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SE 6: Liquid Liquid Extraction Equipment

SE 6: Liquid Liquid Extraction Equipment
     Part 1: Introduction
         1. SOLVENT EXTRACTION EQUIPMENT
             1.1 Equipment Classification and Selection
             1.2 Equipment Design
     Part 2: The Classification and Selection of Solvent Extraction Contactors
         1. INTRODUCTION
             1.1 Background
             1.2 Principles of Solvent Extraction Equipment
             1.3 Current Usage of Extractor Equipment
             1.4 Objectives and Layout
         2.CONTACTOR CLASSIFICATION AND DEVELOPMENT
             2.1 Contactor Classification Scheme
                 2.1.1 Classification Schemes Used in the Literature
                 2.1.2 Developed Scheme
             2.2 Liquid-Liquid Extraction Contactors
                 2.2.1 Vertical Differential (Column) Contactors
                 2.2.2 Horizontal Differential Contactors
                 2.2.3 Vertical Staged Contactors
                 2.2.4 Horizontal Stagewise Contactors (Mixer-Settlers)
                 2.2.5 Centrifugal Extractors
                 2.2.6 Other Contactors
                 2.2.7 Equipment for Supercritical Extraction
         3. EXTRACTORS IN COMMERCIAL USE
             3.1 Random-Packed Column
             3.2 Structured-Packed Column
             3.3 Baffle-Plate Columns /Slat Tower
             3.4 Sieve Plate (Sieve Tray) Column
             3.5 Pulsed Packed Column
             3.6 The Pulsed Perforated Plate Column
             3.7 The Reciprocating Plate (Karr) Extraction Column
             3.8 The Rotating Disc Contactor
             3.9 The Asymmetric Rotating Disc Extractor
             3.10 Oldshue-Rushton Column
             3.11 The Scheibel Column
             3.12 The Kuhni Column
             3.13 The Raining Bucket (Graesser) Contactor
             3.14 The Lurgi Extraction Tower
             3.15 The Combined Mixer-Settler
             3.16 The Integral Box Mixer-Settler
             3.17 Pump Mix Mixer-Settlers
             3.18 The IMI Mixer-Settler
             3.19 Lurgi Mixer-Settlers
             3.20 The Podbielniak Centrifugal Extractor
             3.21 Alfa-Laval Centrifugal Extractor
             3.22 The Westfalia Extractor
             3.23 Eries Robatel BXP Centrifugal Extractor
             3.24 The ANL/SRL Annular Centrifugal Extractor
             3.25 The Luwesta Extractor
             3.26 The Eries Robatel LX Centrifugal Extractor
             3.27 Hydrocyclone and 'Fluidic' Extractors
             3.28 Non-Dispersive Extraction: Hollow Fibre Membrane Extractors
         4. CONTACTOR DESIGN AND SIZING
             4.1 Introduction
             4.2 Data Gathering
             4.3 Design of Columns
                 4.3.1 Column Diameter
                 4.3.2 Column Height
                 4.3.3 Mechanical Design and Operation
                 4.3.4 Column Simulation
             4.4 The Design of Mixer-Settlers
                 4.4.1 Settler Design
                 4.4.2 Mixer Design
                 4.4.3 Phase Dispersed
                 4.4.4 Secondary Haze
             4.5 The Design of Centrifugal Contactors
                 4.5.1 Stagewise, Mixer-Settler, Contactors
                 4.5.2 Differential Contactors
         5. CONTACTOR SELECTION
             5.1 Selection Criteria Point Score Method
                 5.1.1 Data Needed
                 5.1.2 Selection Criteria
             5.2 Decision Tree Method of Selection
                 5.2.1 Basic Selection Criteria
         6. ANCILLARY EQUIPMENT
             6.1 Agitation and Pulsing Equipment
             6.2 Phase Disentrainment
             6.3 Condition Monitoring and Control
                 6.3.1 Interface Detection and Control
                 6.3.2 Sampling Equipment
                 6.3.3 Future Developments
         7. CONCLUSIONS
         8. NOMENCLATURE
         9.REFERENCES
         10. APPENDIX A. CONTACTORS IN USE BY SPS SUBSCRIBING COMPANIES
         11. APPENDIX B. EXAMPLES OF CONTACTOR SELECTION PROCEDURE
     Part 3: Mathematical Methods
     Part 4: Scale up of Liquid-Liquid Extraction Equipment
         1 INTRODUCTION
             1.1 Scale Up Philosophies
             1.2 Contactor Characteristics
             1.3 The Performance of Column Contactors
                 1.3.1 Throughput
                 1.3.2 Mass Transfer
                 1.3.3 Axial Mixing
             1.4 The Performance of Mixer-Settlers
                 1.4.1 The Mixer
                 1.4.2 The Settler
             1.5 General Aspects of Scale Up
         2. UNAGITATED COLUMN CONTACTORS
             2.1 Packed Columns
                 2.1.1 Hydrodynamics
                 2.1.2 Flooding
                 2.1.3 Drop Size
                 2.1.4 Hold-up
                 2.1.5 Mass Transfer
                 2.1.6 Axial Mixing
                 2.1.7 Less Fundamental Studies
                 2.1.8 Conclusions
             2.2 Perforated Plate Columns
                 2.2.1 Introduction
                 2.2.2 Capacity
                 2.2.3 Mass Transfer Performance
                 2.2.4 Axial Mixing
                 2.2.5 Discussion
         3. PULSED COLUMN CONTACTORS
             3.1 Pulsed Perforated Plate Columns
                 3.1.1 Hydrodynamics
                 3.1.2 Drop Sizes
                 3.1.3 Mass Transfer Correlations
                 3.1.4 Axial Mixing
                 3.1.5 Constructional Details and Pulsation Methods
                 3.1.6 Conclusions
             3.2 Reciprocating Plate Columns
                 3.2.1 Hydrodynamics
                 3.2.2 Mass Transfer Performance
                 3.2.3 Power Consumption
                 3.2.4 Prochazka Column
                 3.2.5 Conclusions
             3.3 Pulsed Packed Columns
                 3.3.1 Hydrodynamics
                 3.3.2 Flooding
                 3.3.3 Drop Size
                 3.3.4 Mass Transfer
                 3.3.5 Pulsation Methods
                 3.3.6 Conclusions
         4. ROTARY AGITATED CONTACTORS
             4.1 Rotating Disc Contactors
                 4.1.1 Column Throughput
                 4.1.2 Drop Size
                 4.1.3 Axial Mixing and Mass Transfer
             4.2 Asymmetric Rotating Disc Contactor
             4.3 Oldshue-Rushton Column Contactor
             4.4 Kuhni Column
                 4.4.1 Drop Size
                 4.4.2 Hold-up and Slip Velocity
                 4.4.3. Throughput
                 4.4.4 Axial Mixing
                 4.4.5 Scale Up
             4.5 Scheibel Column
             4.6 Raining Bucket Contactor
         5. CENTRIFUGAL CONTACTORS
         6. MIXER-SETTLERS
             6.1 Power Input
             6.2 Drop Size in the Mixer
             6.3 Batch Kinetics
             6.4 Rate Controlling Mechanisms and Scale up Relationships
             6.5 Stability and Entrainment
             6.6 Settler Area
             6.7 Effect of Drop Size on Depth of Dispersion Band
             6.8 Settler Shape
             6.9 Entrainment from the Settler
         7 CONCLUSIONS AND RECOMMENDATIONS FOR FUTURE WORK
         NOMENCLATURE
         REFERENCES
     Part 5: Column Design
         1. INTRODUCTION
             1.1 Basic Phenomena in Liquid-Liquid Extraction Column Contactors
                 1.1.1 Industrial column contactors
                 1.1.2 Agitation mechanisms
                 1.1.3 Hydrodynamic factors; throughput and flooding
                 1.1.4 Factors affecting mass transfer
                 1.1.5 Selection of dispersed phase
                 1.1.6 Axial mixing; definitions, effects and measurement
             1.2 Constraints on Contactor Selection
                 1.2.1 Volumetric throughput and number of transfer units
                 1.2.2 System physical properties
                 1.2.3 Other constraints
             1.3 Arrangement of Design Report
         2. DESIGN SUMMARY
             2.1 Design Flow Diagram
             2.2 Basic Design Equations
         3. BASIC DATA
             3.1 Physical Properties
                 3.1.1 Density
                 3.1.2 Viscosity
                 3.1.3 Interfacial tension
             3.2 Molecular Diffusivity
             3.3 Equilibrium Data
             3.4 Liquid-Liquid-Solid Wetting Properties
         4. PRELIMINARY CALCULATIONS
             4.1 Number of Transfer Units and Flow Ratio
                 4.1.1 Single transferring solute
                 4.1.2 Multiple Interacting solutes
             4.2 Specific Throughput and Limits on Diameter
             4.3 Phase Dispersed
             4.4 Preliminary Contactor Selection
             4.5 Estimate of Internal Geometry
                 4.5.1 Critical packing size
                 4.5.2 Packing type and material
                 4.5.3 Critical sieve plate perforation or nozzle diameter
                 4.5.4 Compartment height
                 4.5.5 Plate free area, and perforation and aperture diameters
                 4.5.6 Rotor diameter
             4.6 Intensity of Agitation and Power Consumption
                 4.6.1 Pulse amplitude and frequency in a pulsed column
                 4.6.2 Rotor speed in a rotary-agitated column
                 4.6.3 Total and specific power input
             4.7 Future Developments
         5 HYDRODYNAMICS, OPERATING VELOCITIES AND COLUMN DIAMETER
             5.1 Calculation of Flooding Velocity
                 5.1.1 Drop size prediction
                 5.1.2 Terminal velocities
                 5.1.3 Characteristic velocities
                 5.1.4 Calculation of exponent in Richardson and Zaki equation for slip velocity
                 5.1.5 Calculation of velocity and hold-up at flooding due to drop rejection from column
             5.2 Flooding Conditions due to Insufficient Pulsation in a Pulsed Sieve Plate Column
             5.3 Operating Velocities and Hold-up
             5.4 Revised Column Diameter
             5.5 Future Developments
         6. MASS TRANSFER
             6.1 Mass Transfer Coefficients
                 6.1.1 Continuous phase mass transfer coefficient
                 6.1.2 Dispersed phase mass transfer coefficient
                 6.1.3 Overall mass transfer coefficients
             6.2 Height of Transfer Unit in Plug Flow
         7. AXIAL MIXING AND CORRECTED COLUMN HEIGHT
             7.1 Axial Mixing Coefficients
                 7.1.1 Packed columns
                 7.1.2 Pulsed sieve plate columns
                 7.1.3 RDC/ARDC
                 7.1.4 Kuhni column
             7.2 Calculation of Column Height Corrected for Axial Mixing
                 7.2.1 Single or non-interacting solutes and linear equilibrium: method of Pratt
                 7.2.2 Multiple interacting solutes: method of Ricker et al (1981)
         8. MECHANICAL DESIGN AND OPERATION
             8.1 End Section and Phase Distribution Design
                 8.1.1 Design of dispersed phase distributor
                 8.1.2 Disengaging zone
             8.2 Interface Detection and Control
                 8.2.1 Interface detection for automatic control
                 8.2.2 External settler
             8.3 Agitation Equipment
                 8.3.1 Pulsed columns
                 8.3.2 Rotary-agitated columns
             8.4 Start-up and Shut-down
             8.5 Sampling
             8.6 Suspended and Interfacial Contamination
         9. SCALE-UP OF PROVEN COLUMN DESIGN
             9.1 General Principles
                 9.1.1 Effect of scale on HTU for specific equipment
         10. FINAL CONTACTOR SELECTION
             10.1 Materials of Construction
                 10.1.1 Structural materials
                 10.1.2 Sealing materials
                 10.1.3 Laboratory compatibility tests for materials
         11. SAFETY AND ENVIRONMENTAL CONSIDERATIONS
         12. ACKNOWLEDGEMENTS
         13 NOMENCLATURE
         14 REFERENCES
         15 APPENDIX 1 PHYSICAL PROPERTIES OF LIQUID-LIQUID SYSTEMS
         16 APPENDIX 2 WORKED EXAMPLE
             16.1 Problem Setting
                 16.1.1 Physical Properties
                 16.1.2 Equilibrium Data
             16.2 Design Calculations: Packed Column
                 16.2.1 First Iteration
                 16.2.2 Packed Column: Second Iteration
                 16.2.3 Packed Column: Third Iteration
             16.3 Design Calculation: RDC
                 16.3.1 First Iteration
                 16.3.2 RDC Design: Second Iteration
             16.4 Design Calculation: Pulsed Column
                 16.4.1 MEK Balance
                 16.4.2 Number of Transfer Units
                 16.4.3 Calculation of Parameters Specific to a Pulsed Column
                 16.4.4 Drop Size Calculation
                 16.4.5 Terminal Velocities
                 16.4.6 Characteristic Velocity Uo
                 16.4.7 Calculation of Flooding Velocity
                 16.4.8 Operating Velocity
                 16.4.9 Holdup under Operating Conditions
                 16.4.10 Revised Column Diameter
                 16.4.11 Mass Transfer Calculations
                 16.4.12 Height of Plug Flow Transfer Unit
                 16.4.13 Column Height for Plug Flow
             16.5 Preliminary Contactor Selection
             16.6 Calculation of Column Height Corrected for Axial Mixing in RDC
                 16.6.1 Calculation of Continuous Phase Peclet Number
                 16.6.2 Extraction Parameters (Equations 7.8 and 7.10)
                 16.6.3 Coefficients b 1 , l 1 , a 4 (Equations 7.12c, 7.13c, 7.17c, 7.18)
                 16.6.4 Corrected Column Height Z (Equation 7.19c)
     Part 6: Integral Box Mixer Settlers
         1. INTRODUCTION
             1.1 Objectives of a mixer-settler
             1.2 Factors governing performance of mixer
             1.3 Factors governing performance of settler
             1.4 Principal existing types of mixer-settler
             1.5 The integral box mixer-settler
         2. THE DESIGN APPROACH
             2.1 Discussion
             2.2 Summary of design approach
             2.3 Basic Design Guide
         3. GENERATION OF PRELIMINARY DATA
             3.1 Physical properties
             3.2 Separating funnel work and standardised mixing tanks
             3.3 Equilibrium data
             3.4 Kinetic data
             3.5 Phase separation characteristics from batch tests
             3.6 Choice of phase to disperse and hold-up considerations
             3.7 Choice of temperature of operation
         4. PRELIMINARY MIXER-SETTLER DESIGN
             4.1 Volume of mixing vessel
             4.2 Pressure drop through ports between mixer and settler
             4.3 Flow rate over weirs
             4.4 Calculation of liquid levels in the settler
             4.5 Minimum solvent depth
             4.6 Summary of procedure for non-submerged top weirs
             4.7 Total liquid heights for submerged top weirs
             4.8 Summary of procedure for submerged top weirs
             4.9 Effect of dispersion band thickness
             4.10 Effect of density variations
             4.11 Effect of interface level above mixed phase port
             4.12 Settler area
         5. PILOT PLANT
             5.1 Design from batch data
             5.2 Objectives of experimental programme
         6. FINAL MIXER-SETTLER DESIGN
             6.1 Finalise decision on operation with non-submerged or submerged top weir
             6.2 Finalise shape of mixer
             6.3 Finalise settler area for gravity separation without baffles
             6.4 Settler improvement with baffles and packings
             6.5 Position of impeller
             6.6 Choice of impeller speed, impeller diameter and power requirement (1)
             6.7 Scale-up procedures
             6.8 Entrainment
             6.9 Design of terminal stages
             6.10 Design uncertainties
         7. OPERATIONAL CONSIDERATIONS
             7.1 Start-up and Shut Down
             7.2 Dynamic characteristics and control
             7.3 Sampling and control measurements
             7.4 Flooding and inversion
             7.5 Crud formation and treatment
             7.6 Evaporative losses
             7.7 Recovery of entrained phases
             7.8 Materials of construction
             7.9 Safety and environmental considerations
             7.10 Improving the performance of existing mixer-settlers
             7.11 Application of integral box design method to pump-mixer-settler
         8. REFERENCES
         9. NOMENCLATURE
         10. APPENDIX 1
         11. APPENDIX 2 Examples of design calculations
             11.1 Design basis
             11.2 Estimation of mixer volume and stage efficiency from batch tests
             11.3 First estimate of dispersion band thickness/flow equation from batch test
             11.4 Volume of mixing vessel
             11.5 Pressure drops through ports
             11.6 Flow rate over weirs
             11.7 Example calculation of levels for non-submerged top weirs
             11.8 Example calculation of levels with submerged top weirs
             11.9 Example calculation of interface level effect
             11.10 Calculation of settler dimensions
             11.11 Scale-up of batch data using power/unit volume
             11.12 Scale-up of batch data using constant tip speed
     Part 7: Pump-mix Mixer Settlers
         1. INTRODUCTION
             1.1 The pump-mix impeller
             1.2 Aspects of pump-mix impeller performance
             1.3 Settler designs
             1.4 Aspects of settler performance
             1.5 The pump-mix mixer-settler
         2. THE DESIGN APPROACH
             2.1 Introduction
             2.2 Basic design guide
                 2.2.1 Physical properties
                 2.2.2 Estimation of stage efficiencies (Appendix 3)
                 2.2.3 Mixer size
                 2.2.4 Estimated impeller size, speed and power ranges (Section 6.2)
                 2.2.5 Design a pilot plant mixer (Appendix 5.1 to 5.4 and 5.6)
                 2.2.6 Pumping requirements (Section 4.5) (Appendix 5.5)
                 2.2.7 Extraction rate (Appendix 6.2)
                 2.2.8 Full scale design
                 2.2.9 Settler design
         3. GENERATION OF PRELIMINARY DATA AND INTERPRETATION
             3.1 Physical properties
             3.2 Separating funnel work and standardized mixing tanks
             3.3 Equilibrium data
             3.4 Kinetic data
             3.5 Phase separation rate tests
             3.6 Choice of phase to disperse and hold-up considerations
             3.7 Choice of temperature of operation
         4. PRELIMINARY MIXER DESIGN
             4.1 Mixer design principles
             4.2 Equilibrium considerations
             4.3 Mixer configuration
             4.4 Kinetic considerations
             4.5 Pumping performance
             4.6 Other aspects of mixer performance
             4.7 Recommendations for preliminary mixer design
         5. PRELIMINARY SETTLER DESIGN
             5.1 Settler design principles
             5.2 Settler configuration
             5.3 Inlet arrangements
             5.4 Flow patterns in settlers
             5.5 Weir and off-take points
             5.6 Settler liquid depths
             5.7 Multi-tray settlers
             5.8 Coalescers
             5.9 Entrainment
             5.10 Removal of haze
             5.11 Baffles and deep dispersion bands
             5.12 General comments
         6. PILOT PLANT
             6.1 Design from batch data
             6.2 Impeller characterization
             6.3 Objectives of experimental programme
         7. FINAL MIXER-SETTLER DESIGN
             7.1 Impeller type and pumping methods
             7.2 Configuration of mixer
             7.3 Positions of impellers and inlets
             7.4 Impeller size, speed, power
             7.5 Configuration of settler
             7.6 Settler inlet arrangement
             7.7 Settler internals
             7.8 Weirs
             7.9 Design uncertainties
         8. OPERATIONAL CONSIDERATIONS
             8.1 Start-up and shut-down
             8.2 Dynamic characteristics and control
             8.3 Interface level and sampling
             8.4 Flooding and inversion
             8.5 Crud formation and treatment (Ritcey and Ashbrook, 1979)
             8.6 Evaporative losses
             8.7 Materials of construction (Ritcey and Ashbrook, 1979)
             8.8 Safety and environmental considerations
             8.9 Improving the performance of existing mixer-settlers
         9. REFERENCES
         10. NOMENCLATURE
         11. APPENDIX 1 Approximate Properties at 20 to 30 'C
         12. APPENDIX 2 EXAMPLE CALCULATIONS
         13. APPENDIX 3 Estimates for Continuous Extraction from Batch Data
         14. APPENDIX 4 Preliminary Design of Full Scale Plant from Batch Data
             14.1 A4.1 Residence time
             14.2 A4.2 Mixer volume
             14.3 A4.3 Impeller speed
         15. APPENDIX 5 Pilot Plant Design
             15.1 A5.1 Residence time
             15.2 A5.2 Mixer volume
             15.3 A5.3 Impeller speed
             15.4 A5.4 Impeller selection
             15.5 A5.5 Pumping considerations
             15.6 A5.6 Power consumption
             15.7 A5.7 Operational considerations
         16. APPENDIX 6 Collection of Pilot Plant Data
             16.1 A6.1 Pumping characteristics
             16.2 A6.2 Extraction rate
         17. APPENDIX 7 Full Scale Mixer Design
             17.1 A7.1 Extraction rate
             17.2 A7.2 Pumping capacity
             17.3 A7.3 Pumping head requirement
         18. APPENDIX 8 Solvent Depth in an Integral Box Mixer-Settler
         19. APPENDIX 9 Analysis of Separation Rate Data
         20. APPENDIX 10 Design of Settler Using Separation Rate Data
         21. APPENDIX 11 Multi-Tray Coalescer
         22. APPENDIX 12 Baffles and Deep Dispersion Bands
     Part 8: Gravity Settlers
         1. INTRODUCTION
             1.1 Aim and Scope of Design Report
             1.2 Design Constraints
                 1.2.1 Process constraints
                 1.2.2 Mixer constraints
             1.3 Classes of Industrial Settler
                 1.3.1 Bulk flow mainly horizontal
                 1.3.2 Bulk flow mainly radial/vertical
                 1.3.3 Bulk flow vertical: split dispersion band
                 1.3.4 Multi-tray settlers
                 1.3.5 Centrifugal settler
             1.4 Special Case: Clarification by Sedimentation; Coalescence not Rate-limiting
             1.5 Models for Liquid-Liquid Disengagement: The State of the Art
                 1.5.1 Overall features of dispersion disengagement in a settler
                 1.5.2 Mechanisms of coalescence
                 1.5.3 The relationship between dispersion band height and disengagement velocity in continuous flow and batch experiments
             1.6 Superficial and Slip velocities in Differential and Continuous Disengagement
                 1.6.1 Differential
                 1.6.2 Continuous flow
         2. DESIGN GUIDE
             2.1 The Design Flowcharts
             2.2 Summary
             2.3 Basic Design Equations
         3. PREDICTION OF CONTINUOUS FLOW DISPERSION BAND HEIGHT AS A FUNCTION OF DISENGAGEMENT VELOCITY
             3.1 Basis of the Calculations
             3.2 Procedure for a Stopped-Flow Differential Disengagement Test
                 3.2.1 Laboratory mixer
                 3.2.2 Procedure
             3.3 Interpretation of Disengagement Results
                 3.3.1 Types of differential disengagement curve
                 3.3.2 Sedimentation with interdrop coalescence
                 3.3.3 Simple exponential decay of dispersion height
         4. DIMENSIONS OF THE DISENGAGING ZONE
             4.1 Choice of Dispersion Band Depth or Flow Velocity
             4.2 Alternative Settler Shapes
             4.3 Dimensions for a Rectangular Settler
             4.4 Dimensions for a Diverging Settler
         5. INTERNALS OF THE GRAVITY SETTLER
             5.1 Inlet Arrangement
                 5.1.1 Aim of good inlet design
                 5.1.2 Design of the mixed phase inlet port
             5.2 Role of Turbulence-Calming and Flow Redistribution Devices
                 5.2.1 Number of baffle elements
             5.3 Outlet Arrangement
                 5.3.1 Horizontal velocity of separated phases
             5.4 Dimensions of Weirs and Ports
                 5.4.1 Height of light phase weir
                 5.4.2 Height of heavy phase weir
                 5.4.3 Height of dispersed phase in preceding mixer
                 5.4.4 Thickness of slot ports
             5.5 The Function of a Dam Baffle Within the Settler
             5.6 Other Internals
         6. DESIGN STRATEGEM FOR OTHER GEOMETRIES
             6.1 Combined Mixer-Settler
                 6.1.1 Mode of operation
                 6.1.2 Dispersion band heights in the CMS
                 6.1.3 Height of heavy phase weir
             6.2 Multi-Tray Settler
                 6.2.1 Criteria for selection of multi-tray design
                 6.2.2 Proprietary designs
                 6.2.3 Sizing an IMI multi-tray settler
                 6.2.4 Upgrading of an existing box settler
                 6.2.5 Sizing a Lurgi multi-tray settler
                 6.2.6 Multi-tray devices for secondary dispersions
             6.3 Centrifugal Separators
             6.4 The Disengaging Zone of a Column Contactor
                 6.4.1 Sizing of disengaging zone from a batch test
         7. OPERATIONAL CONSIDERATIONS
             7.1 Start-up and Shut-down
             7.2 Dynamic Flowrate Variations and Control
             7.3 Instrumentation
             7.4 Crud Control
             7.5 Safety of Settlers and Associated Plant
         8. MATERIALS OF CONSTRUCTION
             8.1 Structural materials
             8.2 Sealing Materials
             8.3 Laboratory Compatibility Tests for Settler Materials
         9. REFERENCES
         10. NOMENCLATURE
         11. APPENDIX 1 WORKED EXAMPLES
             11.1 EXAMPLE 1 (S-SHAPED COALESCENCE CURVE)
             11.2 EXAMPLE 2 ('EXPONENTIAL' DECAYING COALESCENCE CURVE)
         12. APPENDIX 2 DERIVATION OF EQUATIONS FOR DIFFERENTIAL AND CONTINUOUS FLOW DISENGAGEMENT
             12.1 A2.1 Drop growth during sedimentation
             12.2 A2.2 Sedimentation velocities
             12.3 A2.3 Derivation of sedimenting zone parameters from a differential sedimentation curve
             12.4 A2.4 Sedimentation in continuous flow, height of the dispersion band
             12.5 A2.5 Simplified, high Reynolds Number, analysis
     Part 9: Design of Tank Reactors for the Processing of Dispersed Liquid Systems
         1. INTRODUCTION TO THE DESIGN OF TANK REACTORS
             1.1 General Design Features of Tank Reactors
             1.2 Physical, Kinetic and Transport Data Collation
             1.3 Equations of Conservation of Mass and Energy in a Tank Reactor
             1.4 Arrangement of This Part
         2. DESIGN SUMMARY
         3. CHEMICAL REACTION KINETICS
             3.1 Batch Reactors
                 3.1.1 Mass Transfer Controlled Process
                 3.1.2 Chemical Reaction Controlled Process
                 3.1.3 Batch: Reactions in both Phases
             3.2 Two Phase Continuous Flow Reactors
                 3.2.1 Cross Flow Operation
                 3.2.2 Counterflow Operation
             3.3 Short Cut Design Procedure
             3.4 Choice of Reactor System
                 3.4.1 Yield and Selectivity
                 3.4.2 Safety
         4. AGITATION DESIGN AND RESIDENCE TIME DISTRIBUTION
             4.1 Agitator Design and Selection
                 4.1.1 Basic Flow Patterns and Bulk Velocities in Agitated Tanks
                 4.1.2 Agitator Types
                 4.1.3 Emulsion Formation
                 4.1.4 Vortex Formation and Suppression
                 4.1.5 Agitator Selection
                 4.1.6 Uniformity of Dispersion
                 4.1.7 Power Requirements for Agitation
                 4.1.8 Time For Uniform Blending
             4.2 Residence Time Distributions
                 4.2.1 The F Diagram and Response to a Step Change
                 4.2.2 Interpretation of Age Distribution Diagrams
                 4.2.3 Residence Time Distributions in Two Phase Systems
                 4.2.4 Complex Reactions
         5. HOLD-UP, DROP SIZE AND INTERFACIAL AREA
             5.1 Dispersed Phase Hold-Up
             5.2 Minimum Impeller Speed
                 5.2.1 Complete Mixing
                 5.2.2 Uniform Dispersion
             5.3 Choice of Phase Dispersed
                 5.3.1 Batch Operation
                 5.3.2 Continuous Operation
                 5.3.3 Phase Inversion
             5.4 Interfacial Area
             5.5 Drop Size Prediction
                 5.5.1 Continuous Flow Systems
                 5.5.2 Unbaffled Vessels
                 5.5.3 The Effect of Surfactants or Stabilisers
             5.6 Drop Size Distributions
         6. HEAT TRANSFER
             6.1 Heat Transfer Considerations
             6.2 Agitated-Liquid Side Heat Transfer
             6.3 Coil or Jacket-Side Coefficients
         7. SCALE-UP CONSIDERATIONS
             7.1 Scale-Up: Empirical Rules
                 7.1.1 Scale-Up for Equivalent Dispersion
                 7.1.2 Scale-Up on Equal Peripheral Speed
                 7.1.3 Scale-Up for Heat Transfer
                 7.1.4 Scale-Up of Continuous Dispersion Operations
                 7.1.5 Scale-Up for Constant Mixing Time
         8. APPENDIX 1: WORKED EXAMPLES
             8.1 Design of a Suspension Polymerisation Reactor (Overall Design)
                 8.1.1 Reaction Kinetics of the Polymerisation of Styrene
                 8.1.2 Reactor Selection - Batch vs Continuous
                 8.1.3 Design of CSTR
                 8.1.4 Energy Requirements
                 8.1.5 Impeller Speed (N)
                 8.1.6 Dispersed Phase Hold-up and Interfacial Area
                 8.1.7 Materials of Construction
                 8.1.8 Control
                 8.1.9 Safety Considerations
                 8.1.10 Pressure Relief
             8.2 Calculation of the Ideal Number of Mixer-Settler Stages (Section 3.2)
             8.3 Short Cut Reactor Design Procedure (Section 3.3)
             8.4 Reactor Size Calculation Allowing for Drop Interaction (Section 4.1.6)
             8.5 Estimation of Power Consumption for a Turbine (Section 4.1.7)
             8.6 Calculation of Time for Complete Neutralisation (Section 4.1.8)
             8.7 E and F Table Analysis for Residence Times (Section 4.2.1)
             8.8 Determination of Mean Residence Time Using F Diagrams (Section 4.2.1)
             8.9 Calculation of Sauter Mean Drop Size (Section 5.3)
             8.10 Estimation of Hold-up (Section 5.5)
             8.11 Minimum Agitator Speed for Uniform Dispersion (Section 5.6)
             8.12 Estimation of Heating Time
                 8.12.1 Scale up of Heat Transfer Characteristics (Section 7.1
         9. APPENDIX 2: CHEMICAL REACTION KINETICS
             9.1 Chemical Reactions in a Tank Reactor
                 9.1.1 Metal Chelation Reactions
                 9.1.2 Nitration Reactions
                 9.1.3 Polymerisation Reactions
                 9.1.4 Phase Transfer Catalytic Reactions
             9.2 Two Phase Liquid Batch Reactors
                 9.2.1 The Dispersed Phase Consists of Pure Reactant
                 9.2.2 Batch Two Phase Reactions with Dilute Moderate Concentration Systems
             9.3 Two Phase Continuous Flow Reactors
                 9.3.1 Cross Flow Operation
                 9.3.2 Counterflow Operation
             9.4 Chemical Kinetics and Mass and Heat Transport
             9.5 Yield and Selectivity
         10. APPENDIX 3: REACTOR DESIGN
             10.1 Time for Uniform Blending
                 10.1.1 Homogeneous Systems
                 10.1.2 Mixing Theory
         11. REFERENCES
         12. NOMENCLATURE
     Part 10: In-line Mixers and their Scale-up
         1. INTRODUCTION
             1.1 Static Mixers and their Mode of Action
             1.2 Summary of Scale-up Calculation Procedure
         2. CALCULATION PROCEDURES
             2.1 Pressure Drop in Static Mixers
                 2.1.1 Chemineer Kenics
                 2.1.2 Lightin Inliner
                 2.1.3 Sulzer SMV
             2.2 Creating a Dispersion
                 2.2.1 Mixer length for dispersion
                 2.2.2 Mixer inlet geometry
                 2.2.3 Choice of phase dispersed and wetting; comparison with agitated tank
             2.3 Drop Size
                 2.3.1 Kenics
                 2.3.2 Inliner
                 2.3.3 SMV
             2.4 Extraction Rate
             2.5 Scale-up Considerations
                 2.5.1 Creating a dispersion
                 2.5.2 Drop size
                 2.5.3 Extraction rate
                 2.5.4 Scale-up procedure
                 2.5.5 Scale-up calculations
         3. DISCUSSION
             3.1 Energy Requirements
             3.2 Creating a Dispersion
                 3.2.1 Minimum velocity
                 3.2.2 Minimum number of mixing elements
                 3.2.3 Inlet geometry
                 3.2.4 Phase stability
             3.3 Drop Size
             3.4 Extraction Rate
             3.5 Scale-Up
                 3.5.1 Drop size and mass transfer
                 3.5.2 Pressure drop and energy dissipation
                 3.5.3 Residence time and mixer length
                 3.5.4 Mass transfer compensation for reduced mixing intensity
                 3.5.5 Phase stability
             3.6 Pilot Plant Design
                 3.6.1 Mixer diameter
                 3.6.2 Mixer length
                 3.6.3 Flow rates and velocity
                 3.6.4 Flow ratio
                 3.6.5 Data interpretation
             3.7 Dynamic In-line Mixers
                 3.7.1 Contact time
                 3.7.2 Mixer power
                 3.7.3 Drop size
                 3.7.4 Conclusion
         4. NOMENCLATURE
         5. REFERENCES
         APPENDIX 1. SPECIFICATION AND PRESSURE DROP ESTIMATION FOR KENICS MIXERS
         APPENDIX 2. DARCY FRICTION FACTOR PLOT
         APPENDIX 3. RAPID ESTIMATION OF VELOCITY REQUIRED FOR DISPERSION IN KENICS MIXERS
         APPENDIX 4. NEWTON NUMBERS FOR PRESSURE DROP IN SULZER SMV MIXERS
         APPENDIX 5. CORRELATION OF AVERAGE DROP SIZE WITH WEBER NUMBER
     Part 11: Structured Packing in Solvent Extraction Columns
         1. INTRODUCTION
             1.1 Aims and Structure of this Manual Part
             1.2 Introduction to Structured Packings
             1.3 Drop Breakage and Coalescence
                 1.3.1 Drop Breakage
                 1.3.2 Drop-drop Coalescence
         2. CHARACTERISTIC VELOCITY
         3. SINGLE DROP BREAKAGE
             3.1 Introduction
             3.2 Experimental Technique
             3.3 Experimental Results: Cumene-Water
             3.4 Experimental Results: Butanol-Water
             3.5 Conclusions
         4. MULTI-DROP BREAKAGE
             4.1 Introduction
             4.2 Experimental Technique
             4.3 Experimental Results: Cumene-Water
             4.4 Experimental Results: Butanol-Water
             4.5 Conclusions
         5. BINARY COALESCENCE
             5.1 Introduction
             5.2 Experimental Technique
             5.3 Experimental Results
             5.4 Drop-Drop Coalescence in 'Chasing' Mode
             5.5 Conclusions
         6. MULTI-DROP COALESCENCE
             6.1 Introduction
             6.2 Experimental Technique
             6.3 Experimental Results
             6.4 Conclusions
         7. MASS TRANSFER
             7.1 Introduction
             7.2 Experimental Technique
             7.3 Experimental Results
                 7.3.1 Single Drop Experiments
                 7.3.2 Swarm Experiments
             7.4 Conclusions
         8. OVERALL CONCLUSIONS
         9. NOMENCLATURE
         10. REFERENCES
         11. APPENDICES
             11.1 Breakage Data for Single Drops of Cumene in Water

Part 1   Introduction
Part 2   The classification and selection of solvent extraction equipment
Part 3   Mathematical methods for liquid-liquid extractors
Part 4   Scale-up of liquid-liquid extraction equipment
Part 5   Design of column contactors for liquid-liquid extraction
Part 6   Integral box mixer-settlers for solvent extraction processes
Part 7   The design of pump-mix mixer-settlers
Part 8   Design of simple gravity settlers for the coalescence of liquid-liquid dispersions
Part 9   Design of tank reactors for the processing of dispersed liquid systems
Part 10  In-line mixers and their scale-up

Volume SE VI   Part 1 Introduction.

This part gives an overview of the volume and how to use it to best effect.


Volume SE VI   Part 2 The classification and selection of solvent extraction equipment.

The wide diversity of types of contactor which have been described in the literature presents a bewildering choice to the design engineer not familiar with the subject. Various ways of classifying contactors are described. Most classifications first divide contactors into discrete-stage contactors and continuous differential contactors. These two broad categories can be divided further into sub-groupings. All types of contactor are listed and a brief description of each is given. Contactors used industrially are described in greater detail. The many criteria which need to be considered when selecting a contactor are discussed. Most appertain to a wide range of applications but some are applicable to specific processes. Not all can be satisfied simultaneously and most require value judgements to be made. A comprehensive contactor selection procedure using a point score method is used. The various items of ancillary equipment required for contactor operation are discussed. These include interface control, phase disentrainment, pulsing and sampling equipment.

Examples are given of the point score method of contactor selection for typical process applications.


Volume SE VI   Part 3 Mathematical methods for liquid-liquid extractors.

This report is concerned with the use of models for developing realistic and useful design equations for column contactors. The purpose of these models is to provide more realistic representation of column performance, particularly with regard to residence time distribution characteristics, than is obtained from calculations based on the plug-flow assumption. Plug-flow calculations do however, provide a simple introduction to considerations of equilibrium, mass transfer and mass balances used in the formulation of design equations. More realistic models which take account of the non-plug-flow behaviour are needed in mass transfer calculations for the design and scale-up of industrial columns, and for the interpretation of data from pilot-plant or laboratory columns. The residence time distribution characteristics of column contactors, often termed "axial mixing", are usually described by one of two types of model; differential and stage-wise. The concepts of differential or stage wise contact used in the formulation of these models have the same basis as those used in simple calculations of mass transfer, and the characteristics of the models and their relationship to one another are described. The analysis of concentration profiles and procedures for multicomponent systems are reviewed and an assessment given of the practical considerations which influence the success or otherwise of design procedures.


Volume SE VI   Part 4 Scale-up of liquid-liquid extraction equipment.

Methods for classifying industrial-type contactors are given and the factors which determine the performance of column contactors and mixer-settlers are discussed. The need to exercise caution in applying empirical correlations, determined with small-scale apparatus and pure solutions, to the design of large-scale equipment is stressed. The performance characteristics, in terms of mass transfer and hydrodynamics of unagitated, pulsed and mechanically-agitated columns are discussed. Dispersed phase hold-up, flooding, mass transfer, capacity and axial mixing are taken into account. A short description of the few centrifugal-type contactors available is given. Scale-up of mixer-settlers is described and the major design parameters, power input, drop size, rate of mass transfer, settler area and settler shape, are discussed. The importance of entrainment from the mixer and the settler in mixer-settler design is also discussed.


Volume SE VI   Part 5 Design of column contactors for liquid-liquid extraction.

This part sets out a general method for the design of liquid-liquid extraction column contactors, but with particular emphasis on randomly packed columns, pulsed sieve plate rotating disc and Kuhni columns. The design method is largely based upon experimental data obtained from the SPS liquid-liquid extraction research programme. The design method begins with the measurement of physical properties and the calculation of the number of transfer units. This is followed by hydrodynamic calculations in which the flooding point and hence required diameter of the column is derived from considerations of drop size and the velocity/dispersed phase hold-up relationship. The rate of mass transfer under plug flow conditions is corrected by axial mixing calculations to give a realistic column height. Other items included are the mechanical design of end sections, feed distributors, agitation equipment and safety aspects.


Volume SE VI   Part 6 Integral box mixer-settlers for solvent extraction processes.

Mixer-settlers find frequent application in liquid-liquid extraction processes for the separation and purification of materials, particularly metals, because they provide good contacting between the phases. They are usually simple to construct, low in capital cost and generally require little maintenance. The integral box design is particularly reliable, being compact without inter-stage piping and is ideally suited to small and medium-scale operation. This report gives a systematic procedure for the design of the integral box mixer-settler. An overall design guide is described together with a design decision diagram.

This is followed by a description of the measurement of physical properties, and equilibrium and kinetic data; the need to use real process fluids is stressed. As part of the design procedure it may be necessary to carry out continuous flow tests at either laboratory or pilot scale, and guidance is given as to how best to undertake these tests. The operational characteristics of the integral box mixer-settler are described, and techniques for improving the performance of existing equipment discussed. Sample calculations illustrating each part of the design procedure are given in appendices.


Volume SE VI   Part 7 The design of pump-mix mixer-settlers.

Stagewise contactors such as the mixer-settler provide a particularly simple means of achieving countercurrent liquid-liquid extraction, since the residence time in the mixing stages, for example, for slow mass transfer operations, is well characterised. The pump-mix type is especially suitable for very large-scale operations such as copper from leach liquors, due to its reduced pumping costs and depth of the equipment. The principles of operation of the pump-mix mixer-settler are explained and the many different types reported in the literature are described. The important aspects of impeller performance are discussed; in addition to providing the mixing and pumping requirements the impeller determines the drop size distribution and phase inversion characteristics. Some settler designs are described and aspects of settler performance together with dispersion band characteristics discussed. A design summary with a design decision flow diagram, is provided. Methods are described for the measurement of basic physical properties, and equilibrium and kinetic data. Procedures for pilot plant design and interpretation, leading to final settler design are recommended. A discussion of plant operational characteristics is given and a complete sample calculation is included.


Volume SE VI   Part 8 Design of simple gravity settlers for the coalescence of liquid-liquid dispersions.

The proper design of simple settlers in which liquid-liquid dispersions segregate under the influence of gravity is important in optimising the dimensions of mixer-settler equipment and the disengaging zones of column contactors.

Many settlers are, however, almost certainly oversized for their duty due to the difficulties inherent in predicting settler behaviour. This report gives a systematic design procedure for settlers, based on recent theoretical and experimental work at ETH Zurich and at AEA Technology, Harwell, whereby the continuous-flow disengagement performance of a settler is predicted from batch disengagement data obtained in the laboratory. The state of the art in the theory of liquid-liquid coalescence is reviewed; the contributory mechanisms in liquid-liquid disengagement of settling (sedimentation), interdrop coalescence and interfacial coalescence are introduced. A design guide including a decision flow diagram is given. This is followed by suggested techniques for the conduct and interpretation of batch settling tests, leading to an operating settling velocity. From this the complete design of the settler is elaborated, including feed and outlet port calculations. Concluding chapters consider the retrofitting of existing settlers, operational and safety considerations. Complete worked examples of settler calculation are given.


Volume SE VI   Part 9 Design of tank reactors for the processing of dispersed liquid systems.

Liquid-liquid reaction systems are a class of chemical reaction processes of significant importance in the chemical, petroleum, mining, food and pharmaceutical industries. This report develops a rational design and scale-up procedure for the equipment needed for these reaction processes. Agitator types are described and methods given for selecting the most appropriate one for a particular process. The advantages and disadvantages of batch and continuous stirred tank reactors are fully discussed. Correlations are recommended for estimating the power consumption and the minimum agitator speed needed to maintain a uniform dispersion. The factors which determine drop size distribution and correlations for predicting the mean drop size in agitated tanks are discussed. Also described are the methods and parameters which can be applied to characterise the residence time and residence time distribution in homogeneous tank reactors. The various tank reactor configurations which can be used are described together with requirements for operating at elevated temperatures and pressures. The different types or flow pattern which are produced by the wide range of agitators available are described, including vortex formation and suppression. To assist the designer a flow chart is given for the steps to be followed in arriving at a tank reactor design for a given duty together with a worked example.


Volume SE VI   Part 10 In-line mixers and their scale-up.

In-line mixers are much used in process engineering solvent extraction practice. This manual part is concerned with all types of mixer used in low-residence time in-line applications, not just strictly static designs, where the nature of the pipe flow within, upstream and downstream of the mixing element has a significant bearing on mixing quality. The emphasis is upon design and scale-up methods, and comparisons are made with agitated tank mixers.

The manual part first discusses available types of in-line mixer, and introduces performance characteristics for the turbulent mixing of low-viscosity fluids. Subsequent sections cover the issues of energy requirements, mechanisms for creating a dispersion, phase stability and ambivalence, and drop size prediction. Methods for rate calculation are then described, covering both kinetically slow and rapid reactions.

Finally, the rather sparse information on scale-up methods is reviewed and a recommended scale-up strategy proposed.