Distillation E-Book

Johann G. Stichlmair

• Herausgeber: John Wiley & Sons
• Kategorie: Fachliteratur
• Sprache: Englisch

Seitenzahl: 861

Veröffentlichungsjahr: 2021

Beschreibung

Distillation Principles and Practice Second Edition covers all the main aspects of distillation including the thermodynamics of vapor/liquid equilibrium, the principles of distillation, the synthesis of distillation processes, the design of the equipment, and the control of process operation. Most textbooks deal in detail with the principles and laws of distilling binary mixtures. When it comes to multi-component mixtures, they refer to computer software nowadays available. One of the special features of the second edition is a clear and easy understandable presentation of the principles and laws of ternary distillation. The right understanding of ternary distillation is the link to a better understanding of multi-component distillation. Ternary distillation is the basis for a conceptual process design, for separating azeotropic mixtures by using an entrainer, and for reactive distillation, which is a rapidly developing field of distillation. Another special feature of the book is the design of distillation equipment, i.e. tray columns and packed columns. In practice, empirical know-how is preferably used in many companies, often in form of empirical equations, which are not even dimensionally correct. The objective of the proposed book is the derivation of the relevant equations for column design based on first principles. The field of column design is permanently developing with respect to the type of equipment used and the know-how of two-phase flow and interfacial mass transfer.

Leseprobe

Table of Contents

Cover

DISTILLATION

Copyright

Preface

Nomenclature

Latin Symbols

Greek Symbols

Subscripts

Superscripts

Abbreviations

Dimensionless Numbers

1 Introduction

1.1 Principle of Distillation Separation

1.2 Historical

References

2 Vapor–Liquid Equilibrium

2.1 Basic Thermodynamic Correlations

2.2 Calculation of Vapor–Liquid Equilibrium in Mixtures

2.3 Binary Mixtures and Phase Diagrams

2.4 Ternary Mixtures

References

Notes

3 Single‐Stage Distillation and Condensation

3.1 Continuous Closed Distillation and Condensation

3.2 Batchwise Open Distillation and Open Condensation

3.3 Semi‐continuous Single‐Stage Distillation

References

4 Multistage Continuous Distillation (Rectification)

4.1 Principles

4.2 Multistage Distillation of Binary Mixtures

4.3 Multistage Distillation of Ternary Mixtures

4.4 Multistage Distillation of Multicomponent Mixtures

References

5 Reactive Distillation, Catalytic Distillation

5.1 Fundamentals

5.2 Topology of Reactive Distillation Lines

5.3 Topology of Reactive Distillation Processes

5.4 Arrangement of Catalysts in Columns

References

6 Multistage Batch Distillation

6.1 Batch Distillation of Binary Mixtures

6.2 Batch Distillation of Ternary Mixtures

6.3 Batch Distillation of Multicomponent Mixtures

6.4 Influence of Column Liquid Hold‐up on Batch Distillation

6.5 Processes for Separating Zeotropic Mixtures by Batch Distillation

6.6 Processes for Separating Azeotropic Mixtures by Batch Distillation

References

7 Energy Economization in Distillation

7.1 Energy Requirement of Single Columns

7.2 Optimal Separation Sequences of Ternary Distillation

7.3 Modifications of the Basic Processes

7.4 Design of Heat Exchanger Networks

References

8 Industrial Distillation Processes

8.1 Constraints for Industrial Distillation Processes

8.2 Fractionation of Binary Mixtures

8.3 Fractionation of Multicomponent Zeotropic Mixtures

8.4 Fractionation of Heterogeneous Azeotropic Mixtures

8.5 Fractionation of Azeotropic Mixtures by Pressure Swing Processes

8.6 Fractionation of Azeotropic Mixtures by Addition of an Entrainer

8.7 Industrial Processes of Reactive Distillation

References

9 Design of Mass Transfer Equipment

9.1 Types of Design

9.2 Design of Tray Columns

9.3 Design of Packed Columns

Appendix

References

10 Control of Distillation Processes

10.1 Control Loops

10.2 Single Control Tasks for Distillation Columns

10.3 Basic Control Configurations of Distillation Columns

10.4 Application Ranges of the Basic Control Configurations

10.5 Examples for Control Configurations of Distillation Processes

10.6 Control Configurations for Batch Distillation Processes

References

Notes

Index

End User License Agreement

List of Tables

Chapter 2

Table 2.1 Boiling temperatures at

and parameters

,

, and

for selected co...

Table 2.2 Correlations for molar excess free energy 

and activity coefficien...

Table 2.3 Calculation of boiling and condensation pressure 

and temperature 

Chapter 3

Table 3.1 Carbon dioxide outburst at Lake Nyos, Cameroon, on 21 August 1986.

Chapter 4

Table 4.1 Dependency of the energy requirement of ternary distillation on fee...

Table 4.2 Partial derivatives of material, equilibrium, and enthalpy function...

Chapter 5

Table 5.1 Selected systems for reactive distillation after

DOHERTY AND BUZAD

1...

Chapter 7

Table 7.1 Classification of processes for sharp separation of ideal ternary m...

Table 7.2 Listing of temperature levels and enthalpies of five streams.

Table 7.3 Heat duties and mean logarithmic temperature differences of the opt...

Chapter 8

Table 8.1 Maximum allowable operating temperatures of distillation columns to...

Table 8.2 Maximum product side temperatures and relative costs of some heatin...

Table 8.3 Minimum product side temperatures and relative costs of some coolin...

Table 8.4 Key components for distillation processes of industrial importance ...

Table 8.5 Examples of binary systems processed by distillation and decantatio...

Table 8.6 Examples of systems fractionated by pressure swing processes (Figur...

Table 8.7 Criteria for entrainer selection for processes without distillation...

Table 8.8 Criteria for entrainer selection for processes with distillation bo...

Table 8.9 Examples of systems fractionated by combination of distillation and...

Table 8.10 Examples of systems fractionated by extractive distillation (see p...

Table 8.11 Selected systems for reactive distillation after

DOHERTY AND BUZAD

...

Chapter 9

Table 9.1 Standard geometrical parameters of trays.

Table 9.2 Correlations for the gas capacity factor 

.

Table 9.3 Listing of some correlations for the relative liquid content 

in t...

Table 9.4 Listing of some correlations for the froth height

.

Table 9.5 Liquid entrainment data plotted in Figure 9.17.

Table 9.6 Typical values of specific surface area 

and porosity 

depending ...

Table 9.7 Typical values of volumetric surface

and porosity

for several st...

Table 9.8 Correlations for the liquid hold‐up below the loading point.

Table 9.9 Values of the factor

and the exponent

of correlation Eq. (9.79)....

Table 9.10 Exponents used in correlations for the effective interfacial area 

Table 9.11 Exponents used in correlations for the gas‐side mass transfer coef...

Table 9.12 Exponents used in correlations for the liquid‐side mass transfer c...

Table 9.13 Values of critical surface tension 

of the

ONDA ET AL.

1968 corre...

Table 9.14 Selected values of the factors 

and

of the

BILLET AND SCHULTES

...

Chapter 10

Table 10.1 Letter code for identification of control instrument functions acc...

Table 10.2 Check of flow control configurations for consistency with split Ru...

Table 10.3 Summary of application ranges of control configurations.

List of Illustrations

Chapter 1

Figure 1.1 General principle of fractionation in thermal separation technolo...

Figure 1.2 Distillation and rectification equipment taken from

The Alchemy o

...

Chapter 2

Figure 2.1 Equilibrium in a mixture at isobaric–isothermal condition

with ...

Figure 2.2 Graphical determination of the activity coefficients

and

from...

Figure 2.3 VLE data for the binary acetone/methanol mixture. Antoine equatio...

Figure 2.4

‐diagrams and activity coefficients of binary mixtures with low ...

Figure 2.5 Phase diagrams of seven binary mixtures; top row:

‐diagrams at

Figure 2.6

‐diagram of the water/n‐butanol mixture: boiling and condensatio...

Figure 2.7 Saturation vapor pressure curves of the generic components 

(low...

Figure 2.8 Phase diagrams for three limiting cases; left: complete miscibili...

Figure 2.9 Boiling surfaces of eight different ternary mixtures at

as a fu...

Figure 2.10 Boiling and condensation surface of the acetone/chloroform/metha...

Figure 2.11 Distillation lines of the eight ternary mixtures from Figure 2.9...

Figure 2.11 Distillation lines of the eight ternary mixtures from Figure 2.9...

Figure 2.11 Distillation lines of the eight ternary mixtures from Figure 2.9...

Figure 2.11 Distillation lines of the eight ternary mixtures from Figure 2.9...

Chapter 3

Figure 3.1 Modes of single‐stage distillation.

Figure 3.2 Modes of single‐stage partial condensation.

Figure 3.3 Continuous closed distillation. The binary feed 

is split into t...

Figure 3.4 Dew point and boiling point lines of the mixture propane/isobutan...

Figure 3.5 Schematic of closed distillation of a multicomponent liquid mixtu...

Figure 3.6 Latent heat of vaporization of selected compounds.

 = normal boi...

Figure 3.7 Schematic of an adiabatic flash. Some vapor is generated by expan...

Figure 3.8 Carbon dioxide outburst at Lake Nyos on 21 August 1986.

Figure 3.9 Schematic of batch distillation. Generally, the distillate is col...

Figure 3.10 Batch distillation of an ideal binary mixture calculated with

....

Figure 3.11 Batch distillation of an ideal ternary mixture (calculated with ...

Figure 3.12 Batch distillation of an ideal ternary mixture (calculated with ...

Figure 3.13 Liquid residue curves of the octane/2‐ethoxyethanol/ethylbenzene...

Figure 3.14 Open condensation of a ternary mixture. The dotted bold line des...

Figure 3.15 Vapor residue curves of the octane/2‐ethoxyethanol/ethylbenzene ...

Figure 3.16 Comparison of the courses of liquid residue curves (

), vapor re...

Figure 3.17 Open distillation of an ideal quaternary mixture (calculated wit...

Figure 3.18 Open condensation of an ideal quaternary mixture (calculated wit...

Figure 3.19 Schematic of a semi‐continuous batch distillation. High boiling ...

Chapter 4

Figure 4.1 Multiple distillation of a binary mixture 

. A) Flow diagram. B) ...

Figure 4.2 Improvement of multiple distillation by returning liquid from eac...

Figure 4.3 Equilibrium‐stage concept for determining countercurrent separati...

Figure 4.4 Graphical determination of the number of equilibrium stages 

whe...

Figure 4.5 Transfer‐unit concept for determining countercurrent separation e...

Figure 4.6 Graphical determination of the number of transfer units 

when bo...

Figure 4.7 Flow sheet of a continuously operated distillation column. Part o...

Figure 4.8 McCabe–Thiele diagram for binary distillation. The area between t...

Figure 4.9 Internal concentration and temperature profiles of a binary disti...

Figure 4.10 Feed lines for different values of the caloric state 

of the fe...

Figure 4.11 Distillation column and McCabe–Thiele diagram for multiple feed ...

Figure 4.12 McCabe–Thiele diagram for a distillation column with intermediat...

Figure 4.13 Feasible regions for operating lines of binary distillation. A) ...

Figure 4.14 Enthalpy–concentration diagram developed from the dew and boilin...

Figure 4.15 Representation of distillation in an enthalpy–concentration diag...

Figure 4.16 Enthalpy–concentration diagram of the ethanol/water system. A) M...

Figure 4.17 McCabe–Thiele diagram of a binary mixture at total reflux and re...

Figure 4.18 Plot of the results of Example 4.2. The dashed rectangles repres...

Figure 4.19 McCabe–Thiele diagram of a binary mixture at minimum reflux rati...

Figure 4.20 Minimum reboil ratio with tangential pinch. In such systems the ...

Figure 4.21 McCabe–Thiele diagram of a binary mixture at minimum reflux rati...

Figure 4.22 Minimum reflux and reboil ratios for sharp separations of ideal ...

Figure 4.23 McCabe–Thiele diagram of a binary mixture at minimum reflux rati...

Figure 4.24 Basic equations for calculating the energy requirement 

of dist...

Figure 4.25 Compilation of the relevant equations for the energy requirement...

Figure 4.26 Compilation of the relevant equations for the energy requirement...

Figure 4.27 Energy requirement of ideal binary mixtures as function of the f...

Figure 4.28 Internal liquid concentration profiles of a ternary mixture at f...

Figure 4.29 Results of the tray‐to‐tray calculation of ternary distillation ...

Figure 4.30 Separation regions of a ternary zeotropic mixture at total reflu...

Figure 4.31 Separation regions of a ternary mixture with a

minimum azeotr...

Figure 4.32 Separation regions of a ternary mixture with an

minimum azeot...

Figure 4.33 Separation regions of a ternary mixture with a

minimum azeotr...

Figure 4.34 Determination of feasible pure products of a single distillation...

Figure 4.35 Preferred separation, low boiler separation, and high‐boiler sep...

Figure 4.36 Flow sheet and internal liquid concentration profiles of a colum...

Figure 4.37 Types and loci of pinches at different modes of column operation...

Figure 4.38 Preferred separation of a ternary mixture at minimum reflux. Bot...

Figure 4.39 Separation of a pure low boiler as overhead fraction from a tern...

Figure 4.40 Parallelism of the

‐line and the

‐line of ideal ternary mixtur...

Figure 4.41 Vapor–liquid equilibrium of an ideal ternary mixture. A) If the ...

Figure 4.42 In non‐ideal mixtures the concentration profiles between the bin...

Figure 4.43 Separation of the high boiler as bottom fraction from a ternary ...

Figure 4.44 Results of Example 4.7 for a sharp low boiler separation.

Figure 4.45 Results of Example 4.7 for a sharp high boiler separation.

Figure 4.46 Compilation of the relevant equations for calculating the energy...

Figure 4.47 Energy requirement of preferred separation of the close‐boiling ...

Figure 4.48 Compilation of the relevant equations for calculating the energy...

Figure 4.49 Energy requirement of low boiler separation of the close‐boiling...

Figure 4.50 Energy requirement of low boiler separation of the close‐boiling...

Figure 4.51 Energy requirement of high boiler separation of the close‐boilin...

Figure 4.52 Energy requirement of high boiler separation of the close‐boilin...

Figure 4.53 Schematic of a single equilibrium stage for the derivation of th...

Figure 4.54 Schematic of a packed column for the derivation of a rate‐based ...

Figure 4.55 Dependency of point efficiency on mass transfer kinetics (Eq. 4....

Figure 4.56 Iteration history for solving the two non‐linear equations of Ex...

Figure 4.57 Jacobian matrix in the general form. The matrix contains

 subma...

Figure 4.58 Jacobian matrix of a distillation column. The matrix has a tridi...

Figure 4.59 Structure of the submatrices in the upper side diagonal of the J...

Figure 4.60 Structure of the submatrices in the main diagonal. The number of...

Figure 4.61 Structure of the submatrices in the lower side diagonal of the J...

Figure 4.62 Internal concentration profiles for the methanol/ethanol/n‐propa...

Figure 4.63 Internal concentration profiles for the acetone/chloroform/benze...

Figure 4.64 Internal concentration profiles for the methanol/ethanol/water s...

Chapter 5

Figure 5.1 Chemical equilibrium of the reaction

with

. The stoichiometric l...

Figure 5.2 Distillation lines of an ideal ternary mixture with

and

.

Figure 5.3 Design of a reactive distillation line of an ideal ternary mixtur...

Figure 5.4 A) Determination of reactive azeotropes of the reaction

. B) Det...

Figure 5.5 Determination of reactive azeotropes of the reaction

in a syste...

Figure 5.6 A) Determination of reactive azeotropes of the reaction

in a sy...

Figure 5.7 Reactive distillation line of the reaction

. There exists a reac...

Figure 5.8 Reactive distillation lines of the reaction

with a low boiling ...

Figure 5.9 Reactive distillation lines of Figure 5.8 presented by transforme...

Figure 5.10 Reactive distillation line of the reactions

and

.

Figure 5.11 A) Reactive distillation lines of the reaction

with

. B) Reac...

Figure 5.12 A) Process with sequential realization of reaction and distillat...

Figure 5.13 A) Process with sequential realization of reaction and distillat...

Figure 5.14 A) Conventional process for a decomposition reaction

and separ...

Figure 5.15 A) Conventional process for the decomposition reaction

. The se...

Figure 5.16 A) Conventional process for the reaction

and the side reaction...

Chapter 6

Figure 6.1 Schematics of batch distillation devices. A) Bottom vessel with r...

Figure 6.2 Batch distillation of a binary mixture at constant reflux policy....

Figure 6.3 Minimum energy requirement (at infinite number of stages) of batc...

Figure 6.4 Batch distillation of a binary mixture at constant distillate con...

Figure 6.5 Minimum energy requirement of batch distillation at constant dist...

Figure 6.6 Batch distillation of the n‐butanol/water mixture, which exhibits...

Figure 6.7 Variation of the reflux ratio 

versus relative amount of distill...

Figure 6.8 Comparison of minimum energy requirement (at infinite number of s...

Figure 6.9 Concentration profiles for batch distillation of the zeotropic te...

Figure 6.10 Graphical interpretation of Eq. (6.41). The distillate concentra...

Figure 6.11 Presentation of the concentration profiles of Figure 6.9 in a tr...

Figure 6.12 Influence of the reflux ratio 

on the distillate concentrations...

Figure 6.13 Influence of the number of equilibrium stages 

on the distillat...

Figure 6.14 Concentration profiles for the batch distillation of the ternary...

Figure 6.15 Concentration profiles for the batch distillation of the system ...

Figure 6.16 Concentration profiles for the batch distillation of a ternary s...

Figure 6.17 Batch distillation of an ideal quaternary mixture with relative ...

Figure 6.18 Course of distillate concentration 

versus

of the methanol/et...

Figure 6.19 Separation of the ternary mixture methanol/ethanol/n‐propanol wi...

Figure 6.20 Batch process for separating a binary mixture 

that exhibits a ...

Figure 6.21 Batch process for separating a binary mixture 

that exhibits a ...

Figure 6.22 Process for separating a binary azeotropic mixture by batch dist...

Figure 6.23 Batch process for separating a binary mixture with a maximum aze...

Figure 6.24 Batch process for separating a binary mixture with a minimum aze...

Figure 6.25 Batch process for separating the HCl/H

2

O mixture with the entrai...

Figure 6.26 Batch process for separating the ethanol/water mixture by toluen...

Figure 6.27 Batch process for separating the ethanol/water mixture by ethyle...

Chapter 7

Figure 7.1 Influence of thermal state 

of the feed on minimum energy requir...

Figure 7.2 Reduction of exergy losses of distillation columns. A) Generation...

Figure 7.3 Schematic of integrated heat pumps that use the products of the d...

Figure 7.4 Values of heat capacity ratios versus number of atoms in a molecu...

Figure 7.5 Modification of a heat pump applicable to columns that produce wa...

Figure 7.6 Multiple Stage Flash (MSF) process for the recovery of desalinate...

Figure 7.7 Flow sheet and minimum energy requirement of the

‐path, saturate...

Figure 7.8 Flow sheet and minimum energy requirement of the

‐path, saturate...

Figure 7.9 Flow sheet and minimum energy requirement of the

‐path, saturate...

Figure 7.10 Comparison of the minimum energy requirement 

of all three sepa...

Figure 7.11 Modification of the

‐path by material coupling of columns. The ...

Figure 7.12 Minimum energy requirement of the preferred

‐path with material...

Figure 7.13 Twofold separations in the sharp

‐path.

Figure 7.14 Modification of the

‐path by a side column (rectifying side col...

Figure 7.15 Energy requirement of the

‐path and

‐path with side column for...

Figure 7.16 Twofold separations in the sharp

‐path.

Figure 7.17 Modification of the

‐path by a side column (stripping side colu...

Figure 7.18 Twofold separations in the sharp

‐path.

Figure 7.19 Internal vapor and liquid flows of the preferred

‐path with sid...

Figure 7.20 Modification of the

‐path by a side column (intermediate side c...

Figure 7.21 Minimum energy requirement 

of the preferred

‐path with interm...

Figure 7.22 Three examples of dividing wall columns for separating ternary m...

Figure 7.23 Principle of thermal coupling of columns in the

‐path,

‐path, ...

Figure 7.24 Flow sheet and energy requirement of the

‐path with thermal cou...

Figure 7.25 Flow sheet and energy requirement of the

‐path with thermal cou...

Figure 7.26 Flow sheet and energy requirement of the

‐path with thermal cou...

Figure 7.27 Graphical plot of temperatures and enthalpies of the individual ...

Figure 7.28 Composite curves of the hot and cold streams. A) Hot streams. B)...

Figure 7.29 Position of the composite curves at a pinch temperature differen...

Figure 7.30 Determination of the optimal temperature levels of cold and hot ...

Figure 7.31 Construction scheme of the

grand composite curve

. The composite ...

Figure 7.32 Temperature–enthalpy plot of streams and utilities. This diagram...

Figure 7.33 Flow sheet of the optimal heat exchanger network with temperatur...

Figure 7.34 Grid representation of the heat exchanger network of Figure 7.33...

Figure 7.35 Simplification of the heat exchanger network by decreasing the t...

Figure 7.36 Grid presentation of the simplified heat exchanger network of Fi...

Figure 7.37 Temperature–enthalpy diagram of a network with dual path heat ex...

Figure 7.38 Grid presentation of the dual flow heat exchanger network of Fig...

Chapter 8

Figure 8.1 Comparison of power consumption for compressing of air and pumpin...

Figure 8.2 Vapor–liquid equilibrium and dew and boiling temperatures of H

2

O/...

Figure 8.3 Vapor pressure over a H

2

O/H

2

SO

4

mixture [

PERRY ET AL.

1984]. The ...

Figure 8.4 Process for concentrating diluted sulfuric acid.

Figure 8.5 Vapor pressure of ammonia/water solutions versus temperature [

RIZ

...

Figure 8.6 Process for recovering pure ammonia from wastewater [

WUNDER

1990]...

Figure 8.7 Process for recovery of HCl from waste inert gases [

STICHLMAIR

19...

Figure 8.8 McCabe–Thiele diagram for the process in Figure 8.7.

Figure 8.9 Linde process for air separation.

Figure 8.10 Recovery of oxygen and nitrogen from air by distillation. A) Two...

Figure 8.11 Determination of the operating pressure for thermally coupling o...

Figure 8.12 McCabe–Thiele diagram for the separation of toluene from water....

Figure 8.13 Process for separating high boiling organics from water. In the ...

Figure 8.14 Process for separating low boiling and high boiling organics fro...

Figure 8.15 Direct coupling of columns of the process in Figure 8.14 (see Se...

Figure 8.16 Process for separating low and high boiling organics from water ...

Figure 8.17 Vapor pressure curves for some high boiling organic compounds th...

Figure 8.18 Schematic of batch steam distillation.

Figure 8.19 Schematic of continuous multistage steam distillation.

Figure 8.20 Process for deodorizing of crude ester [

JOHANNISBAUER AND JEROMI

...

Figure 8.21 Process for refining palm oil [

STAGE

1988].

Figure 8.22 Paths for complete separation of a ternary mixture.

Figure 8.23 Determination of number of separation paths of ternary, quaterna...

Figure 8.24 Use of a rectifying side column for argon recovery in the Linde ...

Figure 8.25 Use of side columns in the separation of a quaternary mixture. A...

Figure 8.26 Use of stripping side columns in the atmospheric tower of crude ...

Figure 8.27 Flow sheet and McCabe–Thiele diagram for separation of the binar...

Figure 8.28 Flow sheet and phase diagram for separation of the ternary aceto...

Figure 8.29 Concentration of the azeotrope in the ethanol/water mixture as f...

Figure 8.30 Flow sheet and McCabe–Thiele diagram for separation of the binar...

Figure 8.31 Separation of the azeotropic acetone/heptane mixture using benze...

Figure 8.32 Separation of the azeotropic acetone/heptane mixture using benze...

Figure 8.33 Triangular concentration diagram for a process for separating az...

Figure 8.34 Minimum requirements for the selection for the entrainer 

for t...

Figure 8.35 Process for the separation of a binary mixture with a minimum az...

Figure 8.36 Process for the separation of a binary mixture with a minimum az...

Figure 8.37 Process for the separation of a binary mixture with a maximum az...

Figure 8.38 Process for the separation of a binary mixture with a minimum az...

Figure 8.39 Process for the separation of a binary mixture with a minimum az...

Figure 8.40 Two‐column process for the separation of hydrogen chloride (HCl)...

Figure 8.41 Two‐column process for the separation of a binary mixture (ethan...

Figure 8.42 Two‐column process for the separation of a binary mixture with a...

Figure 8.43 Separation of the ethanol/water mixture using toluene as entrain...

Figure 8.44 Separation of a binary mixture 

with a minimum azeotrope by usi...

Figure 8.45 Concentration of nitric acid and water by using sulfuric acid as...

Figure 8.46 Flow sheet of the process for the separation of the tetrahydrofu...

Figure 8.47 Process for the separation of the dichloromethane/methanol mixtu...

Figure 8.48 Process for the separation of the benzene/cyclohexane mixture by...

Figure 8.49 Process for the separation of the ethanol/water mixture by disti...

Figure 8.50 Process for the separation of mixtures of organics and water by ...

Figure 8.51 Process for dewatering bioethanol by distillation and vapor perm...

Figure 8.52 System properties of the MTBE synthesis process.

Figure 8.53 A) Reactive distillation lines for MTBE synthesis. B) Reactive d...

Figure 8.54 Synthesis of ethylene glycol in a reactive distillation column....

Figure 8.55 Process for synthesis of TAME.

Figure 8.56 Conventional process for the synthesis of methyl acetate from me...

Figure 8.57 Process for the synthesis of methyl acetate from methanol and ac...

Chapter 9

Figure 9.1 Principle of mass transfer processes.

Figure 9.2 Cutaway section of a tray column: (a) downcomer, (b) integrated s...

Figure 9.3 Cutaway section of a packed column with structured packing [

SULZE

...

Figure 9.4 Sketch of the operating region of a tray column (A) and a packed ...

Figure 9.5 Schematic illustration of a tray column with nomenclature and typ...

Figure 9.6 Examples of fixed valves and floating valves. A) Round fixed valv...

Figure 9.7 Correlation of the capacity factor 

for sieve trays according to...

Figure 9.8 Minimum gas load

of sieve trays for three different systems: (1...

Figure 9.9 Operating region of a tray column. The upper limits for gas and l...

Figure 9.10 Influence of the relative free area 

on the maximum and minimum...

Figure 9.11 Maximum and minimum gas load as a function of surface tension 

...

Figure 9.12 Schematic illustration of bubble regime, froth regime, and spray...

Figure 9.13 Comparison of published correlations for the relative liquid con...

Figure 9.14 Comparison of published correlations for the froth height 

(see...

Figure 9.15 Composition of the froth height 

based on the three terms of Eq...

Figure 9.16 Froth height 

versus the relative gas load 

. From this diagram...

Figure 9.17 Plot of published entrainment data versus the relative gas load 

Figure 9.18 Correlation of published entrainment data according to

STICHLMAI

...

Figure 9.19 Liquid mixing in the two‐phase layer on a sieve tray.

Figure 9.20 Liquid mixing in the two‐phase layer on a sieve tray. The dashed...

Figure 9.21 Liquid isotherms in the two‐phase layer on a bubble cap tray of ...

Figure 9.22 Calculated values for the volumetric interfacial area a of the t...

Figure 9.23 Pressure drop of a sieve tray versus gas load factor 

. Paramete...

Figure 9.24 Mechanism of fluid flow through a hole in a thin plate (A) and a...

Figure 9.25 Dependence of the orifice coefficient 

(

) of sieve trays with ...

Figure 9.26 Dependence of the orifice coefficient 

of bubble cap and valve ...

Figure 9.27 Determination of the number of actual trays with knowledge of tr...

Figure 9.28 Sketch of a single sieve tray with notations for point efficienc...

Figure 9.29 Application of the dispersion model to liquid mixing on a tray....

Figure 9.30 Relation between the ratio of overall tray efficiency 

to point...

Figure 9.31 Dependency of point efficiency on the number of transfer units....

Figure 9.32 Typical experimental values of the gas‐side point efficiency 

v...

Figure 9.33 Qualitative comparison of capacity and separation efficiency of ...

Figure 9.34 Selected elements used in random packings: first row: ceramic, s...

Figure 9.35 Structured packing assembled by corrugated sheets.

Figure 9.36 Model structures of packings.

Figure 9.37 Cutaway section of a packed column with structured packing [

SULZ

...

Figure 9.38 Operating region of a packed column.

Figure 9.39 Correlation of flooding point and irrigated pressure drop accord...

Figure 9.40 Correlation of flooding, loading, and irrigated pressure drop ac...

Figure 9.41 Presentation of flooding point data [

BILLET

1995].

Figure 9.42 Sketch for explanation of static and dynamic hold‐up based on

BR

...

Figure 9.43 Liquid hold‐up data of a random packing of metal Bialecki rings ...

Figure 9.44 Modified plot of the hold‐up data of Figure 9.43.

Figure 9.45 Correlation of the friction factor of single particles of some p...

Figure 9.46 Dry and irrigated pressure drop of a random packing of metal Bia...

Figure 9.47 Maldistribution in a random packing of 35 mm metal Pall rings [

M

...

Figure 9.48 Liquid distribution profile calculated with the TUM–WelChem cell...

Figure 9.49 Comparison of experimental (top) and simulated (bottom) liquid d...

Figure 9.50 Flow pattern of water and heptane on a vertical plate. A) Metal ...

Figure 9.51 Wettability of several packing materials [

ZECH

1978].

Figure 9.52 Interfacial area of a metal Pall ring packing (

) predicted by d...

Figure 9.53 Height of a transfer unit 

of a random packing of metal Pll rin...

Figure 9.54 Height of a transfer unit 

of a structured packing (Ralu‐pak 25...

Figure 9.55 Result of direct numerical simulation of binary distillation in ...

Figure 9.A.1 A) Single particle in suspension. B) Swarm of particles in susp...

Figure 9.A.2 Dependence of the exponent 

of Eq. (9.A.2) on the Reynolds num...

Figure 9.A.3 Comparison of experimental fluidization data with Eq. (9.A.14) ...

Figure 9.A.4 Pressure drop data of fixed beds of sheers and granulates accor...

Figure 9.A.5 Pressure drop data of a fixed bed of spheres according to

RUMPF

...

Chapter 10

Figure 10.1 Examples of important control loops. A) Single loop control with...

Figure 10.2 Level controller LC. A) Single control loop. B) Cascade control ...

Figure 10.3 Flow controllers with stream split control; one of the two split...

Figure 10.4 Flow control with split of liquid condensate at the top of the c...

Figure 10.5 Flow control with split of liquid condensate at top of the colum...

Figure 10.6 Flow control with split of liquid at the bottom of the column. A...

Figure 10.7 Pressure control of a distillation column. A) Manipulating draw‐...

Figure 10.8 Pressure control of a distillation column. A) Manipulating flow ...

Figure 10.9 Pressure control of a column with air‐cooled condensers. A) Part...

Figure 10.10 Temperature profile in a distillation column with flattened tem...

Figure 10.11 A) Process flow diagram of a distillation column as interconnec...

Figure 10.12 Basic D–G control configuration.

Figure 10.13 Basic B–L control configuration.

Figure 10.14 Basic L–G control configuration.

Figure 10.15 B–L configuration with ratio control FFC.

Figure 10.16 One‐point composition control with D–G configuration.

Figure 10.17 One‐point composition control with B–L configuration.

Figure 10.18 One‐point composition control with L–G configuration and temper...

Figure 10.19 One‐point composition control with a L–G configuration and temp...

Figure 10.20 Two‐point composition control with a D–G configuration.

Figure 10.21 Two‐point composition control with a B–L configuration.

Figure 10.22 Two‐point composition control with a L–G configuration.

Figure 10.23 Two‐point composition control with a D–B configuration.

Figure 10.24 Graphical illustration of the correlations in Eqs. (10.1) and (...

Figure 10.25 Application ranges of control configurations using split Rule 2...

Figure 10.26 Application ranges of control configurations using split Rule 2...

Figure 10.27 Application ranges of control configuration at minimum reflux a...

Figure 10.28 Application ranges of control configuration at minimum reflux a...

Figure 10.29 Expanded application range of the D–G configuration for a satur...

Figure 10.30 Expanded application range of the B–L configuration.

Figure 10.31 Expanded application range of the L–G configuration.

Figure 10.32 Control configuration of a distillation process for separating ...

Figure 10.33 Control structure of an air separation double column with B–L c...

Figure 10.34 Control configuration of a process for separating a ternary mix...

Figure 10.35 Control configuration of a distillation process for separating ...

Figure 10.36 Control structure of a batch distillation process operated with...

Guide

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DISTILLATION

Principles and Practice

Second Edition

Prof. Dr.-Ing. JOHANN STICHLMAIR

Prof. Dr.-Ing. HARALD KLEIN

Dr.-Ing. SEBASTIAN REHFELDT

Copyright © 2021 by American Institute of Chemical Engineers, Inc. All rights reserved.

A Joint Publication of the American Institute of Chemical Engineers and John Wiley & Sons, Inc.

Published by John Wiley & Sons, Inc., Hoboken, New Jersey.

Edition History

Wiley‐VCH (1e, 1998)

All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, recording or otherwise, except as permitted by law. Advice on how to obtain permission to reuse material from this title is available at http://www.wiley.com/go/permissions.

The right of Prof. Dr.-Ing. Johann Stichlmair, Prof. Dr.-Ing. Harald Klein, and Dr.-Ing. Sebastian Rehfeldt to be identified as the authors of this work has been asserted in accordance with law.

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In view of ongoing research, equipment modifications, changes in governmental regulations, and the constant flow of informataion relating to the use of experimental reagents, equipment, and devices, the reader is urged to review and evaluate the information provided in the package insert or instructions for each chemical, piece of equipment, reagent, or device for, among other things, any changes in the instructions or indication of usage and for added warnings and precautions. While the publisher and authors have used their best efforts in preparing this work, they make no representations or warranties with respect to the accuracy or completeness of the contents of this work and specifically disclaim all warranties, including without limitation any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales representatives, written sales materials or promotional statements for this work. The fact that an organization, website, or product is referred to in this work as a citation and/or potential source of further information does not mean that the publisher and authors endorse the information or services the organization, website, or product may provide or recommendations it may make. This work is sold with the understanding that the publisher is not engaged in rendering professional services. The advice and strategies contained herein may not be suitable for your situation. You should consult with a specialist where appropriate. Further, readers should be aware that websites listed in this work may have changed or disappeared between when this work was written and when it is read. Neither the publisher nor authors shall be liable for any loss of profit or any other commercial damages, including but not limited to special, incidental, consequential, or other damages.

Library of Congress Cataloging‐in‐Publication Data

Names: Stichlmair, Johann, author. | Klein, Harald, author. | Rehfeldt,

  Sebastian, author.

Title: Distillation : principles and practice / Johann Stichlmair, Harald

  Klein, Sebastian Rehfeldt.

Description: Second edition. | Hoboken, New Jersey : Wiley‐AIChE, [2021] |

  Includes bibliographical references and index.

Identifiers: LCCN 2020024694 (print) | LCCN 2020024695 (ebook) | ISBN

  9781119414667 (cloth) | ISBN 9781119414698 (adobe pdf) | ISBN

  9781119414681 (epub)

Subjects: LCSH: Distillation.

Classification: LCC TP156.D5 S85 2021 (print) | LCC TP156.D5 (ebook) |

  DDC 660/.28425‐dc23

LC record available at https://lccn.loc.gov/2020024694

LC ebook record available at https://lccn.loc.gov/2020024695

Cover image: © Mina De La O/Getty Images

Cover design by Wiley

Preface

Distillation is the most important and the most effective technology for the fractionation of multicomponent mixtures. Fields of application are all branches of the process industry, for instance, petroleum refineries, chemical industries, and food industries. The often very tall distillation towers dominate the view of many chemical sites. According to its great importance, distillation is a highly developed technology.

The fundamental mechanism of distillation is the mass transfer between a gaseous and a liquid phase. The driving force for this interfacial mass transfer is the difference between the actual and the equilibrium concentration of the phases.

The book consists of 10 chapters. Chapter 1 deals with the basic principle of distillation and with some historical aspects of the art.

Chapter 2 concentrates on the thermodynamics of vapor–liquid equilibrium, since a good knowledge of vapor–liquid equilibrium is an indispensable prerequisite for the design of distillation processes. As compared to many other textbooks, the mixtures are not limited to two components, but ternary mixtures along with their boiling surfaces and triangular diagrams are considered.

The Chapters 3–6 deal with the thermodynamics of single‐stage distillation (Chapter 3) and multi‐stage distillation (Chapter 4), which is often called rectification, reactive distillation (Chapter 5), and batch distillation (Chapter 6). Special attention is given as described above to ternary mixtures, since they represent a more general case than binary mixtures most textbooks on distillation focus on.

In Chapter 7 the energy requirement of distillation processes is discussed. This chapter demonstrates how the large energy requirement of distillation processes can be drastically reduced by internal column coupling and intelligent process modifications.

Important examples of industrial distillation processes are presented in Chapter 8. Here, special attention is given to processes for the fractionation of azeotropic mixtures.

The design of distillation columns is treated in Chapter 9 with focus on tray columns and packed columns. Finally, the control of distillation columns is the objective of Chapter 10 where the concept of split stream control is applied.

The prime intention of this textbook is to let the reader develop a deep understanding of the art of distillation. Many fully worked out examples demonstrate the easy applicability of the theoretical findings. These examples are arranged in boxes to facilitate the readability of the text.

Of course, not only the authors are involved in the completion of such a comprehensive book. At this point we would like to thank everyone who contributed to the success of this project: Felicitas Engel, M.Sc., Philipp Fritsch, M.Sc., Patrick Haider, M.Sc., Florian Hanusch, M.Sc., Robert Kender, M.Sc., Thomas Kleiner, M.Sc., Maximilian Neumann, M.Sc., Dr.‐Ing. Anna Reif, Marc Xia, M.Sc., Alexander Eder, B.Sc., Florian Kaufmann, M.Sc., and Jan Oettig, B.Sc., as well as the valuable expertise of Dr.‐Ing. Volker Engel. Many thanks also to Stephan Korell for his helpful advice on the LATE X implementation.

Johann Stichlmair,

Harald Klein,

Sebastian Rehfeldt

Munich, February 2020

Nomenclature

Latin Symbols

low boiler

–

specific surface area

specific effective interfacial area

cohesion pressure van der Waals equation

coefficient cubic equation of state of mixture

coefficient cubic equation of state of pure component 

cross coefficient cubic equation of state of component 

and 

activity of component 

–

area

Antoine or Wagner parameter of component 

–

binary parameter Margules and van Laar equation of component 

and 

–

high boiler (binary mixture) or intermediate boiler (ternary mixture)

–

constant

–

co‐volume van der Waals equation

coefficient cubic equation of state of mixture

coefficient cubic equation of state of pure component 

mole amount of bottom product

width of packing channel base

bottom flow rate

virial coefficient of mixture

Antoine or Wagner parameter of component 

–

virial coefficient of pure component 

cross virial coefficient of component 

and 

high boiler (ternary mixture) or intermediate boiler (quaternary mixture)

–

specific or molar heat capacity

constant

–

second mixture virial coefficient of mixture

Antoine or Wagner parameter of component 

–

capacity factor

empiric packing factor

–

high boiler quaternary mixture

–

diameter, distance

diameter

diffusion coefficient

mole amount of overhead product (distillate)

overhead (distillate) flow rate

dispersion coefficient (eddy diffusion coefficient)

Wagner parameter of component 

–

entrainer

–

overall gas‐side point efficiency

–

overall gas‐side tray efficiency

–

exergy

friction factor

–

fugacity of component 

standard fugacity of component 

‐factor (gas load)

mole amount of feed

feed flow rate

surface area fraction/mole fraction UNIQUAC equation of component 

–

gravitational acceleration

molar Gibbs free energy

gas flow rate of component 

partial molar Gibbs free energy of component 

molar mixing Gibbs free energy

molar excess free energy

partial molar excess free energy of component 

binary parameter NRTL equation of component 

and 

–

mole amount of vapor

gas/vapor flow rate

Gibbs free energy

excess free energy

binary parameter NRTL equation of component 

and 

–

specific or molar enthalpy

partial molar enthalpy of component 

molar mixing enthalpy

height

dynamic hold‐up

dynamic hold‐up below loading point

froth height

clear liquid height

liquid hold‐up

height of pressure drop

static hold‐up

weir height

enthalpy

enthalpy flow rate

tray spacing or packing height

Henry coefficient of component 

in component 

molar hold‐up of liquid

height equivalent to one theoretical plate

height of a transfer unit

stripping factor

–

numbers of components in mixture

–

mass transfer coefficient

binary parameter cubic equation of state of component 

and 

–

vapor–liquid equilibrium ratio of component 

–

reaction equilibrium constant

–

(path) length

liquid flow rate of component 

amount of liquid

liquid flow rate

wetted perimeter

slope of equilibrium curve

–

exponent

–

mass

mole amount of mixture in the middle vessel

molecular weight

mixture flow rate

number of equilibrium stages

–

exponent

–

mole amount

molar flow rate

number of transfer units

–

pitch

pressure

partial pressure of component 

saturation vapor pressure of pure component 

reference pressure

number of phases

–

Poynting correction of component 

–

relative van der Waals surface UNIQUAC equation of component 

–

caloric factor (thermal state) of the feed

–

heat

dimensionless concentration change

–

heat flow

relative van der Waals volume UNIQUAC equation of component 

–

molar latent heat of vaporization

ideal gas constant

reactor effluent flow rate

external reboil (boilup) ratio

–

external reflux ratio

–

molar entropy

plate thickness

length of packing channel side

molar flow rate after decanter, side product

entropy

correction factor (

Example 2.2

)

–

time

temperature

boiling temperature of pure component 

superficial velocity

binary parameter UNIQUAC equation of component 

and 

–

internal energy

molar volume

partial molar volume of component 

molar mixing volume

volume

volumetric flow rate

volume fraction/mole fraction UNIQUAC equation of component 

–

mass (weight) fraction of component 

–

mass fraction of component 

 in gas phase

mass fraction of component 

 in liquid phase

work

mole fraction liquid phase of component 

–

transformed mole fraction complete chemical reaction of component 

–

function

transformed concentration of component 

 in reactive systems

–

mole fraction vapor phase of component 

–

estimated mole fraction vapor phase of component 

 (

Example 2.3

)

–

number of interacting molecules UNIQUAC equation

–

number of particles or channels

–

locus, dimensionless tray length

–

mole fraction two‐phase mixture of component 

–

compressibility factor

–

number of independent state variables (degrees of freedom)

–

Greek Symbols

discharge coefficient

–

1Introduction

Distillation is a widely used method for separating liquid mixtures into their components. It is the workhorse for separation in the petroleum, petrochemical, chemical, and related industries. The consensus is that it will continue to dominate these industries in the future, too.

1.1 Principle of Distillation Separation

Distillation utilizes a very simple separation principle: an intimate contact is created between the starting mixture and a second phase in order to enhance an effective mass transfer between these two phases. The thermodynamic conditions are chosen so that primarily the component to be separated from the feed mixture enters the second phase. The phases are subsequently separated into two single phases with different compositions.

Three steps are always involved in the implementation of this separation principle; see Figure 1.1:

Figure 1.1 General principle of fractionation in thermal separation technology. The essential mechanism is the mass transfer between two phases.

Generation of a two‐phase system

Mass transfer across the interface

Separation of the phases

Many separation techniques utilize this very effective separation principle. Absorption, desorption, evaporation, condensation, and distillation involve a gaseous and a liquid phase. Solvent extraction uses two liquid phases. Separation techniques that utilize a fluid phase and a solid phase include adsorption, crystallization, drying, and leaching. In most of these separation processes, the necessary two‐phase system is generated by adding an auxiliary phase to the feed mixture. The substances to be separated collect in diluted form in the auxiliary agent. In distillation, however, the second phase is created by partial vaporization of the liquid feed. Hence, the use of an auxiliary substance (often called a mass separating agent), which requires costly recovery, is avoided, and the components to be separated are recovered as relatively pure substances. Indeed, distillation requires only energy in the form of heat, which can subsequently be easily removed from the system. This is an important advantage of distillation.

In practice, distillation requires intimate contacting of vapor and liquid under such conditions that the desired components of the liquid enter the vapor phase. Governing these conditions is the vapor–liquid equilibrium. Many activities on the art of distillation are devoted to find out how closely the vapor–liquid equilibrium can be approached. In any case, it is necessary to separate the liquid and vapor phases afterward.

The vapor and liquid are brought into intimate contact by countercurrent or crosscurrent flow, and mass exchange occurs because the two phases are not in thermodynamic equilibrium. The phases produced during distillation are formed by evaporation and condensation of the initial mixture. The separation process can be controlled only by the heat supply.

The basis for planning distillation processes is the knowledge of the vapor–liquid equilibrium. As stated earlier, the separation depends primarily on the concentration of the individual substances in the vapor and liquid phases. In this book, principles of vapor–liquid equilibrium are discussed in Chapter 2