Industrial Crystallization Process Monitoring and Control E-Book

• Herausgeber: Wiley-VCH
• Kategorie: Fachliteratur
• Sprache: Englisch

Seitenzahl: 363

Veröffentlichungsjahr: 2012

Beschreibung

Crystallization is an important technique for separation and purification of substances as well as for product design in chemical, pharmaceutical and biotechnological process industries. This ready reference and handbook draws on research work and industrial practice of a large group of experts in the various areas of industrial crystallization processes, capturing the essence of current trends, the markets, design tools and technologies in this key field. Along the way, it outlines trouble free production, provides laboratory controls, analyses case studies and discusses new challenges. First the instrumentation and techniques used to measure the crystal size distribution, the nucleation and solubility points, and the chemical composition of the solid and liquid phase are outlined. Then the main techniques adopted to control industrial crystallizers, starting from fundamental approaches to the most advanced ones, including the multivariable predictive control are described. An overview of the main crystallizer types is given with details of the main control schemes adopted in industry as well as the more suitable sensors and actuators.

Leseprobe

Table of Contents

Related Titles

Title Page

Copyright

Preface

Scope of the Book

Control of Crystallization Processes in Industrial Practice

Content of the Book

References

List of Contributors

Chapter 1: Characterization of Crystal Size Distribution

1.1 Introduction

1.2 Particle Size Distribution

1.3 Particle Size Distribution Moments

1.4 Particle Size Distribution Characterization on the Basis of Mass Distribution

References

Chapter 2: Forward Light Scattering

2.1 Introduction

2.2 Principles of Laser Diffraction

2.3 Scatter Theory

2.4 Deconvolution

2.5 The Effects of Shape

2.6 Multiple Scattering

2.7 Application of Laser Diffraction for Monitoring and Control of Industrial Crystallization Processes

2.8 Conclusions

References

Further Reading

Chapter 3: Focused Beam Reflectance Measurement

3.1 Measurement Principle

3.2 Application Examples

3.3 Advantages and Limitations

References

Chapter 4: Turbidimetry for the Estimation of Crystal Average Size

4.1 Introduction

4.2 Determination of Average Particle Size from Specific Turbidity

4.3 Procedure to Evaluate Average Crystal Size by Turbidimetry for a HighSolid Slurry Concentration

4.4 Conclusion

References

Further Reading

Chapter 5: Imaging

5.1 Introduction

5.2 Literature Overview

5.3 The Sensor Design

5.4 Application of In Situ Imaging for Monitoring Crystallization Processes

5.5 Conclusions

References

Further Reading

Chapter 6: Turbidimetry and Nephelometry

6.1 Introduction

6.2 Measurement of Nucleation and Solubility Points

6.3 The Developed Turbidimetric and Nephelometric Instruments

6.4 The Examined Systems

6.5 Obtained Results

References

Chapter 7: Speed of Sound

7.1 Introduction

7.2 In-Process Ultrasound Measurement

7.3 Determining Solubility and Metastable Zone Width

7.4 Measuring Crystal Growth Rates

7.5 Detecting Phase Transitions with Ultrasound

References

Chapter 8: In-Line Process Refractometer for Concentration Measurement in Sugar Crystallizers

8.1 Introduction

8.2 Measurement Principle

8.3 In-Line Instrument Features and Benefits

8.4 Features and Benefits

8.5 Example of Application in the Crystallization

8.6 Conclusion

References

Chapter 9: ATR-FTIR Spectroscopy

9.1 Introduction

9.2 Calibration

9.3 Speciation Monitoring

9.4 Co-Crystal Formation

9.5 Solubility Measurement

9.6 Crystal Growth Rates

9.7 Polymorph Transformation

9.8 Crystallization Monitoring and Control

9.9 Impurity Monitoring

9.10 Conclusions

References

Chapter 10: Raman Spectroscopy

10.1 Introduction

10.2 Factors Influencing the Raman Spectrum

10.3 Calibration

10.4 Applications

10.5 Conclusions

References

Chapter 11: Basic Recipe Control

11.1 Introduction

11.2 Incentives for Basic Recipe Control

11.3 Main Mechanisms, Sensors, and Actuators

11.4 Basic Recipe Control Strategy

11.5 Seeding as a Process Actuator

11.6 Rate of Supersaturation Generation

11.7 Mixing and Suspension of Solids

11.8 Fines Removal and Dissolution

11.9 Implementation of Basic Recipe Control

11.10 Conclusions

References

Chapter 12: Seeding Technique in Batch Crystallization

12.1 Introduction

12.2 Seeding Operation: Main Principles and Phenomena

12.3 Use of Seeding for Batch Crystallization: Main Process Parameters

12.4 Control of Batch Crystallization by Seeding: Empirical Rules for Design

References

Chapter 13: Advanced Recipe Control

13.1 Introduction

13.2 Incentives and Strategy of the Advanced Recipe Control

13.3 Modeling for Optimization, Prediction, and Control

13.4 Model Validation

13.5 Rate of Supersaturation Generation

13.6 Mixing Conditions

13.7 Implementation

13.8 Example of Modeling, Optimization, and Open-Loop Control of a 75-l Draft-Tube Crystallizer

13.9 Conclusions

References

Chapter 14: Advanced Model-Based Recipe Control

14.1 Introduction

14.2 Online Dynamic Optimization

14.3 MPC for Batch Crystallization

14.4 Conclusions and Perspectives

References

Chapter 15: Fines Removal

15.1 Introduction

15.2 Fines Removal by Heat Dissolution

15.3 Modeling of an MSMPR Continuous Crystallizer with Fines Removal

15.4 Fines Destruction in the Industrial Practice

15.5 CSD Control by Fines Removal for Pilot Scale Crystallizers

15.6 The Cycling Phenomenon as Undesired Effect of Fines Destruction in Industrial Crystallizers

References

Chapter 16: Model Predictive Control

16.1 Introduction

16.2 Approach for Designing and Implementing an MPC Control System

16.3 Process Modeling

16.4 The Performance Index

16.5 Constraints

16.6 The MPC Optimization

16.7 Tuning

16.8 State Estimation

16.9 Implementation

16.10 MPC of Crystallization Processes

16.11 Delta-Mode MPC

16.12 Conclusions and Perspectives

References

Chapter 17: Industrial Crystallizers Design and Control

17.1 Introduction

17.2 Forced Circulation Crystallizer

17.3 Draft-Tube-Baffle Crystallizer

17.4 Process Variables in Crystallizer Operation

17.5 Sensors

17.6 Control Devices

References

Index

Related Titles

Houson, I. (ed.)

Process Understanding

For Scale-Up and Manufacture of Active

Ingredients

2011

ISBN: 978-3-527-32584-9

Pollak, P.

Fine Chemicals

The Industry and the Business

Second edition

2011

ISBN: 978-0-470-62767-9

Duffar, T. (ed.)

Crystal Growth Processes

Based on Capillarity

Czochralski, Floating Zone, Shaping and

Crucible Techniques

2010

ISBN: 978-0-470-71244-3

Tiekink, E. R. T., Vittal, J., Zaworotko,M.

(eds.)

Organic Crystal Engineering

Frontiers in Crystal Engineering

2010

ISBN: 978-0-470-31990-1

Capper, P., Rudolph, P. (eds.)

Crystal Growth Technology

Semiconductors and Dielectrics

2010

ISBN: 978-3-527-32593-1

Tung, H.-H., Paul, E. L., Midler, M.,

McCauley, J. A.

Crystallization of Organic

Compounds

An Industrial Perspective

2009

ISBN: 978-0-471-46780-9

Hessel, V., Renken, A., Schouten, J. C.,

Yoshida, J.-i. (eds.)

Micro Process Engineering

A Comprehensive Handbook

3 Volume Set

2009

ISBN: 978-3-527-31550-5

Scheel, H. J., Capper, P. (eds.)

The Editors

Prof. Dr. Ing. Angelo Chianese

Sapienza University of Rome

Department of Chemical Engineering

Materials Environment

via Eudossiana 18

00184 Rome

Italy

Prof. Dr. Herman J. M. Kramer

Delft University of Technology

Process & Energy Laboratory

Leeghwaterstraat 44

2628 CA Delft

The Netherlands

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© 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Boschstr. 12, 69469 Weinheim, Germany

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ISBN: 978-3-527-33173-4

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Preface

The idea of this book was to disseminate some valuable results achieved by two European projects on monitoring and control of industrial crystallizers:

1. CRYSEN (2000–2003) on the Development of new sensors for industrial crystallization;

2. SINC-PRO (2003–2005) on Self-learning model for INtelligent predictive Control system for crystallization PROcesses. This second European project then became an international project with the partnership extended to Swiss and Japanese teams.

Most of the partners of the two projects were members of the Working Party on Crystallization (WPC) of the European Federation of Chemical Engineers, which accepts the proposal of the book and encouraged the efforts of the two editors in order to provide a new publication to the industrial crystallizer community. Then, the WPC provided a double reviewing of each books chapter by the WPC members, from academia and industry, expert in the specific subject.

Therefore, the two editors are greatly grateful to the two Chairmen of the WPC, who promoted the book writing, Joachim Ulrich and Beatrice Biscans and to the following WPC members, who with their referee's work contributed to improve the quality of the book:

Beatrice Biscans

Colm Campbell

Philippe Carvin

Roger Daudey

Brian Glennon

Laurent Laferrere

Jaime Morales

Zoltan Nagy

Matthias Raouls

Ake Rasmuson

December 2011

Angelo Chianese and Herman J. M. Kramer

Scope of the Book

Control of Crystallization Processes in Industrial Practice

Crystallization from a solution is a separation technique, where one of more components of the solution are separated as a solid phase. Application of a crystallization process can be aimed at the separation of a component from a multicomponent mixture, but in most cases it is focused on the production of a solid product from a liquid mixture. In both types of application, the product quality of the solid product has to meet stringent specifications, and especially for solid products manufacturers have to meet ever-increasing demands of the customers on particle properties such as particle size distribution, crystal shape, degree of agglomeration, caking behavior, and purity. Since for an economic beneficial operation a smooth separation of the produced crystals from the mother liquor is essential, additional demands on filterability and washability need to be obeyed. It is obvious that in order to achieve the increasing demands on product quality, crystallization processes have to be carefully controlled.

Crystallization from a liquid solution is the most important production and separation process in the fine chemical and food industry and one of the most important processes in the chemical process industry as a whole. Overall it is estimated that 70% of the products sold by the chemical process industry are solids. Many intermediates (e.g., adipic acid for nylon production), fine chemicals, pharmaceuticals (e.g., aspirin), biochemical, food additives, and bulk products such as fertilizers are solids obtained through crystallization.