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Distillation: Operation and Applications
Distillation: Operation and Applications
Distillation: Operation and Applications
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Distillation: Operation and Applications

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Distillation: Operation and Applications—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 applications.
  • 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
LanguageEnglish
Release dateJul 16, 2014
ISBN9780123868770
Distillation: Operation and Applications

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Distillation - Andrzej Gorak

Distillation

Operation and Applications

Editors

Andrzej Górak

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

Hartmut Schoenmakers

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

Table of Contents

Cover image

Title page

Copyright

Preface to the Distillation Collection

Preface to Distillation: Operation and Applications

List of Contributors

List of Symbols and Abbreviations

Chapter 1. Distillation Control

1.1. Introduction

1.2. Basic control issues

1.3. Choosing a control structure

1.4. Feed composition sensitivity analysis

1.5. High RR columns

1.6. Control tray selection

1.7. Controller tuning

1.8. Use of ratios and cascade control

1.9. More complex columns

1.10. Columns in a plant-wide environment

1.11. Conclusion

Chapter 2. Common Techniques for Distillation Troubleshooting

2.1. Causes of column malfunctions

Part A: Column troubleshooting: how to investigate

Part B: Column troubleshooting—the tools

Chapter 3. Column Performance Testing Procedures

3.1. Introduction

3.2. Existing test facilities

3.3. Definition and terminology

3.4. Test design and planning

3.5. Mode of operations

3.6. Test column and auxiliary equipment

3.7. Reflux heating

3.8. Test systems and physical properties

3.9. Preparing for installation

3.10. Packed column installation

3.11. Trayed column installation

3.12. Operation and measurements

3.13. Measurements

3.14. Test procedure

3.15. Data reduction

3.16. Experimental errors and test troubleshooting

3.17. Documentation and reporting

Chapter 4. Distillation in Refining

4.1. Scale of the operation

4.2. Refinery flow schemes

4.3. Crude oil characterization

4.4. Refinery crude and vacuum units

4.5. Basic principles of crude units

4.6. Crude vacuum units

4.7. Key factors affecting the fractionation quality

4.8. Column internals for refining applications

4.9. Hazards of pyrophoric scale

4.10. Other distillation units in refining

Chapter 5. Distillation of Bulk Chemicals

5.1. General industrial separations

5.2. Industrial distillation examples

5.3. Conclusion

Chapter 6. Air Distillation

6.1. Introduction

6.2. Process

6.3. Column internals

6.4. Conclusion

Chapter 7. Distillation of Specialty Chemicals

7.1. Introduction

7.2. Distillation at low liquid load

7.3. Reactive distillation

7.4. Fouling

7.5. Aqueous systems

7.6. Modeling, simulation, and scale-up: a conclusion

Chapter 8. Distillation in Bioprocessing

8.1. Introduction

8.2. White biotechnology and biobased processes

8.3. Red biotechnology

8.4. Conventional, hybrid and advanced nonreactive distillation processes

8.5. Conventional, hybrid and advanced reactive distillation processes

8.6. Discussion and outlook

Chapter 9. Special Distillation Applications

9.1. Short path distillation

9.2. HiGee distillation

9.3. Microdistillation

9.4. Membrane distillation

9.5. Microwave-assisted distillation

9.6. Conclusions

Chapter 10. New Separating Agents for Distillation

10.1. Introduction

10.2. Fundamentals

10.3. Solvent families

10.4. Separation examples

10.5. Conclusions

Index

Copyright

Academic Press is an imprint of Elsevier

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Notice

No responsibility is assumed by the publisher for any injury and/or damage to persons or property as a matter of products liability, negligence or otherwise, or from any use or operation of any methods, products, instructions or ideas contained in the material herein

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ISBN: 978-0-12-386876-3

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Bottom left and top right photographs on cover courtesy of FRI and J. Montz GmbH

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: Operation and Applications

This is the last of three books in a series covering all aspects of Distillation. This book on Operation and Applications provides an overview on all operational aspects and describes technologies in various application fields. It consists of 10 chapters of different authors. The approach to the content together with the choice of subjects and examples are the authors' choice but the book represents a comprehensive overview on the operational principles and the wide spread application range of distillation in general.

In Chapter 1 control and operation principles for columns including coupled mass and heat integrated configurations and plantwide control are described. The second chapter deals with column troobleshooting. Analysis of disturbances is introduced and methods to solve the problems are outlined. Strategies for understanding problems in connection with plant operation are given and special investigation techniques are explained in detail. Chapter 3 is on performance testing techniques for industrial scale columns with all types of internals. Instructions for running tests and procedures to evaluate the results are given.

The following four chapters describe in detail the configurations of distillation sequences used in different applications. The content of Chapter 4 is distillation in refining processes. Flowsheets of such processes are explained in detail and the improvement potentials even for well-established processes are shown including the choice of special and new column internals. Chapter 5 deals with distillation in bulk chemicals industry, in which columns of similar dimensions as in refining processes are used but physical properties of the separated components are quite different. Consequently new operational challanges like foaming, fouling, and design problems connected with column efficiencies arise. In Chapter 6 the aspects of distillation in small-scale plants for specialty chemicals that frequently need low-pressure conditions are discussed. Special aspects are low liquid loads in the columns, aqueous three phase systems, and reactions that may occur. In Chapter 7 very special application of air distillation is presented. The different process variants at the extreme conditions of pressure and temperature are explained and problems like maldistribution at the low liquid loads are adressed.

In the last part of the book future trends and developments are described. At first new distillation techniques like high-gravity equipment and microdistillation are shown in Chapter 8. Chapter 9 deals with application of distillation in biotechnology, especially with respect to the different demands connected with red, green, and white biotechnology. The last chapter explains the application of new separating agents like ionic liquids and hyperbranched polymers. Examples are given and the methods for thermodynamic description of these very special solvents are introduced.

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

Dr Hartmut Schoenmakers,     BASF (emeritus)

List of Contributors

Wolfgang Arlt,     University Erlangen-Nuremberg, Erlangen, Germany

Tony J. Cai,     Fractionation Research, Inc., Stillwater, OK, USA

Stuart Fraser,     Consultant. London, UK, Formerly Head of Separations Group, BP Oil

Henry Z. Kister,     Fluor Corporation, Aliso Viejo, CA, USA

Hendrik A. Kooijman,     Department of Chemical Engineering, Clarkson University, Potsdam, New York, USA

Koon Fung Lam,     Department of Chemical Engineering, UCL, London, UK

Philip Lutze,     Department of Biochemical and Chemical Engineering, Laboratory of Fluid Separations, TU Dortmund University, Dortmund, Germany

William L. Luyben,     Department of Chemical Engineering, Lehigh University, Bethlehem, PA, USA

Anton Moll,     Engineering Services, Linde Engineering Division, Pullach, Germany

Eva Sørensen,     Department of Chemical Engineering, UCL, London, UK

Daniel Sudhoff,     Department of Biochemical and Chemical Engineering, TU Dortmund University, Dortmund, Germany

Ross Taylor,     Department of Chemical Engineering, Clarkson University, Potsdam, New York, USA

Gerit Niggemann,     Evonik Industries AG, Hanau/Marl, Germany

Armin Rix,     Evonik Industries AG, Hanau/Marl, Germany

Ralf Meier,     Evonik Industries AG, Hanau/Marl, Germany

List of Symbols and Abbreviations

Latin Symbols

Greek Symbols

Subscripts

Abbreviations

Abbreviations of Chemical Compounds

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

Chapter 1

Distillation Control

William L. Luyben     Department of Chemical Engineering, Lehigh University, Bethlehem, PA, USA

Abstract

Effective control of the many distillation columns in a chemical, petroleum, or biochemical process is vital for the profitable operation of a plant. Initial separations of raw material feedstocks often are performed in distillation columns, and any variability in this initial operation will upset the entire plant. Final purifications of product streams often occur in distillation columns and therefore have a direct impact on product quality.

Distillation columns are typically major consumers of energy, so their efficient operation has a large impact on the bottom line economics. The column control system must be capable of minimizing energy consumption while simultaneously providing stable dynamic control of the unit.

Even a simple single-feed, two-product column presents a multivariable control problem with the unavoidable issues of loop interaction, controlled and manipulated variable pairing, and controller tuning. This chapter attempts to summarize briefly the problems with and approaches to developing effective control structures for a wide variety of distillation columns.

Keywords

Controller tuning; Control structure; Dual-end control; Distillation control; Energy efficiency; Single-end control

Chapter Outline

1.1 Introduction 2

1.2 Basic control issues 2

1.3 Choosing a control structure 4

1.3.1 Conventional vs on-demand control structure 4

1.3.2 Dual-end vs single-end control structures 4

1.3.2.1 Dual-end control structures 4

1.3.2.2 Single-end control structures 6

1.4 Feed composition sensitivity analysis 7

1.5 High RR columns 9

1.6 Control tray selection 11

1.7 Controller tuning 12

1.8 Use of ratios and cascade control 13

1.9 More complex columns 15

1.9.1 Partial condensers 16

1.9.1.1 All-vapor distillate 16

1.9.1.2 Liquid and vapor distillate flowrates 17

1.9.2 Ternary sidestream column 17

1.9.3 Sidestream column with stripper 21

1.9.4 Sidestream column with rectifier 22

1.9.5 Sidestream column with prefractionator 23

1.9.6 Divided wall (Petlyuk) column 24

1.9.7 Heat-integrated columns 24

1.9.8 Extractive distillation process 28

1.9.9 Heterogeneous azeotropic distillation process 29

1.9.10 Superfractionator control 31

1.10 Columns in a plant-wide environment 32

1.11 Conclusion 34

References 35

1.1. Introduction

Distillation control has been the subject of dozens of books and thousands of papers over the past half century. No other unit operation has received as much attention by both academic and industrial workers. A complete listing of all these references is impractical and of limited utility. A list of books that deal explicitly with distillation control is given in the Reference section [1–6]. The earliest reference dates back almost four decades [1], and the latest was published in 2013 [6].

Distillation columns come in many flavors, and no one control structure fits all columns. Differences in feed compositions, relative volatilities, product purities, and energy costs impact the selection of the best control structure for a given column in a given plant.

1.2. Basic control issues

Let us consider a plain vanilla distillation column with a single feed stream that produces a distillate product from a total condenser/reflux drum and a bottom product from a partial reboiler in the column base. Figure 1.1 sketches the flowsheet and gives the nomenclature used in this chapter. All flow rates are molar and all compositions are molar fractions. If the feed stream is set by an upstream unit, there are five control valves in this process (distillate, reflux, cooling water, reboiler steam, and bottoms), each of which must somehow be set. Thus the system is inherently a 5  ×  5 multivariable process. There are five-factorial possible combinations of variable pairings (120 possible control structures).

FIGURE 1.1   Flowsheet of a Basic Distillation Column

There are three variables that must be controlled: pressure, liquid level in the reflux drum, and liquid level in the base. A typical control structure would control pressure with condenser cooling water, reflux drum level with distillate, and base level with bottom stream. This leaves two control degrees of freedom available to control two variables.

In the design of a column, the normal design specifications are the purities (or impurities) of the two products. The amount of heavy key component in the distillate and the amount of light key component in the bottom stream are normally specified. In theory, these same specifications should be used to control the operating column. This dual-composition control structure is used in some columns, usually when separations are difficult (low relative volatilities) and energy is expensive. It requires, of course, two on-line composition measurements, which are sometimes expensive, require high maintenance, and introduce significant deadtimes in the loop. As a result, the vast majority of columns use a more simple control structure in which the two remaining control degrees of freedom hold the temperature on a suitable tray and control the ratio of reflux-to-feed, or reflux ratio (RR).

From a fundamental standpoint, the two parameters that affect product purities are material balance and fractionation. Material balance refers to how the feed stream to the column is split between the distillate and the bottom stream. This is sometimes called the cut point or product split. In an extreme case in which 100% of the feed stream is taken overhead as the distillate product, the composition of the distillate will obviously be equal to the feed composition. No amount of reflux will affect the distillate composition. The same is true if the entire feed stream goes out the bottom. It is clear that the product split has a major effect on the compositions of the products.

By fractionation we mean the energy put into the column to provide the work of unmixing of the components. It can be measured in terms of the RR or steam-to-feed ratio. Obviously, if there is no reflux or no steam, there is no separation. The higher the RR the more difference there is between the purity of the distillate and the purity of the bottom stream. But this difference in purities tends to approach some asymptotic limit. Even with an infinite RR (total reflux), the difference in the product purities is set by the number of trays and the relative volatilities.

Thus it is important to realize that manipulating the material balance (distillate-to-feed ratio or bottom-to-feed ratio) has a greater impact on product compositions than manipulating the fractionation. The first law of distillation control states:

You cannot fix the flow rate of either product (for a fixed feed flow rate) and still control a temperature or composition in the column.

This law is a direct result of the fundamental concept of the dominant effect of the material balance on product compositions. Keep in mind that this manipulation of the material balance can be direct (using the distillate's flow rate to control a composition or temperature) or indirect (using the reflux flow rate for this purpose, with the distillate maintaining the reflux drum level). Both structures are manipulating the material balance (the distillate is being changed).

In the following sections, some typical control structures are discussed and the rationale for their use in particular situations is presented. Once the control structure is selected we still need to tune the controller. This subject will be discussed in a later section.

The software and hardware that permit the use of dynamic simulations to quantitatively assess the effectiveness of various alternative control structures are now available. They provide an efficient means of comparing control structures and tuning methods. Of equal or more importance is their use in assessing the controllability of alternative process configurations. Simulations are much less expensive and less time consuming than trying to extract this type of information from plant tests.

1.3. Choosing a control structure

There is no single control structure that applies to all distillation columns. The control objectives differ from column to column, just as the economics and process conditions differ from plant to plant. There are two basic choices of the type of control structure to be selected. First, the engineer must choose between a conventional control structure (in which the feed stream to the column is set by the upstream unit) or an on-demand control structure. Second, the engineer must choose between a dual-end control structure and a single-end control structure.

1.3.1. Conventional vs on-demand control structure

One fundamental difference in control structures is the selection of what variable sets the throughput. In most columns the feed stream comes from some upstream unit and typically uses a liquid-level control (if the feed stream is a liquid) or a pressure control (if the feed stream is a vapor). In this case the product streams from the column depend on the feed flow rate and composition. The simple control structure shown in Figure 1.2 illustrates this conventional case. Liquid levels in the column set product flow rates.

However, in some plants the flow rate of one of the products is set by a downstream user. Now the feed stream must be manipulated to satisfy the material balance. This is called an on-demand structure. Figure 1.3 gives an example of an on-demand structure in which the flow rate of the bottom stream is flow controlled (and set by a downstream consumer) and the feed stream comes in to control the base level.

1.3.2. Dual-end vs single-end control structures

1.3.2.1. Dual-end control structures

As previously discussed, the theoretically ideal control structure is dual composition. Figure 1.4 shows this ideal, but fairly infrequently used, structure. The bottom composition is controlled by manipulating the reboiler, and the distillate composition is controlled by manipulating the reflux flow rate. This scheme holds both products at their specifications and uses the minimum amount of energy for any feed flow rate and feed composition.

FIGURE 1.2 )

FIGURE 1.3 , reflux-to-feed ratio; TC, temperature controller.

FIGURE 1.4   Dual-Composition Control Structure The arrows indicate the composition controller (CC). FC, flow controller; FT, flow transmitter; LC, level controller; PC, pressure controller; SP, setpoint; TC, temperature controller.

However, it can present potential loop interaction problems because both reflux and vapor boil-up affect both product compositions. On-line composition measurements are often expensive, somewhat unreliable, require high maintenance, and introduce undesirable deadtimes in the loops.

It is sometimes possible to control two tray temperatures instead of two compositions, but this dual-temperature structure can be applied only when there are two locations in the column where temperatures accurately reflect compositions. Normally this means that there must be two temperature breaks in the temperature profile (temperature changes significantly from tray to tray). If there is only one temperature break, a dual-end control structure that controls one temperature and one composition can sometimes be used if indeed two-end control is required.

1.3.2.2. Single-end control structures

All dual-end control structures have the potential problems of loop interaction. It is often possible to use a more simple control structure that controls only one temperature or one composition.

We have already presented an example of this type of structure in Figure 1.2. An appropriate tray is selected whose temperature is controlled, usually by manipulating vapor boil-up. A later section addresses the issue of how we select this tray. Another feature in the structure shown in Figure 1.2 is the choice of a reflux-to-feed control structure. There are other alternatives that could be chosen. How do we know if the reflux-to-feed structure is the best? How do we decide if a single-end control structure will provide adequate control? One practical approach is to do a feed composition sensitivity analysis.

1.4. Feed composition sensitivity analysis

If the only disturbances that a distillation column has to contend with are changes in feed flow rate, a number of single-end control structures would be adequate to keep both the distillate and bottom products at their specified purities under steady-state conditions. Any control scheme that maintained any flow ratio (reflux-to-distillate or reflux-to-feed) and a single temperature (or composition) anywhere in the column would do the job.

One way to understand this concept is to remember that the McCabe–Thiele diagram is constructed using flow ratios. The tray compositions are the same for any feed flow rate. Therefore, simply keeping any ratio of flows constant as feed flow rate changes should give a steady-state condition with the same compositions throughout the column.

This principle applies only when feed composition does not change and there are no changes in pressures or tray efficiencies. In the face of feed composition disturbances, however, the composition profiles in the column will change if all we do is keep a constant flow ratio and a constant temperature on one tray. Product compositions will deviate from their specifications.

Our objective is to find a control structure that keeps the compositions of the two products at (or close to) their specified purities. How much will the column compositions change and how much must the flow ratios change as feed composition varies while keeping the two products at their specified purity?

To answer this question we perform a feed composition sensitivity analysis. A steady-state simulation of the column is used. We start at the design feed composition with the specified product purities and the design RR and reflux-to-feed ratio. The purities of both product streams are maintained at their specified values (in Aspen software this achieved using two Design Spec/Vary functions). The feed composition is varied over the expected range and the required changes in the ratios are examined.

Let us illustrate the method with a numerical example. A distillation column with a five-component hydrocarbon feed mixture has a feed of 100  kmol/h. At design conditions the feed composition is 1  mol% ethane (C2), 40  mol% propane (C3), 29  mol% isobutane (iC4), 29  mol% normal butane (nC4) and 1  mol% isopentane (iC5). The operating objective is to separate the light key component (propane) from the heavy key component (isobutane). Of course, the heavier-than-heavy key components nC4 and iC5 go out the bottom with the iC4. The lighter-than-light key component C2 goes out the top with the propane. Column pressure is set at 16 atm to give a reflux drum temperature of 320  K so that cooling water can be used in the condenser. The column has 37 stages and is fed on stage 18 (using Aspen notation with the reflux drum being stage 1). Distillate impurity is specified as 2  mol% iC4. The impurity of the bottom stream is specified as 1  mol% C3. The RR required to achieve these purities is 2.364 at the design feed composition. Table 1.1 give results of the feed composition sensitivity analysis.

These results clearly show that in this system the required changes in reflux are very small. Therefore, a single-end control structure with a reflux-to-feed ratio has a good chance of providing effective control of both product purities.

So, the procedure to see whether a dual-end control structure is required is as follows:

1. If only feed flow rate disturbances occur (a rare situation), dual-end control is not required. Simply use either a RR or a reflux-to-feed ratio scheme and control one temperature anywhere in the column. This is not exactly true because an operating column will experience pressure drop changes when throughput varies that affect the temperature–composition relationships.

2. If the feed composition sensitivity analysis shows large changes in both ratios (>5 to 10%), dual-end control is required. Structures that control two compositions, two temperatures, or one composition and one temperature should be used to handle feed composition disturbances.

3. If the feed composition sensitivity analysis shows that one of the two ratios does not change much (<5%), single-end control may be adequate to keep both products near their specified purities in the face of both feed flow rate and feed composition disturbances. The single-end control structure may be able to use a tray temperature, depending on the shape of the temperature profile, but in some cases composition control may be required. We discuss in a later section the issues of selecting an appropriate tray for temperature control.

The control structure shown in Figure 1.2 uses single-end control with a reflux-to-feed ratio. Suppose the feed composition sensitivity analysis indicated that an RR would be more effective. What would this control structure look like? Figure 1.5 shows a modified structure in which RR is controlled. Distillate flow rate is manipulated to control the reflux drum level. The distillate flow rate is measured and this signal is set to a multiplier whose other input is the desired RR. The output signal is the setpoint of the reflux flow controller.

Table 1.1

Feed Composition Sensitivity Results

FIGURE 1.5 , Arrow) FC, flow controller; FT, flow transmitter; LC, level controller; PC, pressure controller; SP, setpoint; TC, temperature controller.

There is another ratio that we have not mentioned: vapor boil-up-to-feed. In some columns this ratio is fairly constant as feed stream compositions vary. However, fixing this ratio precludes the use of reboiler heat input as a manipulated variable. Since vapor boil-up rates affect quite quickly all compositions and all temperatures throughout the column, reboiler heat input should usually be kept available for dynamic control performance.

1.5. High RR columns

The control structures shown in Figures 1.2 to 1.5 all control the reflux drum level by manipulating the distillate flow rate. This structure smooths the flow to downstream units and works well for a distillation column with low to moderate RRs. However, if the RR is large (>3), conventional distillation wisdom suggests that the reflux drum level should be controlled by manipulating the reflux flow rate. The flow rate of the reflux is much larger than the flow rate of the distillate. Small changes in the overhead vapor will produce large changes in the distillate if it is controlling the level.

Figure 1.6 shows a modified dual-composition control scheme in which the reflux drum level is controlled by the reflux flow rate. Distillate composition is then controlled by manipulating the distillate flow rate. In this setup, the level loop is nested inside the composition loop, that is, the level controller must be on automatic for the composition loop to work. And if the level loop is tuned for slow averaging control, the composition loop will be slow.

Figure 1.7 shows a more effective modified structure for columns with a high RR. The reflux drum level is still controlled by manipulating the reflux flow rate. But now the reflux flow rate is measured and this signal is sent to a multiplier. The other input to the multiplier is the required distillate-to-reflux ratio that is the controller output signal from the distillate composition controller. The output signal of the multiplier is the setpoint signal of distillate flow controller. Now changes in the overhead vapor flow rate produce changes in both the reflux and distillate flow rates. The composition controller trims up the ratio to drive the distillate composition to its specification since different ratios will be required for different feed stream compositions.

FIGURE 1.6   Dual-Composition Control (CC, Bottom Arrow) Structure for a Column with a Large Reflux Ratio CC, composition controller; FC, flow controller; FT, flow transmitter; LC, level controller (top arrow); PC, pressure controller.

FIGURE 1.7   Modified Dual-Composition Control (CC) Structure for a Column with a Large Reflux Ratio (Bottom Arrow) FC, flow controller; FT, flow transmitter; LC, level controller (top arrow); PC, pressure controller; SP, setpoint.

1.6. Control tray selection

Temperature depends on both pressure and composition in vapor–liquid systems. Column temperature profiles depend on relative volatilities, product purities, RRs, the number of trays, and pressures on the trays (which depend on tray pressure decreases and the pressure in the reflux drum). If relative volatilities are large, there will be large temperature differences from tray to tray in the regions of the column where compositions are changing rapidly. These trays are usually good locations to infer composition from temperature. If relative volatilities are small, the temperature profile will be flat and the use of temperature to infer composition may be ineffective.

Many methods for selecting an appropriate temperature control tray have been proposed in the literature. They vary from the simple (pick a tray where the temperatures are changing rapidly from tray to tray) to the complex (use singular value decomposition to detect the sensitive trays). A detailed discussion is beyond the scope of this chapter. The interested reader is referred to Ref. [6].

1.7. Controller tuning

In this section common controller types are considered, including the proportional, proportional-integral, and proportional-integral-derivative controllers.

If a single-end control structure is used, there is one temperature or one composition controller to be tuned. If a dual-end control structure is required, there are two interacting controllers to be tuned. We discuss these situations below.

Besides these temperature or composition controllers, there are three (or four) other controllers that must also be set up. Simple heuristics can usually be used in these loops. All level controllers (reflux drum and column base) should normally use proportional-only controllers (controller's proportional gain, KC  =  2) to smooth the flow and attenuate flow disturbances moving down the sequence of units in the series. Flow controllers can use KC  =  0.5 and an integral time constant τI  =  0.3 min because of their fast dynamics. Column pressure controllers (manipulating condenser cooling) do not have to provide tight pressure control and can use the nominal settings of KC  =  5 and τI  =  10  min in most situations. We only want to avoid rapid changes in pressure, which can cause flooding or dumping if vapor flow rates change rapidly because of liquid flashing when pressure decreases or vapor condensing when pressure increases.

The temperature and composition controllers require the use of an effective tuning procedure. One simple and practical method is to experimentally determine the dynamic characteristics of the loop using the relay feedback test. This test gives the ultimate gain (KU) and the ultimate period (PU), which can then be used to find controller constants from tuning rules such as Ziegler–Nichols or Tyreus–Luyben (see Table 1.2). The latter are more conservative and more suitable for distillation columns in which rapid changes in manipulated variables are undesirable because they can cause hydraulic problems on the trays (flooding or dumping).

It should be pointed out that running the relay feedback test on a real column works quite well. Running it on a computer simulation requires that the measurement lags and deadtimes that are inevitably present in a real column be explicitly included in the simulation. If this is not done, the relay feedback test will provide useless results since a system must have a phase angle that drops lower than −180° to have an ultimate gain. If these dynamic lags are not included, the performance of the loop predicted in the simulation may be unrealistically better than what will be experienced in the real column.

Table 1.2

Ziegler–Nichols and Tyreus–Luyben Tuning Rules

Deadtime elements can be used to approximate typical measurement dynamics. A 1-min deadtime is suitable for temperature measurements. Composition measurements are typically slower, particularly if gas chromatographic measurement devices are used. Deadtimes of 3–10  min are common.

The discussion above is applicable to a single control loop with no interaction from another loop. The method can be used directly in single-end control structures. But what do we do in the case of a dual-end structure? A more complex column configuration can have three or more interacting temperature or composition loops. How do we handle them?

There are several approaches to the problem; some are quite elegant and require detailed dynamic identification of all the interaction parameters. The most simple and practical approach is to use sequential tuning. The idea is to put all the interacting controllers on manual. In the dual-composition control structure there would be two composition controllers. First, we select the faster of the two loops. This is normally the loop using reboiler duty (steam) as the manipulated variable because vapor boil-up affects all temperatures and compositions more quickly than reflux.

The other controller is left on manual (fixed reflux). The faster controller is tuned using the relay feedback test and an appropriate tuning rule. Then the faster controller is kept on automatic while the slower controller is tested and tuned in the same way. The resulting tuning constants implicitly account for any loop interaction that exists in the system.

1.8. Use of ratios and cascade control

We have already demonstrated several control structures that use ratios. The ratios use multipliers to give the desired flow ratios to handle feed composition disturbances.

But there are other applications of ratios. One of the most important is to achieve feedforward control for improved dynamic load rejection. Consider the basic control structure shown in Figure 1.2. Suppose the feed flow rate is increased. The temperature controller can only respond to the resulting decrease in temperature when it sees this decrease. Therefore, there may be a large dynamic transient drop in temperature, which could result in a similar increase in the light key impurity that drops down into the bottoms.

But we know that more

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