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Distillation: Equipment and Processes

Distillation: Equipment and Processes

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Distillation: Equipment and Processes

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Jun 24, 2014


Distillation: Equipment and Processes—winner of the 2015 PROSE Award in Chemistry & Physics from the Association of American Publishers—is a single source of authoritative information on all aspects of the theory and practice of modern distillation, suitable for advanced students and professionals working in a laboratory, industrial plants, or a managerial capacity. It addresses the most important and current research on industrial distillation, including all steps in process design (feasibility study, modeling, and experimental validation), together with operation and control aspects. This volume features an extra focus on distillation equipment and processes.
  • Winner of the 2015 PROSE Award in Chemistry & Physics from the Association of American Publishers
  • Practical information on the newest development written by recognized experts
  • Coverage of a huge range of laboratory and industrial distillation approaches
  • Extensive references for each chapter facilitates further study
Jun 24, 2014

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  • In an azeotropic distillation process, a third component, the entrainer, is added to a binary mixture to influence the azeotropic system in such a way that collection of pure products is possible.

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Distillation - Academic Press


Equipment and Processes


Andrzej Górak

Laboratory of Fluid Separations, Department of Biochemical and Chemical Engineering, TU Dortmund University, Emil-Figge-Str. 70, D-44227 Dortmund

Žarko Olujić

Delft University of Technology, Process & Energy Laboratory, Leeghwaterstraat 39, NL-2628 CB DELFT

Table of Contents

Cover image

Title page


Preface to the Distillation Collection

Preface to Distillation: Equipment and Processes

List of Contributors

List of Symbols and Abbreviations

Chapter 1. Types of Distillation Column Internals

1.1. Introduction

1.2. Performance characteristics of vapor–liquid contactors

1.3. Criteria for selection of vapor–liquid contactors

1.4. Closing remarks and outlook

Chapter 2. Distillation Trays

2.1. Introduction

2.2. Tray layouts in columns

2.3. Comparison with packings

2.4. Single-pass crossflow trays

2.5. Decks

2.6. Multipass crossflow trays

2.7. Design variables

2.8. Liquid and vapor phases

2.9. Tray hydraulics

2.10. Hydraulic variables

2.11. Deck biphase regimes

2.12. Minimum loadings

2.13. Maximum loadings

2.14. Overall tray performance and efficiency

2.15. Other hydraulic considerations

2.16. Column and tray design

2.17. Tray efficiencies

2.18. Crossflow tray variations

2.19. Dual-flow trays

2.20. Augmented crossflow trays

2.21. Counterflow trays

2.22. Co-current flow trays

2.23. Other trays

2.24. Column feeds and draws

2.25. Mechanical considerations

2.26. Tray revamps

2.27. Safety considerations

2.28. Conclusions

2.29. Outlook

Chapter 3. Random Packings

3.1. Introduction

3.2. Development of packed columns and their significance in distillation and absorption technology

3.3. Fluid dynamic performance of randomly packed columns

3.4. Mass transfer of random packed columns

3.5. Maldistribution in random packings

3.6. Computer programs for packed column design

3.7. Evaluation of model parameters for random packings

3.8. Summary and conclusions

Chapter 4. Structured Packings

4.1. Introduction

4.2. Structured packing types

4.3. Hydraulic performance

4.4. Mass transfer

4.5. Column internals

4.6. Maldistribution

4.7. Applications of structured packings

Chapter 5. Dividing-Wall Columns

5.1. Introduction

5.2. Performance characteristics and concerns

5.3. Fields of application

5.4. Basic types of DWCs

5.5. Thermally coupled distillation columns

5.6. Column internals and construction

5.7. Control of DWCs

5.8. Simulation and design of DWCs

5.9. Conclusions and outlook

Chapter 6. Extractive Distillation

6.1. Introduction

6.2. Extractive distillation in academia and industry

6.3. Entrainer selection for extractive distillation

6.4. Process synthesis and design

6.5. minT azeotrope separation case studies

6.6. maxT azeotrope separation with light or heavy entrainer

6.7. Low-relative-volatility mixture separation

6.8. Heterogeneous extractive distillation

6.9. Conclusions

Chapter 7. Azeotropic Distillation

7.1. Introduction

7.2. Fundamentals

7.3. Separation example: ethanol–water with toluene

7.4. Conclusions

Chapter 8. Reactive Distillation

8.1. Introduction

8.2. Fundamentals

8.3. Process synthesis and design

8.4. Modeling

8.5. Hardware aspects

8.6. Industrial applications

8.7. Batch reactive distillation

8.8. New application trends

Chapter 9. Vacuum and High-Pressure Distillation

9.1. Introduction

9.2. Operating pressure ranges and selection criteria

9.3. Pressure effects

9.4. Column performance considerations

9.5. Equipment design considerations

9.6. Concluding remarks and outlook

Chapter 10. Laboratory Distillation and Scale-up

10.1. Introduction: the scale-up problem

10.2. Process scale-up and equipment scale-up

10.3. Process scale-up: experimental aspects

10.4. Methods to get data for process scale-up

10.5. Equipment scale-up

10.6. Discussion and outlook



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Preface to the Distillation Collection

For more than 5,000 years distillation has been used as a method for separating binary and multicomponent liquid mixtures into pure components. Even today, it belongs to the most commonly applied separation technologies and is used at such a large scale worldwide that it is responsible for up to 50% of both capital and operating costs in industrial processes. It moreover absorbs about 50% of the total process energy used by the chemical and petroleum refining industries every year. Given that the chemical industry consumed 19% of the entire energy in Europe (2009), distillation is the big driver of overall energy consumption.

Although distillation is considered the most mature and best-understood separation technology, knowledge on its manifold aspects is distributed unevenly among different textbooks and manuals. Engineers, by contrast, often wish for just one reference book in which the most relevant information is presented in a condensed and accessible form. Distillation aims at filling this gap by offering a succinct overview of distillation fundamentals, equipment, and applications. Students, academics, and practitioners will find in Distillation a helpful summary of pertinent methods and techniques and will thus be able to quickly resolve any problems in the field of distillation.

This book provides a comprehensive and thorough introduction into all aspects of distillation, covering distillation history, fundamentals of thermodynamics, hydrodynamics, mass transfer, energy considerations, conceptual process design, modeling, optimization and control, different column internals, special cases of distillation, troubleshooting, and the most important applications in various industrial branches, including biotechnological processes.

Distillation forms part of the Handbook of Separation Sciences series and is available as a paper book and as an e-book, thus catering to the diverging needs of different readers. It is divided into three volumes: Fundamentals and principles (Editors A. Górak and E. Sorensen), Equipment and processes (Editors A. Górak and Ž. Olujić), and Operation and applications (Editors A. Górak and H. Schoenmakers). Each volume contains chapters written by individual authors with acclaimed expertise in their fields. In addition to that, readers will find cross-references to other chapters, which allow them to gain an extensive overview of state-of-the-art technologies and various research perspectives. Helpful suggestions for further reading conclude each chapter.

A comprehensive and complex publication such as Distillation is impossible to complete without the support of an entire team whose enduring help I wish to acknowledge. In particular, I wish to express my heartfelt gratitude to the 42 leading world experts from the academia and industry who contributed to the chapters of this book. I thank the co-editors of the three volumes of Distillation—Dr Eva Sorensen, UCL, Dr Žarko Olujić, Delft University of Technology, and Dr Hartmut Schoenmakers, former member of BASF SE, Ludwigshafen—for their knowledgeable input and expertise, unremitting patience, and continuous encouragement. The invaluable editorial assistance of Dipl.-Ing. Johannes Holtbrügge during the entire editorial process is also greatly acknowledged.

Editorial assistance of Vera Krüger is also appreciated. I thank the Elsevier team Jill Cetel, Beth Campbell and Mohanambal Natarajan for their support and valuable help through the whole editing process.

Dr Andrzej Górak,     TU Dortmund University

Preface to Distillation: Equipment and Processes

The book Distillation: Equipment and Processes covers distillation equipment- and processes-related subjects and consists of 10 chapters. The approach, the depth, and the extent of subject coverage depend on the author(s) personal choice and affinities and therefore differ from chapter to chapter. Nevertheless all reflect the state of the art.

Starting chapter describes and discusses basic types and performance characteristics of well-established vapor–liquid contacting devices. Specific features and relative advantages/limitations of common types of trays, random packings, and structured packings are emphasized to facilitate choices in this respect. In Chapter 2 main types of trays and their layouts are described in a general way addressing their performance characteristics and all what needs to be considered to ensure proper function of a tray across a wide range of operating conditions. Random packings are described in Chapter 3 in an elaborated way, starting with a brief historical overview and performance characteristics of columns equipped with random packings. Main body includes a detailed description of important hydraulics and mass transfer performance-related parameters as well as background and features of related design method accounting for performance-deteriorating vapor and liquid maldistribution effects. Similar approach but in a more generalized and illustrative way is utilized in Chapter 4, where main performance characteristics and relative advantages of conventional and high-performance structured packings are described and discussed. Particular attention is paid to initial liquid maldistribution and its detrimental effects as well as that encountered in columns subject to motion. A simple method to estimate its extent as well as counteracting measures is discussed and main benefits of optimal performance illustrated using as examples important industrial applications. Chapter 5 introduces and discusses equipment design, column configuration, and operation-related aspects of the most sustainable among distillation technologies, i.e. dividing wall column (DWC), exploring the potential and prospects for expansion of the application window to four-product separations.

Separation of mixtures including azeotropes is addressed in Chapters 6 and 7. Chapter 6 is a comprehensive overview of advances made in extractive distillation that thanks to improvements in technology and selection of entrainers had gained a revived attention in academia and industry. Azeotropic distillation, as described in a concise way in Chapter 7 still preserves its position and importance in established industrial applications. Chapter 8 is an updated review and systematic and comprehensive coverage of reactive distillation, i.e. a special type of separation wherein the distillation process is accompanied by chemical reactions. Fundamental considerations are followed by discussion of benefits, limitations, modeling approaches, and design methods as well as hardware aspects, and possibilities for coupling with other unit operations to enhance overall performance of green processes are enlightened including recent research. Chapter 9 discusses the operating pressure selection criteria and explores pressure effects on stage and reflux requirement, distillation process in general, and trayed and packed columns hydraulics and efficiency in particular. Finally, Chapter 10 considers issues and describes a method and practices associated with scale-up of equipment in less-known distillation applications.

At the end I would like to thank all the authors for their contributions.

Dr Žarko Olujić,     Delft University of Technology

List of Contributors

Wolfgang Arlt,     FAU Erlangen-Nuremberg, Erlangen, Germany

Markus Duss,     Sulzer Chemtech AG, Winterthur, Switzerland

Vincent Gerbaud

Université de Toulouse, INP, UPS, LGC (Laboratoire de Génie Chimique), 4 allée Emile Monso, F-31432 Toulouse Cedex 04 – France

CNRS, LGC (Laboratoire de Génie Chimique), F-31432 Toulouse Cedex 04 – France

Björn Kaibel,     BASF SE, ZOT/O – C 104, Ludwigshafen, Germany

Tobias Keller,     Laboratory of Fluid Separations, TU Dortmund University, Dortmund, Germany

Jerzy Maćkowiak

ENVIMAC Engineering GmbH, Oberhausen, Germany

ENVIMAC Polska Sp. z o.o., Ostrów Wielkopolski, Poland

Jan F. Maćkowiak

ENVIMAC Engineering GmbH, Oberhausen, Germany

ENVIMAC Polska Sp. z o.o., Ostrów Wielkopolski, Poland

Žarko Olujić,     Process and Energy Laboratory, Delft University of Technology, Delft, The Netherlands

Michael Resetarits,     Fractionation Research, Inc., Stillwater, OK, USA

Ivonne Rodriguez-Donis,     Instituto Superior de Tecnologías y Ciencias Aplicadas (InSTEC). Ave Salvador Allende y Luaces. La Habana. 10400. Cuba

Hartmut Schoenmakers,     Ahornweg, Dossenheim, Germany

Lothar Spiegel,     Sulzer Chemtech AG, Winterthur, Switzerland

List of Symbols and Abbreviations

Latin symbols


Greek symbols


Abbreviations of chemical compounds

Note: Used abbreviations of hydrocarbons on the basis of C atoms.

Dimensionless numbers

Chapter 1

Types of Distillation Column Internals

Žarko Olujić     Process and Energy Laboratory, Delft University of Technology, Delft, The Netherlands


There are basically two different types of distillation column internals: those whose principal role is to create sufficient interfacial area and ensure within given contact times the intimate and intensive contact of vapor and liquid, and those belonging to ancillary equipment that enables both smooth functioning of the former and the operating column as a whole. Detailed accounts on trays, random packings, and structured packings are given in separate chapters (Chapters 2 to 4); the present chapter provides a concise description of generic aspects and addresses in greater detail relative performance characteristics of these particular devices.


Capacity; Column internals; Distillation; Efficiency; Equipment selection criteria; Foaming; Fouling; Liquid holdup; Pressure drop; Random packings; Structured packings; Trays; Turndown

Chapter Outline

1.1 Introduction 2

1.1.1 Distillation column anatomy (internal structure) 3

1.1.2 Methods and main features of distillation equipment operation 5

1.2 Performance characteristics of vapor–liquid contactors 7

1.2.1 Trays 8

1.2.2 Random packings 10

1.2.3 Structured packings 11

1.2.4 Grids 15

1.2.5 Ancillary equipment (internals) for packed columns 16

1.3 Criteria for selection of vapor–liquid contactors 18

1.3.1 Capacity 19

1.3.2 Pressure drop 21

1.3.3 Efficiency 21

1.3.4 Turndown 24

1.3.5 Sensitivity to fouling 24

1.3.6 Sensitivity to corrosion 25

1.3.7 Choice of construction material 26

1.3.8 Access for inspection 26

1.3.9 Scalability 26

1.3.10 Know-how/experience 27

1.3.11 Cost 28

1.3.12 Operating pressure 28

1.3.13 Liquid load 28

1.3.14 Liquid holdup 29

1.3.15 Foaming 29

1.3.16 Heat transfer 29

1.3.17 Installation 30

1.3.18 Revamping 31

1.3.19 Large column diameter 32

1.4 Closing remarks and outlook 32

Acknowledgements 33

References 33

1.1. Introduction

Distillation operations are carried out in columns, that is, cylindrical pressure vessels with large height to diameter ratios, containing various kinds of internals chosen and arranged appropriately to enable cost-effective separation of binary or multicomponent, mainly liquid, feed mixtures into desired pure products or specified fractions.

As mentioned by Stichlmair and Fair in the preface of Distillation—Principles and Practice, which focuses on understanding of the principles and their translation into basic design practices, distillation columns are the workhorses of the petroleum, petrochemical, chemical, and related process industries [1]. A complementary, more pragmatic view is given by Kister in Distillation Design, with emphasis on the practical aspects and reliability as encountered and required during the design of distillation columns [2].

The outgoing point for design of a new distillation column is the top and/or bottom product specification (required purity and/or recovery) for a given feed mixture, with known composition, flow rate, and thermal state at a given pressure and temperature. Upon choosing the operating pressure and assuming column pressure drop, detailed column performance calculations deliver optimum stage and reflux requirements, all based on appropriate vapor–liquid equilibrium data. The next, column dimensioning step is concerned with determining column diameter(s) and height for the chosen type of vapor–liquid contacting device. Critical positions are the top and bottom stage of rectification and stripping sections, and the column shell diameter is usually based on the stage with the maximum vapor load; and to complete the design calculations properly, one or more iterations on pressure drop are required.

Upon completing stage and reflux requirement calculations, the internal flow rates of vapor and liquid as well as corresponding values of relevant physical properties (densities and viscosities of two phases and surface tension) are known per stage and serve as the basis for the determination of column diameter(s). However, the number of theoretical plates or equilibrium stages, which is by definition the number of times the mass transfer equilibrium has to be established between ascending vapor and descending liquid streams above and below the feed to achieve desired separation, cannot be directly translated into column height. Namely, along an operating distillation column the equilibrium between vapor and liquid is never fully established. The column height required to produce the degree of mass transfer equivalent to the given number of equilibrium stages will depend on the type and performance characteristics of equipment (internals) chosen to generate interfacial area, that is, to enable mass transfer to occur so that for each component the required number of moles is transported accordingly, from vapor to liquid and reverse within the contact time available.

1.1.1. Distillation column anatomy (internal structure)

Regarding the equipment used to promote intimate contact of ascending vapor and descending liquid in a distillation column or tower, a distinction is generally made between plate or tray columns and packed columns, and in the case of the latter, between randomly and orderly packed columns, that is, random and structured packings.

Figure 1.1 shows schematically a distillation column shell containing all relevant equipment as employed in packed and/or trayed columns. From the top to the bottom: (1) a demister, i.e. a device for removal of entrained droplets from the vapor leaving the column through the nozzle at the top of the column; a liquid distributor (2) irrigating a randomly packed bed (3) laying on a V-shaped support plate (4). One should note that normally a hold-down plate (hard to see here) is used to prevent bed expansion in an upward direction due to pressure upsets during operation.

The liquid leaving the randomly packed bed is collected in a chevron (vane)-type liquid collector (5), where it is mixed with the liquid feed entering through a nozzle at the side of the column. The mixed liquid enters via a down pipe the liquid distributor (2), irrigating a bed consisting of two different sizes of a corrugated sheet structured packing (6), supported by a support plate (4). The liquid leaving the structured packing bed is collected using a liquid collector (7) with holes in the bottom. This or similar so-called chimney tray liquid collectors (9) are often used in combination with the packed column vapor inlet device (8) shown here, to ensure a good initial distribution of vapor entering the packed bed above. This particular device, known as schoepentoeter, handles with ease two-phase (biphasic) feeds, as delivered by falling film and thermosyphon type reboilers.

In the present case, a chimney tray collector (7) collects and mixes the liquid leaving the packed bed above, and the another one (9) collects the liquid coming from the vapor inlet device (schoepentoeter) (8), and delivers it via a central downcomer to the top tray of a section containing three fixed-valve, two-pass trays (10). The liquid leaving the last tray falls down and is collected in the sump of the column. Above the liquid level there is a vapor inlet nozzle. Usually, no vapor inlet devices are used in tray columns, because the bottom tray generates a large enough pressure drop to ensure a good initial distribution of vapor.

In addition to two vapor and two liquid feed lines, Figure 1.1 shows also two manholes, that is, entrances to the inside of the column for installation during construction and inspection during shutdown. In the case of packed columns, as indicated here, manholes are always placed at the level of liquid distributors. The liquid distributor (2) shown schematically in Figure 1.1 is a narrow trough type with baffles on both sides that receive and spread the liquid jets coming from the equidistantly arranged orifices in the side walls of the troughs. Detailed drawings and photographs and related performance characteristics of devices shown schematically in Figure 1.1 can be found together with all other devices belonging to Sulzer-Chemtech separations column portfolio on the website (www.sulzer.com). Similar information and company-specific or proprietary designs can be found on the websites of other well-established distillation equipment manufacturers, i.e. Koch-Glitsch (www.koch-glitsch.com), Julius Montz (www.montz.de), and Raschig (www.raschig.com).

FIGURE 1.1   A Computer-Aided Drawing Indicating the Main Types of Vapor–Liquid Contacting Devices and Auxiliary Equipment Encountered in Distillation (For color version of this figure, the reader is referred to the online version of this book.) (Copyright Sulzer Technical Review, Sulzer Management Ltd, Winterthur, Switzerland)

As indicated above, the trays as well as random packings and structured packings with auxiliary equipment represent three essential types of vapor–liquid contacting devices used in distillation operations. Typically distillation columns are equipped either with trays, random packings, or structured packings, but if appropriate, a distillation column can contain each combination of these or even all three of them.

1.1.2. Methods and main features of distillation equipment operation

In a distillation column, the liquid enters at the top, as reflux, and somewhere along the column as feed, and descends driven by gravity, experiencing more or less pronounced resistance caused by ascending vapor. The main purpose of distillation equipment is to establish an intimate contact between ascending vapor and descending liquid, by creating a large, intensively refreshed interfacial area. The flow pattern and relative orientation of phases during contact depend on the type of the vapor–liquid contactor.

In a tray column the ascending vapor and descending liquid are contacted stagewise, that is, by repeatedly contacting and disengaging two countercurrently flowing phases over and over again under cross-current conditions. Namely, the liquid coming from inlet downcomer flows horizontally across perforated plates (tray decks) and pours over the outlet weir into the outlet downcomer, moving to the tray below, while the vapor flowing upwardly is forced to pass through perforations in the tray deck and a shallow pool of moving liquid a number of times. The interface, being the surface area of bubbles and/or droplets, is created to an extent depending mainly on operating conditions, that is, the governing flow regime and surface tension in conjunction with chosen tray design. Considering the fact that vapor and liquid brought into an intimate contact on a tray usually leave the tray before reaching equilibrium, the number of actual trays should normally exceed the number of equilibrium stages or theoretical plates required to achieve specified separation at given reflux ratio. Therefore, it is a common practice to consider performance of an actual stage or plate or tray in the terms of the deviation from ideal, e.g. to define the overall tray efficiency per column section as the ratio of the number of equilibrium stages to the number of actual stages (trays or plates) contained in that section. The resulting column height will depend on the tray spacing chosen, which can differ per section if appropriate. Namely, feed point or stage separates a conventional distillation column into an upper (rectification) section and a lower (stripping) section, which, depending on thermal conditions and/or the nature of feed mixture, can differ significantly in operating conditions and consequently in performance of the internals involved.

In a packed column, mass transfer occurs continuously by countercurrent flow of the liquid and vapor, and the efficiency is commonly expressed as the bed height generating composition change equivalent to that of a theoretical plate (HETP). If the HETP is known, then packed bed height required is simply the product of HETP and the number of theoretical plates (equilibrium stages) required for separation at given conditions.

Nevertheless this is not as simple as it appears. Namely, packing serves as carrier for liquid, and the surface of the liquid film provides interfacial area for mass transfer. Complete wetting is a prerequisite for successful operation. To assure this, a well-performing liquid distributor is required to provide adequate quality of initial liquid distribution, while the quality of liquid distribution within the packed bed will depend on type and size of packing, layout of a layer consisting of segments, operating conditions, and surface tension.

However, due to the efficiency-deteriorating effect of liquid maldistribution, which tends to develop with increasing bed depth, the height of a packed bed is usually limited to a height equivalent to a certain number of theoretical plates, 15 being a typical number. The liquid leaving a bed of given height needs to be collected and thoroughly mixed before being delivered to the distributor of the bed below. The column height required to install a liquid redistribution section is up to 2  m, which means that in case of multistage separations ancillary equipment will contribute significantly to total column height and cost. This is in practice considered to be a good reason to avoid a packed column in a new design, while the manufacturers have often been forced in revamp situations to install taller than usual beds, to ensure that liquid redistribution sections can be accessed through existing manholes. It is well known that this was done with success in numerous cases and that in industrial columns equipped with standard-size packings (220–250  m²/m³) there are well-performing beds of exceptional height (more than 20 stages and in excess of 10  m). With this, the outgoing assumption that maximum bed height extended by 2 to 3  m can add, say, three to four stages as well as the height necessary to compensate for anticipated loss in efficiency, was justified. However, this should not be done at the cost of mechanical integrity of the bed; it will depend on the type and size of packing as well as the construction material.

The extent of liquid maldistribution and consequently the allowable bed height will depend on the structure of the packed bed, which may be randomly or orderly packed. In other words, if considering a packed column, a clear distinction is made between random and structured packings. The former, often called dumped packings, are small, open bodies of various shapes and sizes that are dumped into the column (dry or wet, depending on situation) and settle randomly. Their liquid spreading extent is rather limited, that is, it does not exceed the dimension of the body. The structured packings are fabricated from corrugated sheets tightly packed to each other with corrugations of neighboring sheets oriented in opposite direction, forming a multiplicity of triangular flow channels crossing each other at an angle depending on the corrugation inclination angle (usually 45° or 60° with respect to horizontal axes). The height of a sheet metal packing element or packing layer is usually about 0.20  m (European manufacturers) or 0.25  m or more (American manufacturers), and overall size and weight of individual

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