an exothermic reaction (Δh0R < 0) or heat of reaction consumed in an en-
dothermic reaction (Δh0R > 0). The Van ‘t Hoff equation shows that increasing the
temperature decreases the equilibrium constant for an exothermic reaction, moving
the equilibrium toward the reactant side, while it increases the equilibrium con-
stant for an endothermic reaction, moving the equilibrium toward the product side.
32 3 Principles of chemical reaction engineering

With the equilibrium constant known, the expected maximum attainable yield
of the products of the reaction can be estimated. An industrially important example
where the maximum attainable conversion is limited by the thermodynamic equi-
librium is the synthesis of ammonia from nitrogen and hydrogen:

N2 + 3 H2 ! 2 NH3 ðΔ Hr,o s = −45.3 kJ=mol NH3 Þ (3:12)

As a result of the exothermic nature of the reaction and the volume contraction by
conversion to ammonia, it is necessary to operate at relatively low temperatures
and high pressures in order to move the equilibrium to achieve economically viable
production rates. This is illustrated in Fig. 3.2, where the ammonia content of the
equilibrium mixture is plotted as a function of pressure at various temperatures.
Economically favorable conversion rates can only be obtained by catalyzing the re-
action. Iron catalysts give good conversions at about 30 MPa and 500 °C in reactors
of acceptable dimensions. Other typical examples of reactions in which the maxi-
mum attainable conversion is limited by the thermodynamic equilibrium are dehy-
drogenations (i.e., ethyl benzene to styrene), esterifications and polycondensations
(i.e., polyesters, polyamides).

100
200 °C
90
300 °C
Mole% NH 3 at equilibrium

80

70 400 °C

60

50
500 °C
40

30
600 °C
20

10 700 °C

0
0 20 40 60 80 100
pressure (Mpa)

Fig. 3.2: Equilibrium yield of NH3 from N2 and H2.

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“If only I had a wireless signal book,” he sighed. “It may be hard to
raise anybody, for I don’t know a single local call. Probably I’ll have
to send out an SOS. What is the nearest place where they would be
likely to have a Marconi station?”
“Probably San Antonio.”
“How far is that in a straight line?”
“I don’t know exactly. Perhaps a hundred and twenty-five miles—
possibly a hundred and thirty.”
Roy looked at his batteries dubiously. “I’ll make the effort anyway,”
he said. “Maybe they’ll carry that distance.”
“I hope you can get them,” said Roy’s host anxiously. “We need help
badly. We especially need soldiers. Looting has begun.”
“Soldiers!” cried Roy. “Why didn’t I think of them before? There’s an
army post at Brownsville. How far is that?”
“About the same distance as San Antonio.”
“Thank heaven I know their call signal,” cried Roy.
He pressed his finger to his key. Blue sparks leaped across his spark-
gap. “WUZ—WUZ—WUZ,” he flashed.
Then he sat breathless and listened. Would his battery carry far
enough? There was no answering signal.
“WUZ—WUZ—WUZ,” flashed out Roy. Then once more he sat tense,
listening.
Something crackled in his ear. “Who is calling WUZ?”
“Corpus Christi,” flashed back Roy. “City terribly damaged by tidal
wave. Scores drowned. Hundreds of houses washed away. Property
loss millions. Need food, medicines, workers, soldiers. Looting has
begun. For God’s sake rush help. Gordon Boone, Mayor.”
“Who is this talking?” came the reply. “Never heard of a wireless
station at Corpus Christi.”
“This is Roy Mercer, shipwrecked wireless man, talking on
emergency outfit for city authorities. Call ABC.”
So Roy sent abroad the news of the city’s plight, even as Paul
Revere carried to every Middlesex village and farm the news of
Lexington’s peril. Next morning soldiers marched into the city. Martial
law was declared. Sentries were posted. Corpus Christi was safe.
Other helpers rushed to the stricken community. A Red Cross relief
train sped to the rescue. The Salvation Army sent workers.
Physicians and nurses came. Food and supplies poured in. The
stunned city pulled itself together. Workers were organized to search
out and care for the dead, to clear the streets, to look after the
homeless, to feed the hungry. Emergency tent camps arose.
Canteens were opened. Boy scouts collected clothes, carried
messages, and were the legs of the rescue work. And until
telephonic communication was restored, Roy sat at his instrument
hour after hour, sending and receiving messages for the stricken city.
The air and the sea brought help. An army aviator dropped thirty
pounds of sorely needed yeast into the city. The flood had spoiled all
existing stocks. As soon as the sea subsided, boats rushed to Corpus
Christi, bearing gifts. The sea-going tug Rotarian came from
Galveston, carrying money, supplies, and workers.
When Roy learned of the Rotarian’s arrival he sought her out and
went aboard. The captain met him as he came up the gangplank.
“Can you tell me anything about the Lycoming or the Empress?”
demanded Roy.
“Both safe in Galveston,” said the tug’s skipper. “They are pretty
badly battered up, but still sound. They had an awful fight to make
it. The Empress broke her rudder and the Lycoming took her in tow.
Nobody but John Lansford could have done it. I tell you he’s a
wonder—heart like a woman’s—courage like a grizzly—rough as
barnacles on a ship’s bottom. The worst storm that ever blew—and I
guess this was it—couldn’t make him desert a ship in trouble. He
was darn near to port, he was, and didn’t he turn back into the
hurricane and take the Empress in tow. Saved her, too. Put an oil
slick down, got lines aboard of her, and had her turn her engines
just enough to give her headway. His lines would have parted in a
minute if he’d had to pull her whole weight. Oh! He’s a wonder all
right. It was a great rescue—great!”
“Was—was anybody lost?” asked Roy, hesitating.
“Small boat’s crew, including the third mate and the wireless man.”
“And nothing has been heard from them?”
“Absolutely nothing.”
“I am the wireless man,” said Roy quietly.
“The deuce you are!” exclaimed the Rotarian’s captain. “The deuce
you are! Put her there,” and he shook Roy’s hand warmly for a full
minute. “I’m mighty glad you pulled through. They say you did great
work.”
Roy’s heart leaped with joy. At last recognition had come to him. His
captain had changed his mind about him. But to the tug’s captain he
said simply, “I’m glad to hear about the two steamers. I wish we
could get as good news of the third mate and the others in the life-
boat.”
“Aren’t they here with you?”
Roy told him how they had been lost. Then he added, “Will you take
me back to Galveston with you?”
“Surest thing you know,” exclaimed the captain.
So it happened that when the Rotarian, a few days later, tied up at
her pier in Galveston, Roy Mercer was the first person ashore. A
single glance told him that Galveston was unharmed. The captain
had already told him, however, how the sea-wall had saved the city.
Roy raced down the pier and up the gangplank to the Lycoming. The
first person he met was the third mate. Roy stopped dead in
astonishment, then sprang forward and grasped the mate’s hand.
“How did you get here?” he cried in astonishment.
The mate told him that after he, Roy, was washed away from the
others on the overturned boat, the life-boat was driven straight
toward the highest point on Mustang Island. A few sand-dunes
remained above the flood, and on these the crew found refuge. Two
of the sailors died from exposure, for they had to stay on their tiny
refuge, exposed to wind and rain, for fully forty-eight hours. Then
they got across Aransas Pass, found food and shelter, and later
made their way along the railroad to San Patricio, where they got a
train back to Galveston. Barring the sailors who died, all were back
on the Lycoming safe and sound.
Roy pressed on to the captain’s quarters. He was very eager to see
him. He felt sure that this time a warm welcome awaited him. He
rapped on the captain’s door.
“Come in,” said a rough voice.
Roy entered and stood before his commander. “I report for duty
again, sir,” he said.
The captain took his outstretched hand. “I’m glad you escaped,” he
said, “but you had no business in that small boat. Your post of duty
was in the wireless house. You left me in great difficulties. There
was no way to communicate quickly with the Empress. But I’m very
glad you escaped.”
 CHAPTER XIX
VICTORY

P oor Roy! He had come back expecting a warm welcome from the
captain and had been greeted with a reprimand. He backed out
of the captain’s room, and hot tears welled to his eyes despite his
effort to suppress them. He believed that he had come to
understand his captain. He believed that his roughness was but a
mask for a great heart. But it was evident he was wrong. The
captain had no heart. The captain cared nothing for him. The
captain still refused to change his mind about wireless. And that
meant that when the ship got back to New York Roy would pack his
bag and say farewell to her forever. He had done his best to win
recognition and failed. His errors were those of ignorance and
inexperience, not wilful wrongs. He had tried so hard to help save
the Empress. Now he was reprimanded for what he had done.
Suddenly a new thought came into Roy’s mind. “He said that I left
him in difficulties. He said that I left him in difficulties,” repeated Roy
to himself. “That means that I was useful to him and that he missed
my help. I see that it was wrong to leave my post. Others could row
the boat, but no one else could send wireless messages. But since
the two ships are safe, I’m glad I went. I’m glad something made
the old dragon realize that wireless is worth something.”
The purser and the first mate greeted Roy so warmly that it made
him forget his disappointment at the captain’s cold reception. In Mr.
Robbins and Mr. Young, at least, he had two firm friends. So long as
he lived, he would never forget them.
He went to his room and took off his torn and stained uniform. “I
ought to get another,” he muttered, “but I won’t. After I reach New
York I’ll probably never need a uniform.”
He dressed himself in the old suit he had worn the day he came to
New York. That was only three months previously, but Roy had seen
so much and gone through so much that it seemed like ages. What
Roy did not appreciate was how he had grown during those three
months—not in body, but in mind and character. The stern discipline
of his captain had held him so rigidly to his duty that it had become
second nature to do his duty. He had developed those very qualities
that his captain most desired in his subordinates, but apparently
could not see in Roy.
After a while Roy went down on the lower deck, where he heard the
sound of hammers and saws. Rails had been carried away, bulwarks
smashed, and many minor injuries done to the ship. But these could
be readily repaired and carpenters were working busily to remedy
the trouble. Meantime, the cargo was shooting into the hold as fast
as ever. When he had fully inspected the Lycoming, Roy went over to
the Empress. She was battered pretty badly. Roy went aboard and
made the acquaintance of Stimson, the wireless man. The latter
greeted him with the utmost cordiality and introduced him to the
ship’s officers, from the captain down. All expressed their gratitude
to Roy for the part he had had in their rescue. So Roy went back to
the Lycoming much happier in mind than he had been when he left
her.
Twenty-four hours later the Lycoming steamed out of the harbor.
Five days later still she lay at her dock in New York. It was Roy’s last
day aboard of her, he supposed, and he was depressed and sick at
heart. He had become fond of the ship and her crew. He had even
come to love his commander, though not in the way he loved the
purser. Just now he felt very hard toward Captain Lansford. He
expected the new wireless man would come aboard in a few hours.
Before he came, Roy wished to say good-bye to his friends, so that
he could leave promptly. He started for the purser’s office. On the
way, he passed a young man who inquired for the captain. Roy
directed him to the captain’s quarters, then turned away. He heard
the door open and the man say, “Captain Lansford, I’m the new
wireless man. The Marconi people instructed me to report to you for
duty.”
“New wireless man!” Roy heard the captain roar, and though he did
not mean to eavesdrop, he stood as though rooted to the deck.
“New wireless man!” cried the captain. “What do I want of a new
wireless man? I’ve got the best wireless man afloat. Go back and tell
’em so.”
“But I understood that you wanted to make a change—that your
present operator is too young.”
“You did, eh? Well, he is a bit young, but I can trust him absolutely.
And he’s got more brains than your whole outfit put together. It’ll be
a cold day when I go to sea without him. Good-day, sir.”
The surprised Marconi man turned about and made for the pier. Roy
fled to the wireless house. His heart was beating wildly. His whole
soul was singing. He had made good. The captain wanted him to
stay. The captain did like him, despite his rough manner. His
jubilation was so great he could hardly sit still.
Presently his brow puckered. How was he to get the captain to tell
him that he was to stay? An idea came to Roy. He jumped to his feet
and ran down to the captain’s cabin.
“Come in,” said a gruff voice, in answer to his knock.
“I’ve come to say good-bye, sir,” said Roy. “You know my three
months are up. I am sorry, sir, for I should like to stay on the
Lycoming. Good-bye, sir.”
The captain jumped to his feet. “Who told you to leave the ship?” he
roared.
“No one now, sir, but when I came aboard you said I was to stay
three months. The time is up. I supposed you wanted me to leave.”
“I don’t. That is, if I’ve got to have a wireless man aboard you might
as well stay. I don’t want to have to break another one in. You are
not relieved from duty. Go to your quarters, sir.”
Roy went back to the wireless house. The captain’s gruff words
could not still the song that his heart was singing. He had won. He
had made good. His captain liked him, perhaps loved him—in his
strange way. He thanked his lucky stars that he had been an
eavesdropper. Now he knew the truth about the captain. The skipper
of the Rotarian had told the truth. The rough manner was only a
mask to cover a great heart. All Roy’s pent-up affection went out to
this commander. He understood him now. Like the first mate and the
purser, he felt a genuine affection for his captain. It had taken a long
time to see beneath the surface, but nothing could now blind his
eyes. He understood his commander. And, best of all, he had made
good.
“Well,” he sighed joyfully, “I guess I’ll need a new uniform after all.”
 Transcriber’s Notes:
Punctuation has been made consistent.
Variations in spelling and hyphenation were retained as they appear in the original
publication, except that obvious typographical errors have been corrected.
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