Microreactors in preparative chemistry : practical aspects in bioprocessing, nanotechnology, catalysis and more / edited by Wladimir Reschetilowski.

Format:

Book

Contributor:

Reschetilowski, Wladimir, editor.

Language:

English

Subjects (All):

Microreactors.

Physical Description:

xv, 335 pages : illustrations ; 24 cm

Place of Publication:

Weinheim : Wiley-VCH, [2013]

Summary:

This is the first book in the field to focus on these aspects, providing extremely valuable information unavailable elsewhere for anyone seeking the practical application of microreactor technology in preparative chemistry. The topics covered branch out in three different directions. To begin with, the knowledge necessary for the preparative chemistry concerning the influence of the so-called microeffects on the reaction procedure and on mass and heat transfer as well as the surface phenomena are provided in detail. Next, practical aspects of the synthesis of various basic chemicals and fine chemicals, polymers, bioproducts and nanoparticles are discussed, including important advice for both the researcher and industrial chemist. Finally, reaction examples in microreactors whose reaction guidance are best understood are given together with universally applicable correlations as well as modeling approaches and transfer potential on related reaction systems. With its specific instructions, tips and experimental procedures for product syntheses as well as the inclusion of both the technical and theoretical background this is a must-have for beginners and experts alike working in this emerging field. Book jacket.

Contents:

1 Principles of Microprocess Technology / Wladimir Reschetilowski Reschetilowski, Wladimir 1

1.1 Introduction 1

1.2 History 2

1.3 Basic Characteristics 3

1.3.1 Microfluidics and Micromixing 4

1.3.2 Temperature and Pressure Control 5

1.3.3 Safety and Ecological Impact 7

1.4 Industrial Applications 8

1.5 Concluding Remarks 9

References 10

2 Effects of Microfluidics on Preparative Chemistry Processes / Madhvanand Kashid Kashid, Madhvanand, Albert Renken Renken, Albert, Lioubov Kiwi-Minsker Kiwi-Minsker, Lioubov 13

2.1 Introduction 13

2.2 Mixing 15

2.3 Heat Management 18

2.3.1 Heat Transfer in Continuous-Flow Devices 19

2.3.2 Heat Control of Microchannel Reactors 22

2.4 Mass Transfer and Chemical Reactions 26

2.4.1 Fluid-Solid Catalytic Systems 26

2.4.2 Fluid-Fluid Systems 31

2.4.2.1 Flow Regimes 32

2.4.2.2 Mass Transfer 34

2.4.3 Three-Phase Systems 36

2.4.3.1 Gas-Liquid-Solid Systems 36

2.4.3.2 Gas-Liquid-Liquid Systems 40

2.5 Flow Separation 40

2.5.1 Geometrical Modifications 41

2.5.2 Wettability-Based Flow Splitters 42

2.5.3 Conventional Separator Adapted for Microstructured Reactors 44

2.6 Numbering-Up Strategy 45

2.7 Practical Exercise: Experimental Characterization-of Mixing in Microstructured Reactors 46

References 50

3 Modular Micro- and Millireactor Systems for Preparative Chemical Synthesis and Bioprocesses / Frank Schael Schael, Frank, Marc-Oliver Piepenbrock Piepenbrock, Marc-Oliver, Jörn Emmerich Emmerich, Jörn, Joachim Heck Heck, Joachim 55

3.1 Introduction 55

3.2 Modular Microreaction System 57

3.3 Examples for Microreactor Applications 60

3.3.1 Synthesis of Vitamin A Acetate 60

3.3.2 Screening of Process Parameters for a Suzuki-Miyaura Reaction 62

3.3.3 Scale-Up of Thermal Rearrangement of Furfuryl Alcohol 64

3.3.4 Online Reaction Monitoring and Automation of Chemical Synthesis and Bioprocesses 66

3.4 Laboratory Exercise: Suzuki Reaction in a Modular Microreactor Setup 70

References 73

4 Potential of Lab-on-a-Chip: Synthesis, Separation, and Analysis of Biomolecules / Martin Bertau Bertau, Martin 77

4.1 Introduction 77

4.2 Learning from Nature: Analogies to Living Cells 77

4.3 Microenzyme Reactors 79

4.3.1 Enzyme Immobilization on the Microchannel Surface 80

4.3.2 Enzyme Immobilization on Supports 81

4.3.3 Modes of Operation 81

4.3.4 Enzymatic Conversions 81

4.3.5 Enzymatic Cleavage of Peptides 84

4.3.6 Determination of Inhibitor Properties 84

4.3.7 Cytotoxicity Assessment 87

4.4 Microchip Electrophoresis 87

4.4.1 Peptide Analysis 88

4.4.2 Chiral Separation 88

4.4.3 Coupling Biocatalysis and Analysis 88

4.4.4 Determination of Amino Acids in Goods and Foods 89

4.5 Microenzyme Membrane Reactor/Micromembrane Chromatography 89

4.6 Nucleic Acid Analysis in Microchannels 91

4.7 Saccharide Analyses in Microdevices 94

4.8 Practical Exercise: Lipase-Catalyzed Esterification Reaction 96

References 97

5 Bioprocessing in Microreactors / Fridolin Okkels Okkels, Fridolin, Dorota Kwasny Kwasny, Dorota 101

5.1 Introduction 101

5.2 Background 101

5.2.1 Basic Elements of a Biosensor 101

5.2.2 Different Sensing Methods 103

5.2.3 The Effect of Reducing Dimensionality and Length Scales of Biosensors 103

5.2.4 Biosensors Based on Field-Effect Transistors 104

5.2.4.1 The Main Working Principle of FET Sensors 105

5.2.4.2 Fabrication of SiNW FET Sensors 106

5.2.4.3 Functionalization of SiNW FET Sensors Using APTES 107

5.2.5 Shielding by the Buffer Combined Influence from Ions and Charge Carriers 107

5.3 Practical Exercise: Functionalization of Silicon Surface 108

References 113

6 Synthesis of Fine Chemicals / Sandra Hübner Hübner, Sandra, Norbert Steinfeldt Steinfeldt, Norbert, Klaus Jähnisch Jähnisch, Klaus 115

6.1 Introduction 115

6.2 Organic Synthesis in Liquid and Liquid-Liquid Phases 116

6.2.1 Fluorination Reactions 116

6.2.2 Reactions with Diazomethane 127

6.2.3 Ultrasound-Assisted Liquid-Liquid Biphasic and Liquid Reactions 134

6.3 Gas-Liquid Biphasic Organic Synthesis 141

6.3.1 Ozonolysis Reactions 141

6.3.2 Photooxygenation Reactions 151

6.4 Practical Exercise: Photochemical Generation of Singlet Oxygen and Its [4 + 2] Cycloaddition to Cyclopentadiene 159

References 161

7 Synthesis of Nanomaterials Using Continuous-Flow Microreactors / Chih-Hung Chang Chang, Chih-Hung 165

7.1 Introduction 165

7.2 Midofluidic Devices 165

7.3 Synthesis of Nanomaterials Using Microreactors 166

7.4 Kinetic Studies 180

7.5 Process Optimization 183

7.6 Point-of-Use Synthesis and Deposition 185

7.6.1 Deposition of Nanomaterials 185

7.7 Practical Exercises: Synthesis of Nanocrystals 187

7.7.1 Synthesis of ZnO Nanocrystals 187

7.7.2 Synthesis of CdS Nanoparticles 190

References 192

8 Polymerization in Microfluidic Reactors / Jesse Greener Greener, Jesse, Eugenia Kumacheva Kumacheva, Eugenia 197

8.1 Introduction 197

8.2 Practical Considerations 198

8.2.1 Control Over Reaction Conditions 198

8.2.1.1 Batch Reactors 198

8.2.1.2 Microreactors 199

8.2.2 Control of Mixing 199

8.2.3 Control of Reagent Concentrations 200

8.2.4 Distance-to-Time Transformation 200

8.2.5 Potential Negative Impacts of Polymerization Reactions on Reactor Operation 201

8.2.5.1 Buildup in Solution Viscosity 201

8.2.5.2 Precipitation 202

8.2.5.3 Adsorption 202

8.2.6 Selection of Materials for Fabrication of MF Reactors 203

8.2.6.1 Polymer Materials 203

8.2.6.2 Metals 205

8.2.6.3 Glass 205

8.3 Single-Phase Polymerization 205

8.4 Multiphase Polymerization 208

8.4.1 Formation of Polymer Particles 209

8.4.1.1 Formation of Precursor Droplets 209

8.4.1.2 Transformation of Precursor Droplets into Polymer Particles 213

8.4.2 Review of Demonstrated Applications 214

8.4.2.1 Controlled Encapsulation 214

8.4.2.2 Encapsulation and Delivery 215

8.4.2.3 Cell Encapsulation 217

8.4.2.4 Microgels as Model Cells 219

8.5 Beyond Synthesis: New Developments for Next-Generation MF Polymerization 220

8.5.1 Scaled-Up MF Synthesis of Polymer Particles 220

8.5.2 In Situ Characterization of Polymerization in MF Reactors 223

8.5.3 Automated Systems for Polymerization Microreactors 223

8.6 Practical Exercise: MF Polymerization Reactor Kinetics Studies Using In Situ Characterization 224

References 227

9 Electrochemical Reactions in Microreactors / Jun-ichi Yoshida Yoshida, Jun-ichi, Aiichiro Nagaki Nagaki, Aiichiro 231

9.1 Introduction 231

9.2 Electrode Configuration 232

9.2.1 Serial Electrode Configuration 232

9.2.2 Interdigitated Electrode Configuration 233

9.2.3 Parallel Electrode Configuration 233

9.3 Electrolysis without Supporting Electrolytes 234

9.4 Generation and Reactions with Unstable Intermediates 235

9.5 Practical Exercise: Electrochemical Reactions in Flow Microreactors 239

References 241

10 Heterogeneous Catalysis in Microreactors / Evgeny V.

Rebrov Rebrov, Evgeny V. 243

10.1 Introduction 243

10.2 Bulk Catalysts 244

10.3 Supported Catalysts 246

10.3.1 Macroporous Supports 247

10.3.1.1 ZnO Support 247

10.3.1.2 γ-Al₂O₃ Support 247

10.3.1.3 Catalysts Immobilized onto Polymeric Particles 249

10.3.1.4 Silica-Supported Catalysts 251

10.3.1.5 Carbon-Supported Catalysts 253

10.4 Mesoporous Supports 256

10.4.1 Mesoporous Titania 258

10.4.2 Mesoporous Silica 260

10.4.3 Mesoporous Alumina 261

10.5 Microporous Supports 261

10.6 Practical Exercise: PdZn/TiO₂-Catalyzed Selective Hydrogenation of Acetylene Alcohols in a Capillary Microreactor 263

References 265

11 Chemical Intensification in Flow Chemistry through Harsh Reaction Conditions and New Reaction Design / Timothy Noël Noël, Timothy, Volker Hessel Hessel, Volker 273

11.1 Introduction 273

11.2 High-Temperature Processing in Microflow 273

11.3 High-Pressure Processing in Microflow 278

11.4 Solvent Effects in Microflow 280

11.5 Ex-Regime Processing and Handling of Hazardous Compounds in Microflow 283

11.6 New Chemical Transformations in Microflow 284

11.7 Process Integration in Microflow 286

11.8 Practical Exercises 288

11.8.1 Claisen Rearrangement at Elevated Temperatures 288

11.5.2 Copper(I)-Catalyzed Azide-Alkyne Cycloaddition with Integrated Copper Scavenging Unit 290

References 292

12 Modeling in Microreactors / Ekaterina S. Borovinskaya Borovinskaya, Ekaterina S. 297

12.1 Introduction 297

12.2 Processes in Microreactors and the Role of Mixing 298

12.3 Modeling of Processes in Microreactors Based on General Balance Equation 300

12.3.1 Plug Flow Tube Reactor Model 300

12.3.2 Laminar Flow Model 302

12.4 Computation of Reaction Flows in Microreactors 308

12.4.1 Computational Fluid Dynamics 308

12.4.2 Single-Phase Modeling 309

12.4.3 Two-Phase Modeling 310

12.4.3.1 Liquid-Liquid Flow with Chemical Reaction 310

12.4.3.2 Liquid-Gas Flow with Chemical Reaction 312

12.4.4 Three-Phase Modeling 315

12.5 Practical Exercise: Alkylation of Phenylacetonitrile 320

References 323.

Notes:

Includes bibliographical references and index.

ISBN:

9783527332823

3527332820

OCLC:

857992196