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CR 6: Crystallizer Troubleshooting

CR 6: Crystallizer Troubleshooting
     Part 1: Troubleshooting crystal size distributions
         1. INTRODUCTION
             1.1 Objectives and scope of this report
             1.2 Overview of how to use this report
             1.3 Crystal Size Distribution Fundamentals
             1.4 Description of crystal size distribution
                 1.4.1 Number-based distribution
                 1.4.2 Mass-based distribution
             1.5 Parameters characterising the size distribution
             1.6 Theoretical size distributions
             1.7 Measurement of crystal size distributions
         2. FACTORS AFFECTING THE CRYSTAL SIZE DISTRIBUTION
             2.1 Supersaturation
             2.2 Temperature
                 2.2.1 Temperature dependence of solubility
                 2.2.2 Temperature dependence of nucleation and growth rates
             2.3 Evaporation rate
             2.4 Temperature/evaporation profiles for batch crystallizers
                 2.4.1 Programmed cooling
                 2.4.2 Programmed evaporation
             2.5 Concentration
                 2.5.1 Solute concentration
                 2.5.2 Reactant & salting-out reagent concentration
                 2.5.3 Impurity concentration
             2.6 Residence time/batch time
                 2.6.1 Slurry density
                 2.6.2 Residence time (continuous crystallization)
                 2.6.3 Batch time (batch crystallization)
                 2.6.4 Mixing and residence time distributions
             2.7 Seeding
                 2.7.1 Seeding for growth to product
                 2.7.2 Seeding for avoiding primary nucleation
                 2.7.3 Seed preparation
                 2.7.4 Inadvertent seeding
             2.8 Agitation
                 2.8.1 Mass transfer
                 2.8.2 Suspension requirements
                 2.8.3 Nucleation rates
                 2.8.4 Effect on aggregates/agglomerates
             2.9 Vessel geometry
                 2.9.1 Inlet location (continuous crystallizers)
                 2.9.2 Dead zones in circulation
                 2.9.3 Imperfect mixing
                 2.9.4 Agitator design and internal structures
             2.10 Non-MSMPR behaviour
                 2.10.1 Classified product removal (CPR)
                 2.10.2 Fines destruction/removal (FD/FR)
                 2.10.3 Clear Liquor Advance (CLA)
                 2.10.4 Simultaneous classified product removal and fines destruction
             2.11 Stability
             2.12 External equipment
                 2.12.1 External circulation equipment
                 2.12.2 Downstream equipment
             2.13 Miscellaneous
                 2.13.1 Polycrystallinity
                 2.13.2 Solvent
                 2.13.3 Ostwald Ripening
                 2.13.4 Electromagnetic effects
         3. DEFINE PROBLEM WITH CSD
             3.1 Determination of problem type (Figure 3.1)
             3.2 Crystal Size Distribution Analysis (Figure 3.2)
         4. LOW COST/SHORT TERM OPTIONS
             4.1 Solutions to FINES problem (Table 4.1)
             4.2 Solutions to LARGE crystal problem (Table 4.2)
             4.3 Solutions to WIDE distribution problem (Table 4.3)
             4.4 Solutions to ERRATIC distribution problem (Table 4.4)
             4.5 Solutions to low AVERAGE crystal size problem (Table 4.5)
             4.6 Solutions to high AVERAGE crystal size problem (Table 4.6)
         5. MEDIUM COST/MEDIUM TERM OPTIONS
             5.1 Solutions to FINES problem (Table 5.1)
             5.2 Solutions to LARGE crystal problem (Table 5.2)
             5.3 Solutions to WIDE distribution problem (Table 5.3)
             5.4 Solutions to ERRATIC distribution problem (Table 5.4)
             5.5 Solutions to low AVERAGE crystal size problem (Table 5.5)
             5.6 Solutions to high AVERAGE crystal size problem (Table 5.6)
         6. HIGH COST/LONG TERM OPTIONS
             6.1 Solutions to FINES problem (Table 6.1)
             6.2 Solutions to LARGE crystal problem (Table 6.2)
             6.3 Solutions to WIDE distribution problem (Table 6.3)
             6.4 Solutions to ERRATIC distribution problem (Table 6.4)
             6.5 Solutions to low AVERAGE crystal size problem (Table 6.5)
             6.6 Solutions to high AVERAGE crystal size problem (Table 6.6)
         7. DESIGN OF NEW CRYSTALLIZERS
             7.1 Supersaturation level (Section 2.1)
             7.2 Temperature (Section 2.2)
             7.3 Evaporation rate (Section 2.3)
             7.4 Temperature/evaporation profiling (Section 2.4)
             7.5 Concentration (Section 2.5)
             7.6 Residence time/batch time (Section 2.6)
             7.7 Seeding (Section 2.7)
             7.8 Agitation (Section 2.8)
             7.9 Vessel geometry (Section 2.9)
             7.10 Non-MSMPR behaviour (Section 2.10)
             7.11 Stability (Section 2.11)
             7.12 External equipment (Section 2.12)
             7.13 Miscellaneous (Section 2.13)
         8. NOMENCLATURE
             8.1 Symbols
             8.2 Subscripts
         9. REFERENCES
     Part 2: Encrustation of crystallizers
         1. INTRODUCTION
         2. MECHANISMS OF FOULING
             2.1 Introduction
             2.2 Particulate deposition
             2.3 Scaling
             2.4 Freezing
             2.5 Chemical reaction (corrosion)
             2.6 Polymerization
             2.7 Biological fouling
         3. PREVENTION OF FOULING IN DESIGN STAGE
             3.1 Introduction
             3.2 local supersaturation
             3.3 Surface treatment
             3.4 Other techniques
         4. PREVENTION OF FOULING IN OPERATION
         5. CONCLUSIONS
         6. NOMENCLATURE
         7. REFERENCES
     Part 3: Attrition and Breakage
         1.INTRODUCTION.
             1.1 Scope.
             1.2 How to use the report.
             1.3 Links with other reports.
         2. STRATEGIES FOR CONTROL OF ATTRITION AND BREAKAGE.
             2.1 Design of new processes.
             2.2 Troubleshooting existing processes.
         3. IMPACT ATTRITION OF GRANULAR SOLIDS.
             3.1 Introduction.
             3.2 Nature of comminution.
             3.3 Energy for size reduction.
                 3.3.1 Empirical models.
                 3.3.2 Rittinger's Law (Rittinger, 1867)
                 3.3.3 Kick's Law (Kick, 1885) (n = -1).
                 3.3.4 Bond's Law (Bond, 1952)(n = -3/2) .
             3.4 The nature and sources of attrition.
             3.5 Effects of attrition.
             3.6. Attrition dynamics.
             3.7 Influence of the environment.
             3.8 Single particle breakage.
             3.9 Modelling methods.
             3.10 Effect of temperature.
             3.11 Effect of pressure.
             3.12 Attrition assessment.
             3.13 Attrition rate and attrition index.
                 3.13.1 Hardgrove index.
                 3.13.2 Work index / Bond index.
                 3.13.3 Crushing strength index.
                 3.13.4 Attrition test methods.
             3.14 Experiments with crystals.
             3.15 Effect of crystallization process conditions.
             3.16 Specific industrial examples.
                 3.16.1 Chemical industry.
                 3.16.2 Gas-liquid chromatography.
                 3.16.3 Automotive catalytic afterburners.
                 3.16.4 Cement industry.
                 3.16.5 Milling.
                 3.16.6 Food industry.
                 3.16.7 Pharmaceutical industry.
                 3.16.8 Mining and quarrying.
                 3.16.9 Railways.
             3.17. Examples in specific unit operations.
                 3.17.1 Fluidised beds.
                 3.17.2 Cyclones.
                 3.17.3 Sand blasting.
                 3.17.4 Stirred vessels.
                 3.17.5 Bulk materials handling.
         4. ATTRITION BEHAVIOUR IN SLURRIES.
             4.1 Agitated vessels.
             4.2. Implications for scale-up.
             4.3. Effect of growing vs non-growing conditions.
         5. PREDICTION OF PRODUCT PARTICLE SIZE DISTRIBUTION.
             5.1. Population balance.
             5.2. Particle Birth and Death functions.
             5.3. Correlation of S(L) and B(x, L) functions.
             5.4. Effect of residence time distribution on PSD in a comminution process.
         6. DISCUSSION AND CONCLUSIONS.
         7. RECOMMENDATIONS FOR FURTHER WORK.
         8 NOMENCLATURE
         9 BIBIOGRAPHY
         APPENDIX 1. FUNDAMENTALS OF ATTRITION AND BREAKAGE.
             10.1. Introduction.
             10.2. The Griffith concept.
                 10.2.1. Stress concentrators.
                 10.2.2. Griffith energy balance concept: equilibrium fracture.
                 10.2.3. Crack in uniform tension.
                 10.2.4. Molecular theory of strength.
                 10.2.5. Griffith flaws.
                 10.2.6. Further considerations.
             10.3. Continuum aspects of crack propagation.
                 10.3.1. Linear elastic tip field.
                 10.3.2. Crack system as a thermodynamic cycle.
             10.4. Indentation fracture.
                 10.4.1. Crack propagation in contact fields: blunt and sharp indenters.
                 10.4.2. Contact stress fields.
             10.5. Processing flaws in particles.
         APPENDIX 2. ATTRITION TEST METHODS.
             11.1. Introduction.
             11.2. Single particle crushing tests.
             11.3. Single particle impact tests.
             11.4. Multi particle tests.
             11.5. Fluidised bed tests.
             11.6. Shear testing.
             11.7. Drum tests.
             11.8. Grindability tests.
             11.9. Drop shatter tests.
             11.10. Confined compression tests.
             11.11. Paddle wheel tests.
             11.12. Enhanced sieving.
             11.13. Viscometer tests.
             11.14. Chemical reaction tests.
             11.15. Pressure change tests.
             11.16. Decrepitation tests.
             11.17. Fluid transport.
         APPENDIX 3. THE ROLE OF FLUID DYNAMICS.
             12.1. Introduction.
             12.2. Impact attrition.
             12.3. Turbulent attrition.
             12.4. Scale-up.
         APPENDIX 4. Definitions
     Part 4: Chemical and Physical Crystal Purity
         1. INTRODUCTION
             1.1 Scope and Relationship with other Manual Parts
             1.2 Scope and Extent of the Literature
         2. CRYSTAL PURITY AND PROCESSING
             2.1 Definition of Purity Requirements
             2.2 Impurities, Nucleation and Growth
             2.3 Impurity Retention and Downstream Processing
         3. MECHANISMS OF IMPURITY INCORPORATION
             3.1 Physical Impurities
                 3.1.1 Polymorphism
                 3.1.2 Amorphous phases
             3.2 Chemical Impurities
                 3.2.1 Distinct impurity phases
                 3.2.2 Stoichiometric impurities
                 3.2.3 Non-stoichiometric impurities
         4. TROUBLE-SHOOTING STRATEGY
             4.1 Warning Signs and Schemes for Impurity Identification.
             4.2 Methods of Impurity Identification, Location and Quantification.
                 4.2.1 Chemical Impurities.
                 4.2.2 Physical Impurities
             4.3 Identification of remediation options.
         5. PURITY IN PROCESS DEVELOPMENT
             5.1 Review of Anticipated Problems
                 5.1.1 Impurities in feed materials
                 5.1.2 Product requirements
                 5.1.3 Process related purity issues
             5.2 Selection of Isolation Conditions
                 5.2.1 Experiments to determine purity characteristics
                 5.2.2 Impurity incorporation associated with end point
             5.3 Process Optimization
         6. GLOSSARY OF SYMBOLS
         7. REFERENCES
     Part 5: Troubleshooting Guide for Crystallization Systems
         1. PROBLEM IDENTIFICATION
             1.1 Establish Problem Statement
                 1.1.1 Production rate
                 1.1.2 Crystal size
                 1.1.3 Crystal shape
                 1.1.4 Crystal purity
                 1.1.5 Foaming
                 1.1.6 Scale formation
                 1.1.7 Erosion
                 1.1.8 Corrosion
             1.2 Define the System
                 1.2.1 Crystallizer only
                 1.2.2 Crystallizer with preconcentration
                 1.2.3 Crystallizer with centrifuge or filter
                 1.2.4 Crystallizer with centrifuge/filter and dryer
             1.3 Define the Crystallizer
                 1.3.1 Continuous crystallizers
                 1.3.2 Batch crystallizers
                 1.3.3 Reaction crystallizers
                 1.3.4 Evaporative crystallizers
                 1.3.5 Vacuum cooled crystallizers
                 1.3.6 Surface cooled crystallizers
                 1.3.7 Direct contact cooled crystallizers
             1.4 Define the Expected Crystallizer Performance
                 1.4.1 Specified performance
                 1.4.2 Theoretical performance
             1.5 Define the Actual Crystallizer Performance
                 1.5.1 Mass balance
                 1.5.2 Energy balance
                 1.5.3 Chemistry
                 1.5.4 Crystal characterization
             1.6 Define The Actual System Performance
                 1.6.1 System mass balance
                 1.6.2 System energy balance
                 1.6.3 System chemistry
             1.7 Differences Between Expected and Actual Performance
             1.8 Revise / Develop Final Problem Statement
         2. PROBLEM SOLUTION
             2.1 Identification of Similar Cases
                 2.1.1 Case histories
                 2.1.2 Theoretical extrapolations
             2.2 Develop Strategy
                 2.2.1 Solution statement
                 2.2.2 Priorities
             2.3 Test Strategy
                 2.3.1 Energy balance
                 2.3.2 Material balance
                 2.3.3 Chemistry
                 2.3.4 Crystal size
                 2.3.5 Crystal shape
             2.4 Implement Solution
             2.5 Confirmation of Success
         3. Appendix 1
         4. Appendix 2
         5. Appendix 3
         6. Appendix 4
         7. Appendix 5

Volume VI helps the user to avoid operational problems or improve the performance of existing crystallizers.

Volume CR VI  Part 1 Tailoring of crystal size distribution.

The crystal size distribution (CSD) of the product from a crystallizer is obviously important, and the product requirements may specify that a particular distribution must be achieved. The crystal size distribution can also affect downstream processing, solids and slurry transport, and the caking and storage properties of the material. Achievement of the correct crystal size can be vital for economic production.

This guide shows how to modify the product crystal size distribution obtained from a working crystallizer; it also contains a section concerning the design of new crystallizers. Crystal size distribution problems are divided into 6 basic categories:

  • Mean size too low.
  • Mean size too high.
  • Too many fines present.
  • Too many large crystals present.
  • Distribution too wide.
  • Distribution varying erratically.

The guide contains four sets of logic diagrams:

  • Identification of the basic problem category or categories.
  • Identification of low cost/short time scale solutions.
  • Identification of medium cost/medium time scale solutions.
  • Identification of high cost/long time scale solutions.

This report also forms the basis of the CRYSES expert system.


Volume CR VI  Part 2 Encrustation of crystallizers.

Wherever high supersaturation is present in a crystallizer, encrustation and fouling can occur. This will reduce crystallizer performance by:

  • Reducing heat transfer rates.
  • Acting as nuclei sources.
  • Reducing the working volume of the crystallizer.
  • Causing physical damage to the crystallizer if large crystal masses become detached.

Six fouling mechanisms are discussed - particulate deposition, scaling, chemical reaction (corrosion), polymerization, biological fouling and freezing. The prevention or minimisation of fouling is a factor which should be considered when designing or operating crystallizers. The report discusses both aspects, providing guide-lines to both designers of new crystallization equipment and operators of existing equipment encountering fouling and encrustation problems.


Volume CR VI  Part 3 Attrition and Breakage. This report provides guidance on the control of attrition and breakage during crystallization. The report contains sections on characterisation of the impact of attrition on granular solids, attrition behaviour in stirred and description of attrition phenomena in terms of the particle size distribution. The manual also contains extensive appendices on the more fundamental aspects of attrition and breakage, attrition testing methodologies and the role of fluid dynamics on particle breakage.
Volume CR VI  Part 4 Chemical and Physical Purity. This report provides a structured approach to addressing crystal purity problems. It begins by distinguishing between chemical impurity and physical impurity (polymorphism and amorphous phases). It continues with a review of the different mechanisms by which impurities can be incorporated within the product, each mechanism being illustrated with suitable examples from the literature. The report then addresses troubleshooting; it lists potential warning signs, indicates methods to identify, quantify and locate impurities and suggests suitable remediation options. The report ends with a section on purity in process development which offers guidelines on how to improve product purity in development through careful selection of isolation conditions and design of the crystallization process.
Volume CR VI  Part 5 Troubleshooting a Continuous Crystallization Process. This manual part on troubleshooting continuous crystallizers is written from the practical experience gained through many years of developing, commissioning and troubleshooting continuous crystallization plant. The manual begins with the identification of the problem and defining a problem statement. This is followed by a practical approach to specifying the crystallizer and associated plant and its anticipated performance. The next step is the collection of data to help quantify the actual performance of the unit. This is focused around the construction of the heat and mass balance and characterisation of the product stream. The potential pitfalls in this process are identified and strategies to help avoid them are given. Comparison of the anticipated performance of the unit and its actual performance should help to diagnose the problem more fully. At this point the problem statement can be reassessed and modified if necessary and a list of potential causes can be drawn up and reviewed with the process "owner". The potential solutions can then be considered and ranked and an action plan formulated. An important issue at this stage in the process is the management of the implementation of the proposed changes and the expectations of the process owner and operators. This should include the expected response of the system to the proposed change, the perceived probability of success and the next line of action to be taken in the event of failure. The report ends with some guidance on ensuring the problem is solved and does not recur. The report is written to be used in a troubleshooting situation and its style reflects this, it is not an academic thesis, but rather a practical document designed to assist those facing operational problems.