i

PALLAVI KUMARI
Y9227397

A Thesis Submitted in Partial Fulfillment of the

Requirement for the

B. TECH – M. TECH DUAL DEGREE

Under the supervision of

DR. NITIN KAISTHA

CONTROL SYSTEM DESIGN FOR ENERGY EFFICIENT ON-

TARGET PRODUCT PURITY OPERATION OF A HIGH
PURITY PETLYUK COLUMN

DEPARTMENT OF CHEMICAL ENGINEERING

INDIAN INSTITUTE OF TECHNOLOGY KANPUR
MAY, 2014
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Acknowledgement
My first and sincere gratitude goes to my supervisor, Prof. Nitin Kaistha, for his
continuous supervision, invaluable insight and motivational encouragement at all stages
of this thesis. I have been enriched by not only his unsurpassed knowledge, objective
and principled approach to research method, but also I have learnt the vital skill of
disciplined critical thinking.

I am deeply thankful to my lab-mates Rahul, Ojasvi, Vivek, Abhishek and Harish for
creating a cheerful and constructive environment. Specifically I would comprehend my
thanks to Rahul for his immense patience with stimulating discussions and constant
motivation to complete the work and Ojasvi for his kind assistance and encouragement.

I would like to thank my family, especially my parents for always believing in me, for
their continuous love and their supports in my decisions.

Last but not least, I would like to thank my friends for their unconditional support,
efficacious remarks and constant encouragement throughout my degree. In particular, I
truly appreciate the patience and understanding shown by my wing-mates particularly
during the last year.

Pallavi
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Abstract
In this work, energy efficient, on-target product purity operation of a high-purity

three product benzene-toluene-xylene ternary Petlyuk column is studied. The basic

regulatory control system consists of four temperature inferential control loops with a

fixed prefractionator vapor to fresh feed ratio. An economic control system on top of the

regulatory layer adjusts these 5 setpoints. It consists of three product purity controllers

that adjust three temperature setpoints along with a reboiler duty reduction controller

that adjusts the remaining two free setpoints in the regulatory layer. The latter makes

these adjustments to prevent the downward curvature in the prefractionator and main

column middle section temperature profiles from being too large. Closed loop results

for large feed composition changes show significant energy savings (up to 15%) are

realized via temperature profile curvature control compared to column operation for

fixed xylene and benzene impurity mol fraction in the side-draw (constant setpoint

operation). The case study highlights the need for innovative control strategies for

realizing the sustainability benefit of the integrated complex Petlyuk column during

actual operation.

Keywords: Energy efficient operation, Petlyuk column, economic control, optimum

process operation
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Table of Contents

1. Introduction ............................................................................................................ 1

2. Petlyuk Column Optimum Design ......................................................................... 6

3. Control Structure Design ..................................................................................... 12

3.1. Regulatory Control Structure ............................................................................... 12

3.2. Control Structure for Economic Operation ......................................................... 17

3.2.1 Product Quality Control System................................................................... 18

3.2.2. Control System for Reboiler Duty Reduction ............................................. 21

4. Dynamic Simulations and Closed Loop Results.................................................. 30

4.1. Equipment Sizing and Plumbing ......................................................................... 30

4.2. Controller Tuning ................................................................................................ 30

4.3. Closed Loop Results ............................................................................................ 31

5. Discussion ............................................................................................................ 40

6. Conclusion ........................................................................................................... 42
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List of Figures

Figure 1. The ternary Petlyuk column configuration

(a) Conventional configuration (b) Dividing wall configuration

Figure 2. Petlyuk column design and optimized operating conditions

Figure 3. QR variation with VP for different values of xS,X

Figure 4. Petlyuk column base-case profiles (a) Temperature and (b) Composition

profile

Figure 5. Petlyuk column regulatory control structure

Figure 6. Petlyuk column tray temperature sensitivities

Figure 7. Quality control system on top of regulatory structure

Figure 8. Variation in steady state temperature profile with feed composition change for

CSCC operation at constant setpoints and reoptimized setpoints.

Figure 9. Quantifying curvature in a temperature profile

Figure 10. Mapping curvature (C) to large downward curvature (y)

Figure 11. TS1/TS5 curvatures for the different feed composition changes for fixed and

reoptimized VP/F and xS,X

Figure 12. Petlyuk column control system for QR reduction

Figure 13. CSR transient response to (a) throughput disturbance; (b) feed composition

disturbance

Figure 14. CSCC and CSEC transient response to benzene composition disturbance

Figure 15. CSCC and CSEC transient response to toluene composition disturbance

Figure 16. CSCC and CSEC transient response to xylene composition disturbance
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List of Tables

Table 1: Prefractionator bottom benzene composition variation for feed composition

disturbances with xD,T, xS,T, xB,T, VP and xS,T constant

Table 2: Comparison of QR and QRMIN for feed composition disturbances

Table 3: Controller tuning parameters for CSR, CSCC ans CSEC

Table 4: Purity of the three product streams for principal disturbances to CSR

Table 5: Comparison of QR for CSCC, CSEC, CSEC with only yC1 on manual and CSEC

with only yC5 on manual

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Chapter 1
1. Introduction

In the process industry, distillation remains the most preferred and widely used

unit operation for separating liquid mixtures into its constituent pure (pseudo)

components 1. The basic idea is to utilize the difference in the volatility of the mixture

components by repeated flashing to purify it. This is accomplished via countercurrent

vapour-liquid contact on the trays of a simple distillation column with the reboiler

providing the vapour stream into the bottom and the condenser providing refluxed

liquid to the top of the column. The process is then naturally energy intensive with the

reboiler heat driving the separation so that distillation alone can contribute up to 53% of
2
plant energy costs . Thus, innovations towards energy efficient distillation

configurations for a given separation task has traditionally been of interest to the

process industry. The volatility in energy prices in recent years has particularly renewed

interest in the synthesis, design, operation and control of complex column

configurations that can be significantly more energy efficient than a conventional light-

out-first (direct sequence) or heavy-out-first (indirect sequence) train of simple

distillation columns.
3
In pioneering work, Petlyuk et al. suggested a complex configuration

consisting of a prefractionator followed by a main column with a side draw for

separating a ternary ideal mixture into its constituent pure components, as in Figure

1(a). Compared to a conventional two-column direct or indirect sequence, the

prefractionator in the Petlyuk configuration mitigates remixing of the middle boiler,

which distributes itself between the prefractionator top and bottom products. This

reduces the inherent process irreversibility leading to potentially significant energy

savings. Literature reports (see e.g. Triantafyllou and Smith 4) indicate impressive
 2

energy savings up to 40% for a Petlyuk configuration over a conventional two-column

sequence. A further innovation to the Petlyuk configuration is incorporation of the

prefractionator within the body of the main column by inserting an appropriately

positioned vertical wall as in Figure 1(b). This is appropriately referred to as the divided

wall column (DWC). It is conceptually similar to the Petlyuk configuration with the

additional benefit of reduced capital cost. Literature reports suggest that BASF has

several (60-70) operating DWCs for improved energy efficiency 5.

Since Petlyuk’s original path-breaking article, researchers have used its basic
6-9
idea to develop other energy efficient complex column configurations . The reader is
10-12
referred to seminal work by Agarwal and co-workers for a generalized systematic

methodology to synthesize energy efficient complex column configurations for multi-

component mixtures.

The literature on complex distillation configurations suggests a mature

understanding of issues in their synthesis and design. Even so, the practical realization

of significant energy savings from such a configuration during actual process operation

requires a control strategy that ensures near minimum boil-up operation regardless of

disturbances, particularly in the feed composition. The available literature on minimum

energy / optimal operation and control of complex columns is however quite limited.

Most reported studies consider the operation of a ternary Petlyuk column with a

relatively impure side-product (see e.g. Kaibel et al. 13).

In possibly the earliest work on operation and control of a high-purity ternary

Petlyuk column, Wolff and Skogestad 14 performed a steady state bifurcation analysis to

suggest that only three product compositions should be controlled and the remaining

two dofs adjusted to minimize energy consumption. To keep the column operation near-
15
optimal, Halvorsen and Skogestad suggested holding appropriate feedback variables
 3

based on steady state analysis. The candidate variables for near-optimal operation

included position of maximum composition of intermediate component in main

fractionator, temperature profile symmetry on both sides of wall, heavy key impurity in

pre-fractionator top, impurity of non-keys in both ends of pre-fractionator, pre-

fractionator flow split and temperature difference over the pre-fractionator. In both these

articles, no closed loop dynamic results were presented so that the recommendations

remain dynamically untested.

In possibly the first article on high purity Petlyuk DWC control with closed loop
16
dynamic results, Ling and Luyben developed a control structure for a benzene-

toluene-xylene (BTX) column, where the principal impurity in the three product streams

are controlled along with the xylene spill-over from the prefractionator top. The work is
17
further extended to temperature inferential control of the BTX DWC , where

controlling the difference between appropriately chosen tray locations in the

prefractionator top, main column rectification section, middle section and stripping

section, is shown to provide near minimum energy column operation. A closer

examination of the closed loop results in both papers however shows that the side-draw

product (toluene) purity shows small deviations from its 99% purity target.

In a very recent paper, Dwivedi et al.18 comprehensively evaluated four

decentralized control structures with appropriate composition controllers for (near)

optimal operation of a ternary Petlyuk column and showed that overrides are needed to

mitigate excessive light component leakage down the prefractionator bottom for very

large feed composition changes. In their work too, the side draw product purity deviates

from its target value as the feed composition changes.

All of the high product purity ternary Petlyuk column control studies in the

literature thus allow the side-draw product purity to float away from its target value
 4

while pursuing minimum energy operation. The debatable question then is how to

control a high purity Petlyuk column for near optimal (minimum energy) operation with

on-target purity of all the three product streams. To the best of our knowledge, this has

not been studied in the extant literature and this work addresses the same. We highlight

that on-target product purity is crucial in today’s competitive markets, as overall

profitability is determined by value added product premium charged by the guarantee

of minimum product quality to the customer.

In the following, the benzene-toluene-xylene (BTX) Petyuk column design with

base-case optimum operating conditions is first described followed by a systematic

synthesis of the regulatory control system for closing the total

material/component/energy balances. We then develop the economic control system

consisting of the product quality control loops and temperature profile straightening

loops that adjust free regulatory layer setpoints for reboiler duty reduction. Closed loop

dynamic results are then presented to quantify the reboiler duty reduction benefit

compared to constant setpoint process operation. After a brief discussion of the results,

the article is concluded.

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(a) (b)

Figure 1. The ternary Petlyuk column configuration

(a) Conventional configuration (b) Dividing wall configuration
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Chapter 2
2. Petlyuk Column Optimum Design

The industrially significant ternary separation of benzene, toluene, and p-xylene

(BTX) in a Petlyuk column is studied here. Hysys with the SRK property package is

used for steady state and dynamic process modelling. We want to design a ternary

Petlyuk column, which contains 6 tray sections (TS1 – TS6) as in Figure 1, to process

100 kmol/h of equimolar BTX feed into 99 mol% pure constituents. The BTX normal

boiling points are, in order, 79.8, 109.8, and 137.8 °C, respectively. A condenser

pressure of 100 kPa is then considered appropriate giving a condenser temperature of

~80 °C (nearly pure benzene distillate) for a water cooled condenser.

At atmospheric pressure, the BTX relative volatility in order, is about

5.16:2.21:1 implying that the separation is not a difficult one. To design the column, we

must choose the number of trays in each of the six sections of the column, as in Figure

1. In the prefractionator, TS1 prevents p-xylene from leaking up the top in its vapour

product (VM). Similarly, TS2 prevents benzene from leaking down the bottom in its

liquid product (LM). In the main column, TS4 prevents the benzene in the

prefractionator top product from moving down and contaminating the side-draw toluene

product (S). Similarly, TS5 prevents the xylene from the prefractionator bottom product

from moving up and contaminating the side-draw. TS3 prevents toluene leakage up the

top in the benzene distillate product (D) and TS6 prevents toluene leakage down the

bottom xylene product (B).

To fix the number of trays in each of the tray sections, we note that a divided

wall arrangement requires the number of prefractionator trays to be equal to the number

of middle section (TS4 and TS5) trays in the main column. Since, the prefractionator

split is much easier (benzene-xylene split with large relative volatility of ~5) compared
 7

to the middle section splits for TS4 and TS5 (relative volatility 2.2-2.7), it follows that

TS4 and TS5 together set the prefractionator height. We then need to only obtain the

number of trays in the main column trays sections (TS3 – TS6). These are set to twice

the minimum trays necessary for achieving a principal impurity leakage of 1 mol% for

the particular tray section, which corresponds to a separation factor of ~500. This gives

11, 12, 12 and 11 trays for TS3, TS4, TS5 and TS6 respectively. The prefractionator

then has 24 trays. Trays for TS1 and TS2 are obtained similarly and 24 trays of

prefractionator are distributed in TS1 and TS2 in their ratio. Hence, the feed to the

prefractionator is chosen to be on 14th tray.

Figure 2 provides a schematic of the complex column along with the base-case

design and operating conditions optimized for minimum reboiler duty. A pressure drop

of 0.44 kPa per tray gives a bottom pressure of 120 kPa for a condenser pressure of 100

kPa. For the given feed and column pressure profile, the column steady state operating

degree of freedom (dof) is 5. The specification variables, toluene impurity in distillate

(xD,T), toluene purity of sidestream (xS,T), toluene impurity in bottom (xB,T), xylene

impurity in sidestream (xS,X) and vapour side draw to prefractionator (VP), are used to

exhaust the 5 dofs and robustly converge the flowsheet. Of these five specifications,

three get used up for fixing the three product purities at 99 mol% each. This is most

easily accomplished by setting xD,T = 1 mol%, xS,T = 99 mol% and xB,T = 1 mol%. The

remaining 2 specifications (xS,X and VP) are then manually adjusted to obtain the

minimum boil-up operating condition. This “brute-force” minimization of QR is shown

in Figure 3, which plots its variation with VP for different values of xS,X. A minimum

reboiler duty of 1619 kW is thus obtained for xS,X = 0.0092 and VP = 111 kmol/h. The

column temperature and composition profiles at this optimized base-case are shown in

Figure 4.
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Note that any xylene (heavy component) that spills over from the prefractionator top

necessarily moves down the main column and hence contaminates the side-draw. Similarly, any

benzene (light component) that spills over from the prefractionator bottom necessarily moves up

the main column and hence contaminates the toluene side product. Of these two spill-overs, as
16
insightfully pointed out by Ling and Luyben , heavy xylene would prefer the liquid phase

while light benzene would prefer the vapour phase. Since the toluene product stream is a liquid

side draw, the optimum impurity distribution in the toluene side draw is predominantly xylene

(0.92%) with some benzene (0.08%).

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Figure 2. Petlyuk column design and optimized operating conditions

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Figure 3. QR variation with VP for different values of xS,X

––:x
S,X = 0.0093; ––: x S,X = 0.0092; ––: xS,X = 0.0091; – –: xS,X = 0.0090
 11

(a)

(b)
Figure 4. Petlyuk column base-case profiles
(a) Temperature profile (b) Composition profile
in main fractionator (black lines) and in prefractionator (grey lines)

––: Benzene; – –: Toluene; –∙– : p-Xylene

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Chapter 3
3. Control Structure Design

The Petlyuk column has 8 control dofs (independent control valves), discounting

the feed valve, which is set by an upstream process or equivalently, sets the processing

rate / throughput (see Figure 5). These 8 control valves must be used to effectively close

the independent overall component, material and energy balances so that all

accumulation (total material, component or energy) terms are quickly driven to zero.

This constitutes the basic regulatory control system, in which typically, fast, cheap and

reliable process variables such as flows, levels, pressures and temperatures are

controlled using dynamically fast pairings for effective closure of the material/energy

balances. The regulatory loop setpoints determine the process inventory levels and the

corresponding steady state at which it eventually settles. These setpoints may further be

adjusted to drive the process to an economically favourable steady state. The much

slower economic/supervisory layer on top of the regulatory layer performs this

adjustment.

3.1. Regulatory Control Structure

In the Petlyuk column, the regulatory control objectives include controlling the

reflux drum and main column sump levels (1st-2nd objectives) to balance the respective

total liquid inventories. It is assumed that the liquid from the prefractionator drains

under gravity to the main column so that there is no control valve on LM. Also, the

column pressure must be controlled to balance the process total vapour inventory (3rd

objective). Further, on the prefractionator, the xylene and benzene leakage respectively,

up the top and down the bottom, must be regulated (4th and 5th objectives). Similarly, on

the main column, the toluene impurity in the distillate and the bottoms must be
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regulated (6th and 7th objectives). Finally, the side-product toluene purity must be

regulated (8th objective). These last 5 regulatory objectives (4th to 8th) correspond to

closing the independent component inventory balances on the prefractionator and the

main column. Instead of measuring composition, which is typically expensive, slow and

unreliable, we prefer to use temperature based measurements to infer the particular

component inventory.

Of the eight regulatory objectives, total liquid/vapour inventory regulation is

more important, as large drifts in the total inventory levels would necessarily lead to

safety issues such as an overflowing/dried-up surge drum or a ruptured disc due to high

pressure differential etc. Also, total inventory regulation indirectly regulates the

component inventories. We therefore pair loops for total inventory regulation first,

followed by loops for component inventory regulation.

To close the liquid and vapour inventory balances (first three objectives),

conventional “local” pairings are used. Thus, the reflux drum level is regulated by

manipulating the distillate (D), the main column sump level is regulated by

manipulating the bottoms (B) and the condenser pressure is regulated by manipulating

the condenser duty (QC).

With the total liquid balance controllers in place, we focus attention on

component inventory regulation. On the prefractionator, we have two independent

component balances. Of these, regulating the xylene spillover up the top is critical as

this sets the principal impurity level in the liquid side-draw product (xS,X). Accordingly,

a sensitive prefractionator enriching tray temperature is controlled for tight regulation of

the same. On the other hand, loose regulation of the benzene spillover down the bottom

may be acceptable as benzene prefers the vapour phase and is therefore the minor

impurity in the side-draw. Given that the prefractionator is highly overdesigned in terms
 14

of the number of trays for the easy benzene-xylene split, regulating the top xylene

spillover indirectly regulates the bottom benzene spillover. This may be inferred from

the steady state simulation results in Table 1, which show that even for large changes in

the feed composition (feed rate remains fixed at base-case value), the prefractionator

bottom benzene composition changes negligibly with xD,T, xS,T, xB,T, VP and xS,X chosen

as the 5 convenient column specifications and fixed at their respective base-case values.

Note that xS,X indirectly fixes the prefractionator top xylene spillover. The data in Table

1 suggests that at fixed feed rate, maintaining xS,X constant at constant VP provides tight

self-regulation of the benzene spillover down the bottom. Accordingly, we hold VP in

ratio with the fresh feed rate (F), the ratio being necessary for handling large throughput

changes. Maintaining a sensitive enriching section tray temperature and VP/F thus

closes the two independent component balances on the prefractionator.

On the main column, the three independent component balances to be regulated

correspond to toluene leakage in the distillate and the bottoms, and maintaining the

side-draw toluene purity. To accomplish the same, sensitive tray temperatures in the

enriching, middle and stripping sections are controlled by adjusting, respectively, the

reflux rate (R), side-draw rate (S) and reboiler duty (QR).

The basic regulatory control structure discussed above is schematically depicted

in Figure 5 and is labelled CSR for convenient reference. To obtain the sensitive control

tray temperature locations, sensitivity analysis with respect to the four manipulated

variables, namely, LP, R, S and QR is performed. Figure 6 plots the temperature

sensitivities. From the plot, prefractionator tray 7 (TP7), main column rectification

section tray 7 (TM7), middle section tray 33 (TM33) and stripping section tray 40 (TM40)

are candidate control tray locations. The Niederlinksi Index (NI) for the 3x3 main

column temperature control system however is close to zero implying unfavourable

 15

multivariable interaction. Subsequent dynamic simulations exhibited extreme difficulty

in getting the column to settle at a steady state with these four tray temperatures being

controlled. For a better NI, we choose to control tray 16 temperature (TM16) instead of

TM33, which gives a positive NI closer to 1. Note from the base-case temperature profile

(Figure 4), that TM16 is in the region where the temperature profile is still sharp. It is

then an appropriate location for sensing the movement of the separation zone due to

accumulation/depletion of toluene in the column middle section and adjusting the side-

draw rate for closing the toluene component balance.

Table 1. Variation in prefractionator bottom benzene

spill-over for feed composition disturbances
with xD,T, xS,T, xB,T, VP and xS,T constant
Disturbance (mol%) xB in LM
Base Case 0.0010
B 27 0.0015
B 39 0.0012
T 27 0.0009
T 39 0.0013
X 27 0.0013
X 39 0.0014
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Figure 5. Petlyuk column regulatory control structure

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TP Sensitivity to LP TM Sensitivity to R

TM Sensitivity to S TM Sensitivity to QR

Figure 6. Petlyuk column tray temperature sensitivities

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3.2. Control Structure for Economic Operation

The regulatory control structure CSR closes the material/energy balances and

drives the process to a steady state. Of the 8 regulatory layer setpoints, the liquid level

setpoints have only a transient effect and do not affect the final steady state at which the

process settles. We also assume the pressure controller setpoint is kept fixed at its

design value to avoid pressure compensation of temperature controller setpoints. The

SP
remaining five setpoints, namely, VP/F , TP7SP, TM7SP, TM16SP and TM40SP, then

determine the final steady state at which the process settles. It is desirable that this

steady state be such that the process profitability is maximized. This requires

appropriate adjustment of the regulatory setpoints, which is accomplished by the

economic control system.

For the Petlyuk column, the first and foremost economic operation requirement

is that the purity of the three products be on-target at 99 mol% each. These would

consume three regulatory layer setpoints leaving two free setpoints that may be further

adjusted to reduce / minimize the reboiler duty and hence the energy consumption per

kmol feed processed. The economic control system thus consists of the product quality

control system and the reboiler duty reduction control system. These are developed in

the following.

3.2.1 Product Quality Control System

On-target product quality control requires that the impurity leakage in the

product streams be tightly controlled. This is accomplished by cascade composition

controllers that manipulate appropriate regulatory layer temperature setpoints, as shown

in Figure 7. The distillate product composition controller adjusts TM7SP to maintain the

toluene impurity at 1 mol%. The distillate contains no xylene so that the distillate purity
 19

then is 99 mol% benzene. Similarly, the bottoms product composition controller adjusts

TM40SP to maintain its toluene impurity at 1 mol% for a 99 mol% pure xylene product.

The side-draw stream contains xylene as the principal impurity (0.92 mol%) with some

benzene impurity (0.08 mol%). For on-target 99% pure toluene side-draw, the most

convenient option is to maintain both the xylene and benzene impurities in the side-

draw at their base-case values. This is accomplished by a side draw xylene impurity

controller which adjusts TP7SP, and a toluene purity controller which adjusts TM16SP.

Note that adjusting TP7SP changes the prefractionator top xylene spillover, which

achieves tight control of the principal xylene impurity in the side draw. With the xylene

impurity controlled tightly, controlling the side-draw toluene purity is equivalent to

controlling its benzene impurity since xS,B = 1% - xS,X for xS,T = 99%. For convenience,

we have chosen to control xS,T instead of xS,B as then the toluene purity controller

setpoint, xS,TSP, remains constant at 99%, regardless of the choice of the xylene impurity

setpoint, xS,XSP.

The decentralized quality control structure on top of the regulatory control

system is shown in Figure 7, and is labelled CSCC for convenient reference. The

setpoints xD,TSP, xB,TSP, xS,TSP, xS,XSP and VP/F SP

correspond to the five steady state

operating dofs. Of these, the first three setpoints are fixed for on-target product quality.

The last two setpoints are then adjustable for reducing the reboiler duty (QR) towards

enhanced process energy efficiency.

We can operate the column using CSCC at fixed base-case optimum values for
SP
the two free setpoints, VP/F and xS,XSP. The control system should provide on-target

quality control regardless of changes in the feed composition. However, since the two

unconstrained setpoints are kept fixed post-disturbance and not re-optimized, QR is

likely to be sub-optimal, i.e. more than the minimum achievable reboiler duty (QRMIN)
 20

for the altered feed composition. To get a quantitative feel for the suboptimality in QR

with fixed setpoint operation, Table 2 compares QRMIN with QR for ~6 mol% feed

composition change in either direction for each component, with the other two

components remaining equimolar. The Table data suggests that the degree of QR

suboptimality depends strongly on the direction of the feed composition disturbance. It

is most severe when the benzene mol fraction in the feed increases from 33% to 39%,

for which QR is a significant 16% more than QRMIN. Less severe suboptimality with QR

being ~ 12% more than QRMIN, is observed for a toluene lean feed. For a xylene lean

feed, QR is about 8% more than QRMIN. For the other composition disturbances, the QR

increase over QRMIN is no more than 3%. This suggests that for particular feed

composition disturbances, fixed setpoint operation can result in significant energy

inefficiency. There then exists incentive to adjust the two unconstrained setpoints, xS,XSP

and VP/F SP to reduce QR towards QRMIN.

Table 2. Comparison of QR using CSCC and QRMIN for feed composition disturbances
Disturbance (mol%) QR QRMIN QR - QRMIN % suboptimality
B 39 1859 1600 259 16.19
B 27 1740 1690 50 2.95
T 39 1736 1704 32 1.88
T 27 1758 1576 182 11.55
X 39 1651 1615 36 2.23
X 27 1798 1664 134 8.05
 21

Figure 7. Quality control system on top of regulatory structure

3.2.2. Control System for Reboiler Duty Reduction

The conceptually simplest way of ensuring near minimum reboiler duty

operation is to adjust VP/FSP and/or xS,X to control appropriate process variable(s) that

remain invariant (or close to invariant) at the QRMIN solution. Luyben refers to such

control structures as eigenstructures 19 while Skogestad refers to them as self-optimizing

 22

15
. What constitutes such a process variable is however not straightforward. For the

present case, we avoid process variables that require tray composition measurements

and limit ourselves to appropriate combinations of tray temperatures. This is a

reasonable assumption as today’s columns are quite well instrumented with multiple

tray temperatures across the entire column being available, whereas composition

measurements remain cumbersome, expensive, unreliable and delayed.

To obtain the appropriate self-optimizing process variable(s), we compare the

column final steady state temperature profiles for the feed composition disturbances for

(a) fixed VP/F and xS,X and (b) VP/F and xS,X adjusted to minimize QR. In our

simulations, we found that the temperature profiles obtained in Hysys steady state mode

simulations and pressure-driven dynamic mode simulations were noticeably different.

This is likely because in the steady state mode, Hysys assumes a fixed column pressure

profile regardless of column internal flows, whereas in dynamics mode, the local tray

pressure drops vary with column internal flows. This variation in the column pressure

profile can cause the temperature profile to be different between the two modes. Since

we are interested in operating the column in dynamics, we compare the temperature

profiles obtained in dynamics mode and use differences between the optimal profile and

the profile for fixed setpoint operation to extract an appropriate temperature based

process variable for driving QR towards QRMIN.

Figure 8 compares the final optimum steady state temperature profiles of the

prefractionator enriching section (TS1) and the main column middle section below side-

draw (TS5) for the feed composition disturbances with the corresponding profile for

fixed VP/F and xS,X (i.e. no reoptimization of free setpoints). The base-case optimum

temperature profile is also shown for reference. All the optimum temperature profiles

are relatively straight and the QR suboptimality due to fixed VP/F and xS,X operation is
 23

most clearly visible in the large downward curvature of the temperature profiles. For the

case of a benzene rich feed, the TS5 temperature profile is curved significantly

downwards. For a benzene lean feed on the other hand, the TS1 profile curves

significantly downwards. A careful evaluation of the temperature profiles also shows

that at constant setpoint operation, a large downward curvature occurs in either TS1 or

TS5 for a toluene rich/lean feed and a xylene lean feed but not a xylene rich feed. This

then suggests that preventing downward curvature in the TS5/TS1 temperature profiles

by adjusting the two free setpoints should help drive QR towards QRMIN, for most of the

feed composition changes, including the most severe disturbance (in terms of degree of

suboptimality due to fixed setpoints) of a benzene rich feed.

We now need a convenient metric for TS1/TS5 temperature profile downward

curvature. The simplest method is to draw a straight line between two appropriate fixed

tray locations and obtain the curvature as the deviation of the actual profile around this

line. As shown in Figure 9, when the actual tray temperatures are all above / below the

straight line, the curvature magnitude would be large. On the other hand, in case some

of the actual temperatures are above and others below the straight line, cancellations

would occur and the curvature magnitude would be small.

More specifically, let TM and TN be the chosen lower and higher tray temperature

locations, respectively. Then, the straight-line interpolated temperature of the ith tray

above TM (i = 1 to N-M-1) is

ti = TM + i*(TN-TM)/(N-M+1)

The curvature (summed deviation) of the actual tray temperatures around this line then

is
 24

Since we want to make adjustments only when the profile moves significantly

downwards, i.e. the curvature becomes large negative, the process variable to be

controlled, y, is defined as

As shown in Figure 10, this ensures y is zero for positive or slightly negative (>-α)

curvatures. When we control y with ySP = 0, control action gets taken only when y

becomes large negative i.e. the temperature profile curves significantly downwards. The

parameter α may be used as a controller tuning parameter for enhanced reboiler duty

reduction while avoiding limit cycles due to the on-off switch inherent in the definition

of y.

We are interested in regulating the temperature profile downward curvature of

the prefractionator enriching section (TS1), yTS1, and middle section below side-draw

(TS5), yTS5. In this example, yTS1 is defined taking the tray immediately above the feed

tray as the lower tray (TM) and the prefractionator top tray as the higher tray (TN). For

the TS5 downward curvature, yTS5, TM is taken as tray 36 (middle section bottom tray)

and TN is taken as tray 29 (5 trays below side-draw). This choice of tray locations allows

for easier temperature profile curvature based distinction in the fresh feed composition.

This is evident from Figure 11, which plots the curvatures, CTS1 and CTS5 for the

different feed composition changes with fixed / reoptimized VP/F and xS,X. The large

negative curvatures in either CTS1 or CTS5 for fixed setpoint operation correlate to

changes in the feed composition (except a xylene rich feed). The absence of the large

negative curvature in the corresponding optimum profiles implies that curvature may be

used to infer suboptimality in QR and make appropriate adjustments in the available free

setpoints to drive the operation towards optimality (QRMIN).

 25

The QR reduction control system then consists of manipulating the two free

setpoints, VP/F and xS,X, to maintain yTS1 and yTS5. The straightforward decentralized

pairing is to maintain yTS1 by manipulating VP/F SP and regulate yTS5 by adjusting xS,XSP.

Since the xS,XSP controller is likely to be slow due to large lags associated with

composition measurements, a dynamic improvement is to let the yTS5 controller bypass

the xS,X controller and directly manipulate the prefractionator tray temperature controller

setpoint, TP7SP. This completes the overall control system with the regulatory control

loops, the quality control loops and the reboiler duty reduction loops. The full control

system for economic operation is shown in Figure 12 and labelled CSEC (economic

control) for convenient reference.

 26

Figure 8. Variation in steady state temperature profile with feed composition change for
CSCC operation at constant setpoints (dashed lines) and reoptimized setpoints (solid
lines).

–●–: Base case profile; Black : Composition increase; Grey: Composition decrease
TM Sensitivity to QR
 27

Figure 9. Quantifying curvature in a temperature profile

Figure 10. Mapping curvature (C) to large downward curvature (y)

 28

Figure 11. TS1/TS5 curvatures for the different feed composition changes for fixed and
reoptimized VP/F and xS,X
 29

Figure 12. Petlyuk column control system for QR reduction

 30

Chapter 4
4. Dynamic Simulations and Closed Loop Results
To test the proposed control system, a rigorous dynamic simulation is built in

Hysys and closed loop results are obtained for principal disturbances, namely large

changes in the fresh feed composition and a ±20% step change in the fresh feed rate

(throughput). Feed composition changes are tested for each component (B, T or X)

changing as a step from 33 mol% (base-case) to 39 mol% or 27 mol% with the other

two components remaining equimolar.

4.1. Equipment Sizing and Plumbing

The equipment are sized using heuristics to fix hold-ups and hence the

equipment dynamic time constants. The prefractionator and main-column inner

diameter (ID) are chosen for a 0.6 m/s maximum vapour superficial velocity assuming

20% coverage by the tray downcomers. The condenser and reboiler are sized for ~10

min liquid residence time at 50% level at the base-case conditions in Figure 2. For a

pressure driven simulation, the tray resistance to vapour flow is calculated at the base-

case steady state vapour flow – pressure profile and used. Appropriate plumbing (pumps

and valves) is provided on the distillate, side-draw and bottoms lines. Note that Hysys

allows direct setting of the reflux rate and the vapour/liquid rate to the prefractionator so

that no plumbing is configured on these lines.

4.2. Controller Tuning

After appropriate sizing / plumbing modifications for a pressure driven

simulation, the regulatory and economic layer controllers are installed and tuned. A 2

min lag is applied in all temperature loops to account for sensor dynamics. The

composition measurements have a 5 min delay and are sampled every 5 mins. The PI

pressure controller uses a large gain and small time constant for tight column pressure
 31

control. The two level controllers are P only with a gain of 2. The feed flow controller is

PI and tuned for a fast but non-oscillatory servo response. The four temperature

controllers are PI and tuned sequentially using the Hysys autotuner with further

refinement of the tuning for a slightly underdamped servo response. First, the

prefractionator temperature loop (TP7-LP) is tuned (all other temperature loops on

manual) followed by the main column loops in bottom-up sequence, i.e., TM40-QR, TM16-

S, TM7-R, in that order, with previously tuned loops on automatic. The composition

controllers are PI and tuned individually by first setting the reset time to approximately

the 2/3rd response completion time and the controller gain to the inverse of the process

gain. These tuning parameters are then further refined for a slightly underdamped servo

response. The two temperature profile downward curvature controllers (yTS1-VP/F and

yTS5-xS,X) are PI and tuned by hit-and-trial for a fast and not-too-oscillatory regulatory

response to the principal disturbances. The curvature offset, α, described previously, is

chosen based on Figure 8 so that the y for the optimal conditions map to 0. To avoid a

limit cycle due to the on-off non-linearity in the definition of y, the α for yTS1 is relaxed

a bit. The controller parameters of the salient loops used in this work are reported in

Table 3.

4.3. Closed Loop Results

Closed loop dynamic simulation results for the principal disturbances are now

presented and discussed. To better appreciate the incremental improvement by the use

of additional loops on top of the regulatory control system, results are presented for

each of the three control structures CSR, CSCC and CSEC.

Figure 13 plots the transient response of salient process variables to the

throughput and feed composition disturbances, obtained for the basic regulatory control

system, CSR. The response curves suggest that the four-point temperature inferential
 32

control structure, CSR, robustly handles the throughput/feed composition changes in

either direction with smooth changes in the manipulated process flow and the transient

response completing in about 6 h. Nonlinearity is evident in the response to feed

composition changes with the total change in QR and LP, which set the column internal

flows, exhibiting asymmetry.

Table 4 reports the purity of the three product streams for the principal

disturbances using CSR. Noticeable product purity deviations are evident for the feed

composition change disturbances. This is expected since a change in the feed

composition requires a readjustment in the prefractionator and middle-section split

requiring the temperature profiles to shift, as in Figure 8, which is prevented by holding

TP7 and TM16 constant. Quality deviations are also observed for throughput changes.

This is attributable to variability in the column pressure profile at the altered internal

flows so that the composition of the tray, whose temperature is controlled, is slightly

different implying a slightly altered split and hence product purity deviations. Since the

column top pressure is controlled, the effect is naturally more pronounced towards the

ends of the column, which show larger “local” tray pressure deviations. The product

purity controllers in CSCC and CSEC should appropriately adjust the temperature

setpoints for zero-offset in the product purities at the final steady state.

The transient response of CSCC and CSEC to benzene, toluene and xylene

composition step changes in the fresh feed is shown in Figure 14, Figure 15 and Figure

16 respectively. The solid and dashed lines correspond to CSCC and CSEC responses,

respectively, while the black and grey lines are for a composition increase and decrease,

respectively. In all cases, the response completes in about 20 hrs with the final total

impurity in each of the product streams settling at 1 mol% for on-target product purity

of 99 mol% each. The QR responses show that the final steady state QR using CSEC
 33

(dashed lines) is always less than CSCC implying that the temperature profile curvature

control helps improve the process energy efficiency. The savings in QR are particularly

significant for a benzene rich (Figure 14, black dashed line) and a toluene lean feed

(Figure 15, grey dashed line) with marginal savings for the other feed composition

changes. The transient responses also show that the curvature controllers, through their

manipulation of VP/FSP and TP7SP and the consequent nested action of the product purity

controllers, cause the appropriate “shift” in the prefractionator and middle section

temperature profiles for QR reduction. This is evident in the mostly large differences

between the final steady state TP7 and TM16 values for CSEC (dashed lines) and CSCC

(solid lines).

For a quantitative comparison of the energy savings by using the temperature

profile downward curvature controllers, Table 5 compares QR for CSCC, CSEC, CSEC

with the yTS1 (TS1 downward curvature) controller on manual (i.e. VP/F SP kept fixed at

base-case value) and CSEC with yTS5 (TS5 downward curvature) controller on manual

(i.e. xS,XSP is kept fixed at base-case value with xS,X controller manipulating TP7SP). The

quantitative data shows that the two curvature controllers together help significantly

reduce QR towards QRMIN for the benzene rich and toluene lean feed composition

disturbances with marginal improvement for the other feed composition disturbances.

The results also suggest that a substantial fraction of the QR reduction benefit can be

attained from only the yTS5 controller with the yTS1 controller achieving only marginal

improvements in QR. For the system studied, downward curvature in the temperature

profile of the middle tray section below side-draw product (TS5) thus appears to have a

more significant impact on QR reduction.

To explain the same, consider regulating only yTS5 by directly adjusting TP7SP

holding VP/FSP constant. A large negative yTS5 indicates substantial suboptimality in QR.
 34

To bring yTS5 back towards zero, the direct acting yTS5 controller would reduce TP7SP

which alters the prefractionator top xylene spillover and hence the side-draw purity. The

deviation in the side draw purity is detected by its purity controller, which would adjust

TM16SP. It is then expected that the final steady state at which the column settles would

have an altered impurity mix in the side-draw. Thus e.g., for the benzene rich feed

composition disturbance, at the final steady state with only yTS5 regulated, xS,X changes

from 0.92 mol% to 0.88 mol% (xS,X + xS,B = 1 mol% for 99 mol% pure toluene side

product). This re-adjustment of the product impurity distribution corresponds to QR

reducing from 1859 kW to 1652 kW, which is quite close the QRMIN value of 1600 kW.

Even as the absolute change in the benzene and toluene impurity mol fractions appears

small, the relative change in the impurity distribution is quite substantial with the

xS,B:xS,X ratio changing from 0.087 to 0.133. This then suggests that the side-product

impurity distribution (which is constrained by the side-product purity target) is a key

determinant of the reboiler energy consumption. Its proper adjustment with feed

composition is then critical towards energy efficient operation and any meaningful

control strategy must necessarily address the same to realize the energy efficiency

benefit of the complex column configuration, particularly when large changes in the

feed composition are expected.

 35

Table 3. Controller tuning parameters for CSR, CSCC and CSEC

Supervisory Layer
CV MV KC Ti (min) Set Point PV Span MV Span
CC EC CC EC
CS CS CS CS
xD,T TM7 0.2 0.25 60 60 0.01 0.0001-0.0200 77.3-107.3°C
xS,T TM16 0.11 0.2 90 90 0.99 0.9600-1.0000 96.5-126.5°C
xB,T TM40 0.1 0.15 60 60 0.01 0.0001-0.0200 119.5-149.5°C
xS,X TP7 0.12 - 90 - 0.0092 0.0001-0.0300 83.5-113.5°C
*
yTS1 VP/F - 0.05 - 75 0 -20 - +20 0-2.26
**
yTS5 TP7 - 0.1 - 35 0 -20 - +20 83.5-113.5°C
Regulatory Layer
TM7 R 2.5 30 94.6 77.3-107.3°C 0-225 kmol/h
TM16 S 3.5 70 115.2 96.5-126.5°C 0-66 kmol/h
TM40 QR 0.3 40 141.3 119.5-149.5°C 0-3333 kW
TP7 LP 1.4 20 101.3 83.5-113.5°C 0-75 kmol/h
*Reverse action; **Direct action

Table 4. Purity of the three product streams for principal disturbances to CSR
Disturbance (mol%) xD,B xS,T xB,X
B 27 0.9928 0.9869 0.9893
B 39 0.9859 0.9758 0.9910
T 27 0.9875 0.9866 0.9891
T 39 0.9916 0.9863 0.9909
X 27 0.9885 0.9831 0.9917
X 39 0.9912 0.9936 0.9882
F -20 0.9921 0.9961 0.9916
F +20 0.9885 0.9739 0.9879

Table 5. Comparison of QR for different operating strategies

CSEC: yTS1 CSEC: yTS5
CSCC CSEC
Disturbance manual manual
(mol%) % sub % sub % sub % sub
QR QR QR QR
optimality optimality optimality optimality
B 39 1859 16.2 1652 3.3 1652 3.3 1863 16.4
B 27 1740 3.0 1690 0.0 1740 3.0 1690 0.0
T 39 1736 1.9 1712 0.5 1736 1.9 1714 0.6
T 27 1758 11.5 1608 2.0 1608 2.0 1760 11.7
X 39 1651 2.2 1650 2.2 1650 2.2 1650 2.2
X 27 1798 8.1 1735 4.3 1735 4.3 1800 8.2
 36

(a)

(b)
Figure 13. CSR transient response to (a) throughput disturbance; (b) feed composition
disturbance

––: F +20%; ––: F -20%; ––: B 39 mol%; ––: B 27 mol%;

– –: T 39 mol%; – –: T 27 mol%; –∙–: X 39 mol%; –∙–: X 27 mol%
 37

Figure 14. CSCC and CSEC transient response to benzene composition disturbance

––: B 39 mol%; ––: B 27 mol%

 38

Figure 15. CSCC and CSEC transient response to toluene composition disturbance

––: T 39 mol%; ––: T27 mol%

 39

Figure 16. CSCC and CSEC transient response to xylene composition disturbance

––: X 39 mol%; ––: X 27 mol%

 40

Chapter 5
5. Discussion

Based on the results presented, some comments on the operability of a ternary

Petlyuk column vis-à-vis a conventional direct / indirect sequence are in order. The

basic argument in favour of a Petlyuk column is that an optimized design for a given

throughput and feed composition is significantly more energy efficient and less capital

intensive compared to an optimized direct/indirect sequence. The energy efficiency of

the optimized high-purity Petlyuk column design however deteriorates significantly (up

to 16% for the example case study), unless the two free setpoints (unconstrained dofs)

are readjusted to appropriately rebalance the prefractionator / middle section splits

towards minimum energy consumption. This rebalancing in an automated feedback

arrangement is, however, not a straightforward task. For the commonly applied constant

setpoint operating policy in the industry (CSCC for the studied example), the Petlyuk

column energy efficiency may then deteriorate significantly due to large feed

composition changes. Since the split rebalancing readjusts the impurity distribution in

the side-draw, the deterioration in energy efficiency may be mitigated if small

deviations in the side-draw product purity from its target are allowed i.e. the side draw

product purity is allowed to float. From the operational standpoint, it then stands to

reason that a high-purity Petlyuk column would be preferable over a conventional

distillation train when (a) large changes in the feed composition are not expected or (b)

relatively “loose” side-draw product purity control is acceptable. Alternatively, the

Petlyuk configuration may also be preferred when the side-draw product purity target is

not too stringent (e.g. 90 mol% pure instead of 99 mol%).

We note that the current study has considered a conventional Petlyuk column

where the liquid/vapour flow rate to the prefractionator is directly adjustable. In the
 41

DWC arrangement however, typically only the liquid split ratio (and not flowrate) is

adjustable with the vapour split ratio not being adjustable, as it is fixed by the dividing

wall partitioning of the column cross-sectional flow area. Control system design for

optimal operation with on-target product purity control of a DWC must then account for

the loss in a control dof. In particular, the feasibility of the desired product impurity

targets becomes an issue, which is also referred to as the black-hole problem 20. We are

currently researching control strategies for on-target product purity control with reboiler

duty reduction for the ternary Petlyuk DWC arrangement and hope to report the

findings shortly.

Lastly, we highlight the prefractionator and middle section temperature profiles

shift quite a bit for handling the feed-composition disturbances (see e.g. Figure 8). If the

product composition measurements are very infrequent (e.g. once a shift / day), the

composition based updates in the temperature setpoints would be very infrequent. The

column would then, in-effect, operate at constant temperature setpoints for prolonged

durations (until the next update). Holding a prefractionator/middle section tray

temperature constant necessarily prevents the respective profiles from shifting. This

would significantly degrade product purity and reboiler duty reduction control. In such

situations, we recommend the use of differential temperature difference in temperature

17 21
of two trays in a section or double differential temperature , instead of absolute

temperature, to infer the tray section splits to mitigate the economic control

performance degradation. We also highlight that differential temperature measurements

would also mitigate inadvertent changes in the tray section splits due to variability in

the column pressure profile.

 42

Chapter 6
6. Conclusion
In conclusion, this work has systematically developed and evaluated the

performance of a control system for energy efficient on-target product purity operation

of a high purity BTX Petlyuk column. Results show that four-point temperature control

at constant prefractionator vapour to fresh feed ratio provides effective column

regulation for large throughput and feed composition changes. The adjustment of these

temperature setpoints, as in CSCC, to maintain the four principal impurities (toluene in

distillate and bottoms; xylene and benzene in side-draw) in the product streams results

in significant energy inefficiency. For feed composition changes, the reboiler duty is

noticeably higher than the minimum duty possible with on target product purities. The

suboptimality is particularly severe (~16%) for a benzene rich feed. It is shown that

large downward curvature in the temperature profile of the prefractionator enriching

section and the middle section below side-draw can be used to infer the suboptimality.

By preventing large downward curvature in these profiles by manipulating the vapour to

the prefractionator and the prefractionator control tray temperature setpoint, as in CSEC,

the suboptimality is significantly mitigated. The worst-case reboiler energy

consumption penalty is then only 4,26% more than the minimum possible. The work

highlights the need for innovative control solutions for realizing the energy-efficiency

benefit of the ternary Petlyuk column for large disturbances.

 43

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