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Crystallization. Basic Concepts and Industrial Applications - Product Image

Crystallization. Basic Concepts and Industrial Applications

  • Published: February 2013
  • 360 Pages
  • John Wiley and Sons Ltd

Crystallization is a natural occurring process but also a process abundantly used in the industry. Crystallization can occur from a solution, from the melt or via deposition of material from the gas phase (desublimation). Crystals distinguish themself from liquids, gases and amorphous substances by the long-range order of its building blocks that entail the crystals to be formed of well-defined faces, and give rise to a large number of properties of the solid.

Crystallization is used at some stage in nearly all process industries as a method of production, purification or recovery of solid materials. Crystallization is practiced on all scales: from the isolation of the first milligrams of a newly synthesized substance in the research laboratory to isolating products on the mulit-million tonne scale in industry. The book describes the breadth of crystallization operations, from isolation from a reaction broth to purification and finally to tailoring product properties.

In the first section of the book, the basic mechanisms - nucleation, growth, attrition and agglomeration are introduced. It ensures an understanding of supersaturation, the driving force of crystallization. READ MORE >

List of Contributors XIII

1 Crystallization: Introduction 1
Wolfgang Beckmann

2 Mechanisms of Crystallization 7
Wolfgang Beckmann

2.1 Crystal Lattice 7

2.2 Nucleation of Crystals 17

2.3 Growth and Growth Rate of Crystals 25

Further Reading 33

3 Solubility and Solution Equilibria in Crystallization 35
Heike Lorenz

3.1 Phase Equilibria and Phase Diagrams: General Issues 36

3.2 Melt Phase Diagrams 44

3.3 Solution Equilibria 53

References 74

4 Agglomeration during Crystallization 75
Wolfgang Beckmann

4.1 Mechanisms and Kinetics of Agglomeration 75

4.2 Parameters Influencing Agglomeration 77

4.3 Agglomeration during Crystallization 80

4.4 Mechanical Properties of Agglomerates 83

References 84

5 Polymorphism of Crystalline Systems 85
Rolf Hilfiker

5.1 Introduction and Definitions 85

5.2 Occurrence and Properties of Polymorphs and Solvates 86

5.3 Thermodynamics of Polymorphs of Solid-State Forms 87

5.4 Thermodynamics of Hydrates 91

5.5 Experimental Techniques to Elucidate Thermodynamics 94

5.6 Formation of Various Polymorphs and Solid-State Forms-Polymorph Screens 97

5.7 Selection of Optimal Form for Development 101

Symbols 102

References 102

6 The Influence of Additives and Impurities on Crystallization 105
Christiane Schmidt, Matthew J. Jones, and Joachim Ulrich

6.1 Influence of Additives and Impurities on Crystallization 105

6.2 Influence of Impurities: Modeling 116

6.3 Tailor-Made Additives 122

6.4 Modeling the Influence of Solvents 122

References 124

7 Purification by Crystallization 129
Heike Lorenz and Wolfgang Beckmann

7.1 Introduction 129

7.2 Mechanisms of Impurity Incorporation and Purification 131

References 147

8 Characterization of Crystalline Products 149
Rolf Hilfiker

8.1 Introduction 149

8.2 Characterization of Intrinsic Properties of a Solid 149

8.3 Characterization of Particle Shape and Size 161

8.4 Powder Flow Properties 165

8.5 In-Process Characterization 167

References 171

9 Basics of Industrial Crystallization from Solution 173
Wolfgang Beckmann

9.1 Generation of Supersaturation in a Crystallizer 173

9.2 Mass and Population Balance for Growth from Suspension 176

9.3 Operation of a Continuous Crystallizer: Basics 178

9.4 Operation of a Batch Crystallizer: Basics 183

10 Development of Batch Crystallizations 187
Dierk Wieckhusen

10.1 Setting Goals 187

10.2 Crystallization of Organic Moieties 188

10.3 Generation of Supersaturation in Batch Crystallizations 189

10.4 Initiation of Crystallization – Nucleation Phase 192

10.5 Seeded Batch Crystallizations 193

10.6 Crystallization Period 197

10.7 Scale-Up Considerations 198

10.8 Manipulating Particle Shape 201

11 Continuous Crystallization 203
Günter Hofmann and Christian Melches

11.1 Concept and Design of Continuous Crystallizers 204

11.2 Various Continuous Crystallizers 218

11.3 Periphery 226

11.4 Special Features of the Process 229

11.5 Adjustment of Suspension Densities 232

References 233

12 Precipitation 235
Wolfgang Beckmann

12.1 Precipitation from Solution by Mixing Two Streams 235

12.2 Semi-Batch Precipitations 236

12.3 Model of Mixing during Precipitation 238

12.4 Precipitations Using Supercritical Fluids 239

12.5 Crystal Issues 241

12.6 Particle Size as a Function of Operating Conditions 244

13 Mixing in Crystallization Processes 247
Bernd Nienhaus

13.1 Mixing in Batch and Continuous Crystallization Processes 247

13.2 Basic Mixing Tasks – Mixing Tasks in Crystallization 248

13.3 Impellers and Agitation Systems 249

13.4 Power Consumption of an Impeller System [2] 253

13.5 Blending 256

13.6 Suspending 259

13.7 Scale-Up of a Crystallization Process 268

References 273

14 Downstream Processes 275
Dierk Wieckhusen and Wolfgang Beckmann

14.1 Transfer of Suspension and Filter Cake 275

14.2 Solid–Liquid Separation 275

14.3 Drying 280

References 288

15 Melt Crystallization 289
Joachim Ulrich and Torsten Stelzer

15.1 Characteristics of Melt Crystallization 289

15.2 Processes of Melt Crystallization 292

15.3 Postcrystallization Treatments 295

15.4 Laboratory Techniques 301

References 304

16 Examples of Realized Continuous Crystallization Processes 305
Günter Hofmann and Christian Melches

16.1 Choosing the Drain Point in Process Design 305

16.2 Example Crop Crystallization for Organic Compounds 310

16.3 Example Crystallization of Table Salt 316

16.4 Results 323

17 Design Examples of Melt Crystallization 325
Joachim Ulrich and Torsten Stelzer

17.1 Concepts of Melt Crystallization 325

17.2 Outlook 334

References 335

Index 337

Wolfgang Beckmann is Senior Expert at Bayer Technologies. Dr. Beckmann studied Chemical Engineering and Physical Chemistry in Germany and the US. He spent one year as Postdoctoral Fellow in Marseille. Wolfgang Beckmann has spent the last 20 years working at Bayer and prior to this at Schering, developing crystallization processes for pharmaceutical compounds. He has authored several chapters in books and approximately 50 publications in reviewed journals.

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