Industrial Crystallization Process Monitoring

This ready reference and handbook draws on the experience and expertise 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. The first part of the book presents the instrumentation and techniques used to measure the crystal size distribution, the nucleation point and solubility point, and the chemical composition of the solid and liquid phase. The second part describes the main techniques adopted to control industrial crystallizers, starting from fundamental approaches to the most advanced ones, including the multivariable predictive control. 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. The contents are tailor-made for readers facing the threshold challenges between research and commercial applications.

Angelo Chianese is full Professor of Chemical Plant Design at the University of Rome La Sapienza. He worked as a process engineer for the first 10 years of his working life, before joining academia. Prof. Chianese has more than 30 years in the field of industrial crystallization. In this respect, he collaborated with the major academic laboratories all over the world and major industrial companies. Between 1998 and 2001 he was the coordinator of the European Thematic Network on Industrial Crystallization (acronym. CRYSOPT) and since 1990 was partner in many European projects. He is one of the two Italian delegates at the European Working Party on Crystallization. Herman J. M. Kramer is associate professor at the Delft University of Technology, The Netherlands, working on the design, monitoring and control of crystallization and precipitation processes. He headed a large number of international multi client, multidisciplinary, research projects on design, monitoring and control of industrial crystallization. He was president of the Dutch Association of Crystal growth and is nowadays member of the European Working Party of Industrial Crystallization.

Preface	p. XI
Scope of the Book	p. XIII
List of Contributors	p. XXI
Characterization of Crystal Size Distribution	p. 1
Introduction	p. 1
Particle Size Distribution	p. 1
Particle Size Distribution Moments	p. 4
Particle Size Distribution Characterization on the Basis of Mass Distribution	p. 5
References	p. 6
Forward Light Scattering	p. 7
Introduction	p. 7
Principles of Laser Diffraction	p. 8
Scatter Theory	p. 10
Generalized Lorenz-Mie Theory	p. 12
Anomalous Diffraction	p. 12
Fraunhofer Diffraction	p. 13
Deconvolution	p. 13
Direct Inversion Using the Nonnegativity Constraint	p. 14
Philips Twomey Inversion Method	p. 14
Iterative Methods	p. 15
The Effects of Shape	p. 15
Multiple Scattering	p. 16
Application of Laser Diffraction for Monitoring and Control of Industrial Crystallization Processes	p. 17
Conclusions	p. 19
References	p. 20
Further Reading	p. 20
Focused Beam Reflectance Measurement	p. 21
Measurement Principle	p. 21
Application Examples	p. 21
Solubility and Metastable Zone Width (MSZW)	p. 21
Seed Effectiveness	p. 22
Polymorph Transformations	p. 22
Effect of Different Impurity Levels	p. 23
Nucleation Kinetics	p. 24
Improved Downstream Processing	p. 24
Process Control	p. 25
Advantages and Limitations	p. 26
References	p. 27
Turbidimetry for the Estimation of Crystal Average Size	p. 29
Introduction	p. 29
Determination of Average Particle Size from Specific Turbidity	p. 29
Procedure to Evaluate Average Crystal Size by Turbidimetry for a High Solid Slurry Concentration	p. 31
Conclusion	p. 34
References	p. 34
Further Reading	p. 34
Imaging	p. 35
Introduction	p. 35
Literature Overview	p. 36
The Sensor Design	p. 39
Optics and Illumination	p. 40
The Camera System and the Resolution	p. 42
Image Analysis	p. 43
Statistics	p. 46
Application of In Situ Imaging for Monitoring Crystallization Processes	p. 46
Example 1	p. 46
Example 2	p. 47
Conclusions	p. 48
	p. 49
	p. 50
Turbidimetry and Nephelometry	p. 51
Introduction	p. 51
Measurement of Nucleation and Solubility Points	p. 51
The Developed Turbidrmetric and Nephelometric Instruments	p. 52
The Examined Systems	p. 53
Obtained Results	p. 54
References	p. 57
Speed of Sound	p. 59
Introduction	p. 59
In-Process Ultrasound Measurement	p. 59
Determining Solubility and Metastable Zone Width	p. 60
Measuring Crystal Growth Rates	p. 65
Detecting Phase Transitions with Ultrasound	p. 66
References	p. 68
In-Line Process Refractometer for Concentration Measurement in Sugar Crystallizers	p. 71
Introduction	p. 71
Measurement Principle	p. 72
In-Line Instrument Features and Benefits	p. 74
Accuracy	p. 74
Concentration Determination	p. 74
Process Temperature Compensation Factor	p. 75
Process Sensor	p. 75
Features and Benefits	p. 76
Example of Application in the Crystallization	p. 76
Seeding Point and Supersaturation Control in Sugar Vacuum Pan	p. 77
Conclusion	p. 79
Atr-Ftir Spectroscopy	p. 81
Introduction	p. 81
Calibration	p. 82
Speciation Monitoring	p. 84
Co-Crystal Formation	p. 84
Solubility Measurement	p. 86
Crystal Growth Rates	p. 86
Polymorph Transformation	p. 87
Crystallization Monitoring and Control	p. 89
Impurity Monitoring	p. 89
Conclusions	p. 90
References	p. 90
Raman Spectroscopy	p. 93
Introduction	p. 93
Factors Influencing the Raman Spectrum	p. 94
Calibration	p. 95
Univariate Approaches	p. 95
Multivariate Approaches	p. 98
Applications	p. 99
Solid-Phase Composition Monitoring	p. 99
Liquid Phase Composition Monitoring	p. 99
Amorphous Content Quantification	p. 200
Conclusions	p. 101
References	p. 102
Basic Recipe Control	p. 105
Introduction	p. 105
Incentives for Basic Recipe Control	p. 105
Main Mechanisms, Sensors, and Actuators	p. 106
Crystallization Mechanisms	p. 106
Sensors	p. 106
Measurement of the Solute Concentration	p. 107
Measurement of the Crystal Number, Size, Distribution, and Morphology	p. 107
Actuators	p. 108
Basic Recipe Control Strategy	p. 109
How to Obtain a Recipe?	p. 110
Scaling Up the Recipe	p. 111
Seeding as a Process Actuator	p. 111
Initial Supersaruration	p. 112
Seed Mass	p. 112
Seed Size and Size Distribution	p. 113
Seed Quality and Preparation Procedure	p. 113
Methods of Addition of Seeds	p. 114
Rate of Supersaturation Generation	p. 114
Mixing and Suspension of Solids	p. 116
Fines Removal and Dissolution	p. 118
Implementation of Basic Recipe Control	p. 119
Conclusions	p. 122
References	p. 122
Seeding Technique in Batch Crystallization	p. 127
Introduction	p. 127
Seeding Operation: Main Principles and Phenomena	p. 127
Use of Seeding for Batch Crystallization: Main Process Parameters	p. 128
Control of Batch Crystallization by Seeding: Empirical Rules for Design	p. 131
References	p. 137
Advanced Recipe Control	p. 139
Introduction	p. 139
Incentives and Strategy of the Advanced Recipe Control	p. 139
Modeling for Optimization, Prediction, and Control	p. 141
Model Validation	p. 143
Rate of Supersaturation Generation	p. 144
Mixing Conditions	p. 145
Implementation	p. 150
Example of Modeling, Optimization, and Open-Loop Control of a 75-1 Draft-Tube Crystallizer	p. 150
Objectives and Advanced Recipe Control	p. 150
Process Description and Modeling	p. 151
Dynamic Optimization	p. 153
Experimental Validation Results	p. 155
Conclusions	p. 157
References	p. 158
Advanced Model-Based Recipe Control	p. 161
Introduction	p. 161
Online Dynamic Optimization	p. 163
MPC for Batch Crystallization	p. 168
Conclusions and Perspectives	p. 172
References	p. 173
Fines Removal	p. 175
Introduction	p. 175
Fines Removal by Heat Dissolution	p. 175
Modeling of an MSMPR Continuous Crystallizer with Fines Removal	p. 177
Fines Destruction in the Industrial Practice	p. 178
CSD Control by Fines Removal for Pilot Scale Crystallizers	p. 180
The Cycling Phenomenon as Undesired Effect of Fines Destruction in Industrial Crystallizers	p. 182
References	p. 184
Model Predictive Control	p. 185
Introduction	p. 185
Receding Horizon Principle	p. 185
Advantages and Disadvantages of MPC	p. 187
Approach for Designing and Implementing an MPC Control System	p. 189
Process Modeling	p. 190
The Performance Index	p. 192
Constraints	p. 193
The MPC Optimization	p. 193
Tuning	p. 193
State Estimation	p. 194
Implementation	p. 196
MPC of Crystallization Processes	p. 197
Delta-Mode MPC	p. 198
Conclusions and Perspectives	p. 199
References	p. 200
Industrial Crystallizers Design and Control	p. 203
Introduction	p. 203
Forced Circulation Crystallizer	p. 204
Draft-Tube-Baffle Crystallizer	p. 209
"Oslo" Growth-Type Crystallizer	p. 213
Process Variables in Crystallizer Operation	p. 218
Continuous Operation	p. 218
Batch Operations	p. 219
Sensors	p. 219
Level	p. 220
Density	p. 220
Crystal Size	p. 221
Control Devices	p. 222
References	p. 224
Index	p. 225
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Industrial Crystallization Process Monitoring and Control

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