Contents

Preface

Acknowledgments

About the Author

Nomenclature

Chapter 1 Introduction to Separation Process Engineering

1.0. Summary—Objectives

1.1. Importance of Separations

1.2. Concept of Equilibrium

1.3. Mass Transfer Concepts

1.4. Problem-Solving Methods

1.5. Units

1.6. Computers and Computer Simulations

1.7. Prerequisite Material

1.8. Other Resources on Separation Process Engineering

References

Homework

Chapter 2 Flash Distillation

2.0. Summary—Objectives

2.1. Basic Method of Flash Distillation

2.2. Form and Sources of Equilibrium Data

2.3. Graphical Representation of Binary VLE

2.4. Binary Flash Distillation

2.4.1. Sequential Solution Procedure

Example 2-1. Flash separator for ethanol and water

2.4.2. Simultaneous Solution Procedure

2.4.3. Simultaneous Solution and Enthalpy-Composition Diagram

2.5. Multicomponent VLE

2.6. Multicomponent Flash Distillation

Example 2-2. Multicomponent flash distillation

2.7. Simultaneous Multicomponent Convergence

Example 2-3. Simultaneous solution for flash distillation

2.8. Three-Phase Flash Calculations

2.9. Size Calculation

Example 2-4. Calculation of drum size

2.10. Using Existing Flash Drums

References

Homework

Appendix A. Computer Simulation of Flash Distillation

Appendix B. Spreadsheets for Flash Distillation

2.B.1. Binary Flash Distillation with Excel

2.B.2. Multicomponent Flash Distillation with Excel

Chapter 3 Introduction to Column Distillation

3.0. Summary—Objectives

3.1. Developing a Distillation Cascade

3.2. Distillation Equipment

3.3. Specifications

3.4. External Column Balances

Example 3-1. External balances for binary distillation

References

Homework

Chapter 4 Binary Column Distillation: Internal Stage-by-Stage Balances

4.0. Summary—Objectives

4.1. Internal Balances

4.2. Binary Stage-by-Stage Solution Methods

Example 4-1. Stage-by-stage calculations by the Lewis method

4.3. Introduction to the McCabe-Thiele Method

4.4. Feed Line

Example 4-2. Feed line calculations

4.5. Complete McCabe-Thiele Method

Example 4-3. McCabe-Thiele method

4.6. Profiles for Binary Distillation

4.7. Open Steam Heating

Example 4-4. McCabe-Thiele analysis of open steam heating

4.8. General McCabe-Thiele Analysis Procedure

Example 4-5. Distillation with two feeds

4.9. Other Distillation Column Situations

4.9.1. Partial Condensers

4.9.2. Total Reboilers

4.9.3. Side Streams or Withdrawal Lines

4.9.4. Intermediate Reboilers and Intermediate Condensers

4.9.5. Stripping and Enriching Columns

4.10. Limiting Operating Conditions

4.11. Efficiencies

4.12. Simulation Problems

4.13. New Uses for Old Columns

4.14. Subcooled Reflux and Superheated Boilup

4.15. Comparisons Between Analytical and Graphical Methods

References

Homework

Appendix A. Computer Simulation of Binary Distillation

Appendix B. Spreadsheets for Binary Distillation

Chapter 5 Introduction to Multicomponent Distillation

5.0. Summary—Objectives

5.1. Calculational Difficulties

Example 5-1. External mass balances using fractional recoveries

5.2. Profiles for Multicomponent Distillation

5.3. Stage-by-Stage Calculations for CMO

Example 5-2. Bubble-point calculation

References

Homework

Appendix A. Simplified Spreadsheet for Stage-by-Stage Calculations for Ternary Distillation

Example 5-3. Stage-by-stage calculations for stripping column

Appendix B. Automated Spreadsheet with VBA for Stage-by-Stage Calculations for Ternary Distillation

Chapter 6 Exact Calculation Procedures for Multicomponent Distillation

6.0. Summary—Objectives

6.1. Introduction to Matrix Solution for Multicomponent Distillation

6.2. Component Mass Balances in Matrix Form

6.3. Initial Guesses for Flow Rates and Temperatures

6.4. Temperature Convergence

Example 6-1. Matrix and bubble-point calculations

6.5. Energy Balances in Matrix Form

6.6. Introduction to Naphtali-Sandholm Simultaneous Convergence Method

6.7. Discussion

References

Homework

Appendix. Computer Simulations for Multicomponent Column Distillation

Chapter 7 Approximate Shortcut Methods for Multicomponent Distillation

7.0. Summary—Objectives

7.1. Total Reflux: Fenske Equation

Example 7-1. Fenske equation

7.2. Minimum Reflux: Underwood Equations

Example 7-2. Underwood equations

7.3. Gilliland Correlation for Number of Stages at Finite Reflux Ratios

Example 7-3. Gilliland correlation

References

Homework

Chapter 8 Introduction to Complex Distillation Methods

8.0. Summary—Objectives

8.1. Breaking Azeotropes with Other Separators

8.2. Binary Heterogeneous Azeotropic Distillation Processes

8.2.1. Binary Heterogeneous Azeotropes—Single-Column System

8.2.2. Binary Heterogeneous Azeotropes—Two-Column System

8.2.3. Drying Organic Compounds That Are Partially Miscible with Water

Example 8-1. Drying benzene by distillation

8.3. Steam Distillation

Example 8-2. Steam distillation

8.4. Pressure-Swing Distillation Processes

8.5. Complex Ternary Distillation Systems

8.5.1. Distillation Curves

8.5.2. Residue Curves

Example 8-3. Development of distillation and residue curves for constant relative volatility

8.6. Extractive Distillation

8.7. Azeotropic Distillation with Added Solvent

8.8. Distillation with Chemical Reaction

References

Homework

Appendix A. Simulation of Complex Distillation Systems

Appendix B. Spreadsheet for Residue Curve Generation

Chapter 9 Batch Distillation

9.0. Summary—Objectives

9.1. Introduction to Batch Distillation

9.2. Batch Distillation: Rayleigh Equation

9.2.1. Mixed Distillate Product

9.2.2. Distillate Product Fractions

9.3. Simple Binary Batch Distillation

Example 9-1. Simple binary Rayleigh distillation

9.4. Constant-Mole Batch Distillation

9.5. Batch Steam Distillation

9.6. Multistage Binary Batch Distillation

9.6.1. Constant Reflux Ratio

Example 9-2. Multistage batch distillation

9.6.2. Variable Reflux Ratio

9.7. Multicomponent Simple Batch Distillation

Example 9-3. Multicomponent simple batch distillation

9.8. Operating Time

References

Homework

Appendix A. Spreadsheet for Simple Multicomponent Batch Distillation, Constant Relative Volatility

Chapter 10 Staged and Packed Column Design

10.0. Summary—Objectives

10.1. Staged Column Equipment Description

10.1.1. Trays, Downcomers, and Weirs

10.1.2. Inlets and Outlets

10.2. Tray Efficiencies

Example 10-1. Overall efficiency estimation

10.3. Column Diameter Calculations

Example 10-2. Diameter calculation for tray column

10.4. Balancing Calculated Diameters

10.5. Sieve Tray Layout and Tray Hydraulics

Example 10-3. Tray layout and hydraulics

10.6. Valve Tray Design

10.7. Introduction to Packed Column Design

10.8. Packings and Packed Column Internals

10.9. Height of Packing: HETP Method

10.10. Packed Column Flooding and Diameter Calculation

Example 10-4. Packed column diameter calculation

10.11. Economic Trade-Offs for Packed Columns

10.12. Choice of Column Type

References

Homework

Appendix. Tray and Downcomer Design with Computer Simulator

Chapter 11 Economics and Energy Conservation in Distillation

11.0. Summary—Objectives

11.1. Equipment Costs

11.2. Basic Heat Exchanger Design

11.3. Design and Operating Effects on Costs

Example 11-1. Cost estimate for distillation

11.4. Changes in Plant Operating Rates

11.5. Energy Conservation in Distillation

11.6. Synthesis of Column Sequences for Almost Ideal Multicomponent Distillation

Example 11-2. Sequencing columns with heuristics

11.7. Synthesis of Distillation Systems for Nonideal Ternary Systems

Example 11-3. Process development for separation of complex ternary mixture

References

Homework

Chapter 12 Absorption and Stripping

12.0. Summary—Objectives

12.1. Absorption and Stripping Equilibria

12.2. McCabe-Thiele Solution for Dilute Absorption

Example 12-1. McCabe-Thiele analysis for dilute absorber

12.3. Stripping Analysis for Dilute Systems

12.4. Analytical Solution for Dilute Systems: Kremser Equation

Example 12-2. Stripping analysis with the Kremser equation

12.5. Efficiencies

12.6. McCabe-Thiele Analysis for More Concentrated Systems

Example 12-3. Graphical analysis for more concentrated absorber

12.7. Column Diameter

12.8. Dilute Multisolute Absorbers and Strippers

12.9. Matrix Solution for Concentrated Absorbers and Strippers

12.10. Irreversible Absorption and Cocurrent Cascades

References

Homework

Appendix. Computer simulations of absorption and stripping

Chapter 13 Liquid-Liquid Extraction

13.0. Summary—Objectives

13.1. Extraction Processes and Equipment

13.2. Dilute, Immiscible, Countercurrent Extraction

13.2.1. McCabe-Thiele Method for Dilute Systems

Example 13-1. Dilute countercurrent immiscible extraction

13.2.2. Kremser Method for Dilute Systems

13.3. Dilute Fractional Extraction

13.4. Immiscible Single-Stage and Cross-Flow Extraction

Example 13-2. Single-stage and cross-flow extraction of protein

13.5. Concentrated Immiscible Extraction

Example 13-3. Concentrated immiscible extraction

13.6. Immiscible Batch Extraction

13.7. Extraction Equilibrium for Partially Miscible Ternary Systems

13.8. Mixing Calculations and the Lever-Arm Rule

13.9. Partially Miscible Single-Stage and Cross-Flow Systems

Example 13-4. Partially miscible single-stage extraction

13.10. Countercurrent Extraction Cascades for Partially Miscible Systems

13.10.1. External Mass Balances

13.10.2. Difference Points and Stage-by-Stage Calculations

13.10.3. Complete Partially Miscible Extraction Problem

Example 13-5. Countercurrent extraction

13.11. Relationship Between McCabe-Thiele and Triangular Diagrams for Partially Miscible Systems

13.12. Minimum Solvent Rate for Partially Miscible Systems

13.13. Extraction Computer Simulations

13.14. Design of Mixer-Settlers

13.14.1. Mixer Design

13.14.2. Settler (Decanter) Design

Example 13-6. Mixer-settler design

References

Homework

Appendix. Computer Simulation of Extraction

Chapter 14 Washing, Leaching, and Supercritical Extraction

14.0. Summary—Objectives

14.1. Generalized McCabe-Thiele and Kremser Procedures

14.2. Washing

Example 14-1. Washing

14.3. Leaching with Constant Flow Rates

14.4. Leaching with Variable Flow Rates

Example 14-2. Leaching calculations

14.5. Introduction to Supercritical Fluid Extraction

14.6. Application of McCabe-Thiele and Kremser Methods to Other Separations

References

Homework

Chapter 15 Introduction to Diffusion and Mass Transfer

15.0. Summary–Objectives

15.1. Molecular Movement Leads to Mass Transfer

15.2. Fickian Model of Diffusivity

15.2.1. Fick’s Law and the Fickian Definition of Diffusivity

15.2.2. Steady-State Binary Fickian Diffusion and Mass Balances without Convection

Example 15-1. Determination of diffusivity in dilute binary mixture

Example 15-2. Steady-state diffusion without convection: Low-temperature evaporation

15.2.3. Unsteady Binary Fickian Diffusion with No Convection (Optional)

15.2.4. Steady-State Binary Fickian Diffusion and Mass Balances with Convection

Example 15-3. Steady-state diffusion with convection: High-temperature evaporation

15.3. Values and Correlations for Fickian Binary Diffusivities

15.3.1. Fickian Binary Gas Diffusivities

Example 15-4. Estimation of temperature effect on Fickian gas diffusivity

15.3.2. Fickian Binary Liquid Diffusivities

15.3.3. Numerical Solution with Variable Binary Diffusivity

Example 15-5. Numerical solution for variable diffusivity and molar concentration

15.4. Linear Driving-Force Model of Mass Transfer for Binary Systems

15.4.1. Film Theory for Dilute and Equimolar Transfer Systems

15.4.2. Transfer through Stagnant Films: Absorbers and Strippers

15.4.3. Binary Mass Transfer to Expanding or Contracting Objects

Example 15-6. Shrinking diameter of oxygen bubble

Example 15-7. Dissolution of solid particle

15.5. Correlations for Mass Transfer Coefficients

15.5.1. Dimensionless Groups

15.5.2. Theoretically Derived Mass Transfer Correlations

15.5.3. Semi-Empirical and Empirical Mass Transfer Coefficient Correlations

Example 15-8. Estimation of mass transfer coefficients

15.5.4. Correlations Based on Analogies

15.6. Difficulties with Fickian Diffusion Model

15.7. Maxwell-Stefan Model of Diffusion and Mass Transfer

15.7.1. Introductory Development of the Maxwell-Stefan Theory of Diffusion

15.7.2. Maxwell-Stefan Equations for Binary Nonideal Systems

15.7.3. Determining Independent Fluxes Nj,z

15.7.4. Maxwell-Stefan Difference Equation Formulations

15.7.5. Relationship between Maxwell-Stefan and Fickian Diffusivities

Example 15-9. Maxwell-Stefan nonideal binary diffusion

15.7.6. Ideal Ternary Systems

Example 15-10. Maxwell-Stefan ideal ternary system

15.7.7. Ternary Mass Transfer to Expanding or Contracting Objects

Example 15-11. Ternary transfer from an evaporating drop

15.7.8. Nonideal Ternary Systems

15.8. Advantages and Disadvantages of Different Diffusion and Mass Transfer Models

References

Homework

Appendix. Spreadsheets Examples 15-10 and 15-11

Chapter 16 Mass Transfer Analysis for Distillation, Absorption, Stripping, and Extraction

16.0. Summary—Objectives

16.1. HTU-NTU Analysis of Packed Distillation Columns

Example 16-1. Distillation in a packed column

16.2. Relationship of HETP and HTU

16.3. Mass Transfer Correlations for Packed Towers

16.3.1. Bolles and Fair Correlation for Random Packings

Example 16-2. Estimation of HG and HL

16.3.2. Simple Correlations for Random Packings

16.4. HTU-NTU Analysis of Concentrated Absorbers and Strippers

Example 16-3. Absorption of SO2

16.5. HTU-NTU Analysis of Cocurrent Absorbers

16.6. Prediction of Distillation Tray Efficiency

Example 16-4. Estimation of distillation stage efficiency

16.7. Mass Transfer Analysis of Extraction

16.7.1. Extraction Mass Transfer Equations and HTU-NTU Analysis

16.7.2. Calculation of Stage Efficiency in Extraction Mixers

Example 16-5. Conversion of mass transfer coefficients and estimation of mixer stage efficiency

16.7.3. Drop Size in Mixers

16.7.4. Mass Transfer Coefficients in Mixers

16.7.4.1. Mixer Mass Transfer Coefficients for Individual Drops (Optional)

16.7.4.2. Mass Transfer Coefficients for Drop Swarms in Mixers

16.7.4.3. Conservative Estimation of Mass Transfer Coefficients for Extraction

16.8. Rate-Based Analysis of Distillation

References

Homework

Appendix. Computer Rate-Based Simulation of Distillation

Chapter 17 Crystallization from Solution

17.0. Summary–Objectives

17.1. Basic Principles of Crystallization from Solution

17.1.1. Crystallization Process

17.1.2. Binary Equilibrium and Crystallizer Types

17.2. Continuous Cooling Crystallizers

17.2.1. Equilibrium and Mass Balances for Single Solute Producing Pure Solute Crystals

Example 17-1. Continuous cooling crystallizer mass balances without hydrates

Example 17-2. Continuous cooling crystallizer mass balances for hydrates

Example 17-3. Mixing solutions when hydrates are dissolved in water

17.2.2. Eutectic Systems

Example 17-4. Eutectic equilibrium and mass balances

17.3. Evaporative and Vacuum Crystallizers

17.3.1. Equipment

17.3.2. Analysis of Evaporative Crystallizers for Single-Solute Systems Producing Pure Solute Crystals

Example 17-5. Evaporative crystallizer without hydrate

Example 17-6. Evaporative crystallizer with hydrate

17.3.3. Simultaneous Mass, Energy, and Equilibrium Calculations

Example 17-7. Vacuum crystallizer: Simultaneous mass, energy, and equilibrium calculations

17.4. Sieve Analysis

Example 17-8. Screen analysis of crystallization data

17.5. Introduction to Population Balances

17.6. Crystal Size Distributions for MSMPR Crystallizers

17.6.1. Crystal Nucleation and Growth

17.6.2. Development of MSMPR Equation and Determination of G and n° from Experiment

Example 17-9. Determination of kinetic parameters from screen analysis data

17.6.3. Development and Application of Distributions for MSMPR Crystallizers

Example 17-10. Use of differential mass distribution to analyze screen analysis data

Example 17-11. Prediction of sieve analysis

Example 17-12. Combination of equilibrium and MSMPR distribution

17.7. Seeding

17.7.1. CSD Analysis for Growth on Seeds in Continuous Crystallizers

Example 17-13. CSD of seeded crystallizer

17.7.2. Controlling Crystal Size by Seeding

Example 17-14. Increasing crystal size with seeding

17.8. Batch and Semibatch Crystallization

17.8.1. Temperature Control for Batch Cooling Crystallizers

17.8.2. Antisolvent Crystallization

Example 17-15. Antisolvent crystallization

17.9. Precipitation

17.9.1. Precipitation by Antisolvent Addition

17.9.2. Precipitation by Salting Out

Example 17-16. Salting out with a common ion

References

Homework

Appendix. Spreadsheets

Chapter 18 Introduction to Membrane Separation Processes

18.0. Summary—Objectives

18.1. Membrane Separation Equipment

18.2. Membrane Concepts

18.3. Gas Permeation

18.3.1. Gas Permeation of Binary Mixtures

18.3.2. Binary Permeation in Perfectly Mixed Systems

Example 18-1. Well-mixed gas permeation—sequential, analytical solution

Example 18-2. Well-mixed gas permeation—simultaneous solutions

18.3.3. Multicomponent Permeation in Perfectly Mixed Systems

Example 18-3. Multicomponent, perfectly mixed gas permeation

18.3.4. Effect of Holes in Membrane

Example 18-4. Effect of holes

18.4. Reverse Osmosis (RO)

18.4.1. Analysis of Osmosis

18.4.2. Analysis of Reverse Osmosis

18.4.3. RO in Well-Mixed Modules

Example 18-5. Determination of RO membrane properties

Example 18-6. RO without concentration polarization

18.4.4. Mass Transfer Analysis of Concentration Polarization

Example 18-7. RO with concentration polarization

Example 18-8. Prediction of RO performance with concentration polarization

18.5. Ultrafiltration (UF)

Example 18-9. UF with gel formation

18.6. Pervaporation (Pervap)

18.6.1. Pervap Basics

18.6.2. Pervap Design Using Experimental Data

Example 18-10. Pervaporation—feasibility calculation

18.6.3. Theoretical Design of Pervap Systems

Example 18-11. Analysis of pervap data

18.7. Bulk Flow Pattern Effects

Example 18-12. Flow pattern effects in gas permeation

18.7.1. Binary Crossflow Permeation

18.7.2. Binary Cocurrent and Countercurrent Permeation

References

Homework

Appendix. Spreadsheet for Crossflow Gas Permeation

Chapter 19 Introduction to Adsorption, Chromatography, and Ion Exchange

19.0. Summary—Objectives

19.1. Sorbents and Sorption Equilibrium

19.1.1. Definitions

19.1.2. Sorbent Types

19.1.3. Adsorption Equilibrium Behavior

Example 19-1. Adsorption equilibrium

19.2. Solute Movement Analysis for Linear Systems: Basics and Applications to Chromatography

19.2.1. Movement of Solute in a Column

19.2.2. Solute Movement Theory for Linear Isotherms

19.2.3. Application of Linear Solute Movement Theory to Purge Cycles and Elution Chromatography

Example 19-2. Linear solute movement analysis of elution chromatography

19.3. Solute Movement Analysis for Linear Systems: Temperature and Pressure Swing Adsorption and Simulated Moving Beds

19.3.1. Temperature Swing Adsorption

Example 19-3. Thermal regeneration with linear isotherm

19.3.2. Pressure Swing Adsorption

Example 19-4. PSA system

19.3.3. Simulated Moving Beds

Example 19-5. SMB system

19.4. Nonlinear Solute Movement Analysis

19.4.1. Diffuse Waves

Example 19-6. Diffuse wave

19.4.2. Shock Waves

Example 19-7. Self-sharpening shock wave

19.5. Ion Exchange

19.5.1. Ion Exchange Equilibrium

19.5.2. Movement of Ions

Example 19-8. Ion movement for divalent-monovalent exchange

19.6. Mass and Energy Transfer in Packed Beds

19.6.1. Mass Transfer and Diffusion

19.6.2. Column Mass Balances

19.6.3. Lumped Parameter Mass Transfer

19.6.4. Energy Balances and Heat Transfer

19.6.5. Derivation of Solute Movement Theory

19.6.6. Detailed Simulators

19.7. Mass Transfer Solutions for Linear Systems

19.7.1. Lapidus and Amundson Solution for Local Equilibrium with Dispersion

19.7.2. Superposition in Linear Systems

Example 19-9. Lapidus and Amundson solution for elution

19.7.3. Linear Chromatography

Example 19-10. Determination of linear isotherm parameters, N, and resolution for linear chromatography

19.8. LUB Approach for Nonlinear Sorption Systems

Example 19-11. LUB approach

19.9. Checklist for Practical Design and Operation

References

Homework

Appendix. Aspen Chromatography Simulator

Appendix A Aspen Plus Troubleshooting Guide for Separations

Appendix B Instructions for Fitting VLE and LLE Data with Aspen Plus

Appendix C Unit Conversions and Physical Constants

Appendix D Data Locations

Answers to Selected Problems

Index

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