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Separation and Purification Technology 80 (2011) 403–417

Contents lists available at ScienceDirect

Separation and Purification Technology


journal homepage: www.elsevier.com/locate/seppur

Review

Dividing wall columns in chemical process industry: A review on current activities


Ömer Yildirim a, Anton A. Kiss b, Eugeny Y. Kenig a,⇑
a
University of Paderborn, Faculty of Mechanical Engineering, Chair of Fluid Process Engineering, Pohlweg 55, D-33098 Paderborn, Germany
b
AkzoNobel Research, Development and Innovation, Process Technology Expert Capability Group, Velperweg 76, 6824 BM, Arnhem, The Netherlands

a r t i c l e i n f o a b s t r a c t

Article history: In spite of being an energy intensive process, distillation remains the most important separation method
Received 13 January 2011 in the chemical process industry. Especially for the separation of mixtures with three or more compo-
Received in revised form 28 April 2011 nents, the total energy requirement and the capital cost are very high. In this respect, dividing wall col-
Accepted 7 May 2011
umns (DWCs) represent a very promising technology allowing a significant energy requirement
Available online 26 May 2011
reduction. This article reviews current industrial applications of DWCs and related research activities,
including column configuration, design, modelling and control issues. Furthermore, the application of
Keywords:
DWCs for azeotropic, extractive and reactive distillation is highlighted.
Dividing wall column
Distillation
Ó 2011 Elsevier B.V. All rights reserved.
Control
Azeotropic distillation
Extractive distillation
Reactive distillation

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 404
2. DWC configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 405
3. DWC control issues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 406
3.1. Degrees of freedom . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 406
3.2. DWC control structures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 407
3.2.1. Three-point control structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 407
3.2.2. Three-point control structure with alternative pairing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.3. Four-point control structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.4. Three-point control structure with nested loops . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.5. Performance control of prefractionator sub-system using the liquid split . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.6. Control structures based on inferential temperature measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.6.1. Controlling the temperature in the top of the prefractionator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.6.2. Controlling the temperature in the bottom of the prefractionator. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.7. Feedforward control to reject frequent measurable disturbances . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
3.2.8. Advanced control techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 409
3.3. Guidelines for DWC control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 409

Abbreviations: A-DWC, azeotropic dividing wall column; ACM, Aspen Custom


Modeller; CSTR, continuous stirred-tank reactor; DMC, dynamic matrix control;
DWC, dividing wall column; E-DWC, extractive dividing wall column; ETBE, ethyl-
tert-butyl-ether; EtOH, ethanol; GMC, generic model control; HETP, height
equivalent to a theoretical plate; HPNA, heavy poly nuclear aromatic; LQG,
linear-quadratic gaussian; LQR, linear-quadratic regulation; MIMO, multi-input
multi-output; MeOH, methanol; MPC, model predictive control; NMP, N-methyl
pyrolidine; PID, proportional integral derivative; PEP, Pacol Enhancement Process;
R-DWC, reactive dividing wall column; RBA, rate-based approach; SISO, single-
input single-output.
⇑ Corresponding author. Tel.: +49 (0) 5251 60 2408.
E-mail address: eugeny.kenig@upb.de (E.Y. Kenig).

1383-5866/$ - see front matter Ó 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.seppur.2011.05.009
404 Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417

4. Design and modelling of DWCs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 409


5. DWC applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 409
5.1. Separation of ternary mixtures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 410
5.2. Separation of mixtures with more than three components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 411
5.3. Reactive DWC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 412
5.4. Azeotropic DWC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 412
5.5. Extractive DWC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 413
5.6. Revamping to DWC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 414
6. Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415

Nomenclature

B bottoms rate b internal split ratio in DWC


D distillate rate
L reflux rate Subscripts
Q heat duty B bottom
R reflux ratio C condenser
S side stream rate D distillate
V vapour boilup rate L liquid
x mole fraction R reboiler
S side stream
Greek letters V vapour
a relative volatility

1. Introduction in the second column. The improvement of the thermal efficiency,


due to avoiding unnecessary mixing effects, leads to considerable
Process intensification represents a dominating trend in the energy savings of about 30% [3] compared to the direct or indirect
chemical process engineering, mostly due to increasing awareness sequences. Since only one reboiler and one condenser are used, the
of the society of limited energy resources [1]. Besides, the last capital costs are also reduced.
achievements in the process modelling as well as growing compu- Further integration and cost saving can be obtained, if these two
tational power and advanced numerical methods make process columns are integrated into one shell. This alternative to conven-
intensification possible. Amongst others, apparative process inte- tional columns is identified as a dividing wall column (DWC) and
gration shows a great potential. illustrated in Fig. 3 [4]. Due to the large number of design param-
For the separation of multicomponent mixtures, most often a eters, for many years, it has been virtually impossible to simulate,
sequence of distillation columns is applied. In case of three compo- design and built DWCs. The first industrial application of DWCs
nents, at least two columns are necessary, for instance, the direct was accomplished in 1985 by BASF SE [5]. Since then the number
and indirect sequence shown in Fig. 1. An energetically favourable of application of DWCs has increased rapidly to more than 100 in
alternative configuration is shown in Fig. 2. In this so-called Pet- 2010 [6]. According to Schultz et al. [3], the DWC will become a
lyuk configuration, the vapour and liquid streams leaving the first standard distillation tool in the next 50 years.
column are directly connected with the second column [2]. The A recent review by Dejanović et al. [7] gives a comprehensive
first column performs a sharp split between A (light boiling com- overview of DWCs, covering both the theoretical description and
ponent) and C (heavy boiling component), whereas the middle boi-
ler B is distributed naturally between the top and bottom products.
A further separation towards high-purity components takes place A

a b
A B A

ABC
1 2 B

ABC 1 2 ABC 1 2
BC
AB

C C B

Fig. 1. Direct (a) and indirect (b) sequence for separating a three-component C
mixture (ABC; A: light boiling component, B: middle boiling component, C: heavy
boiling component). Fig. 2. Petlyuk configuration.
Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417 405

a b c
Liquid split
A

Dividing wall

ABC B

Prefractionation
section
Main column

Vapour split Fig. 5. Different positions and shape of the dividing wall.

Fig. 3. Dividing wall column. a b

the patent area. The present paper can be considered as an exten-


sion to the review of Dejanović et al. [7], with the focus being put
on the specific industrial applications and control issues.

2. DWC configurations

For a three-component separation, two different DWC configu-


rations can be applied. The first type shown in Fig. 4a is patented
by Wright [8] and is more common. The dividing wall as well as
the feed and side draws are usually placed close to the middle of
the column [9]. The second configuration is shown in Fig. 4b and
c. The wall is located either at the lower or at the upper part of
the column. This configuration is patented by Monro [10] and first
applied in 2004 [11]. The column in Fig. 4b is referred to as split
Fig. 6. Dividing wall columns for the separation of four-component mixtures.
shell column with common overhead section and divided bottoms
section, while the column shown in Fig. 4c is named split shell
column with divided overhead section and common bottoms section [13]; the two middle-boiling products are accumulated at the right
[12]. Moreover, the wall can be shifted from the centre towards side of the dividing wall. According to Kaibel et al. [11], the config-
the column walls, as shown in Fig. 5a, and can have diagonal uration with only one wall is thermally inefficient, it can be im-
sections (Fig. 5b and c). proved by application of additional dividing walls, as shown in
DWCs can also be applied for the separation of more than three Fig. 6b. This configuration is referred to as Sargent arrangement
components. With increasing number of components, the number [14]. However, no industrial application has been reported so far.
of possible configurations grows. For this separation, the basic A further configuration shown in Fig. 7a is known as the Agrawal
DWC types applied for such separations are shown in Fig. 6. In
the configuration illustrated by Fig. 6a (reffered to as Kaibel col-
umn), the separation is performed in a shell with one dividing wall a b
ABCD
A

a b c
B

ABCD
C
I II III
B I II III

D
A D

Fig. 4. Basic types of dividing wall columns. Fig. 7. Agrawal arrangement for the separation of four components.
406 Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417

arrangement [15]. In this configuration, the feed enters the middle be assured that the packing material does not touch the column
partition of the DWC. This can easily be understood, if the DWC is walls. According to Kaibel et al. [11], this would result in excessive
seen from the top view (Fig. 7b). Further arrangements for the wall liquid flow and negatively affect the separation.
are also conceivable, for instance a configuration shown in Fig. 8. Recently, the non-welded wall technology has been developed
Recently Rong [16] has introduced a procedure allowing a quick in a cooperation of Julius Montz GmbH and BASF SE. Using unfixed
synthesis of three-products DWCs for a given separation task and walls, the column design becomes much simpler. Another advan-
has shown possible alternative configurations for the separation tage of non-welded dividing walls is a faster and more precise
of a four-component mixture (Fig. 9), but this study does not cover installation [11]. Other benefits include fewer manholes and lower
the configuration of the Kaibel column. weight, since the manufacturing requires less metal. The revamp-
A proper selection of column internals is necessary to achieve ing of conventional columns becomes faster, simpler and cheaper,
efficient heat and mass transfer and, hence, the required purity. too. After the first implementation of non-welded walls in mid
Dividing wall columns can be equipped with trays or with different 1990s, the number of DWCs delivered by Montz GmbH has in-
kinds of packings. Generally, the selection criteria for the optimal creased considerably and reached around 85 deliveries in 2009 [7].
column internals for DWCs are similar to those for conventional
distillation columns. In most industrially available DWCs, struc- 3. DWC control issues
tured packings are applied. BASF SE exclusively applies packed col-
umns; other companies, e.g. Koch Glitsch and CEPSA Refinery, The advantages of using DWCs for ternary separation are the
install trays [17]. The latest advances in trays and packings were main drivers for commercial implementation. However, there are
reported by Olujić et al. [18]. also major hurdles [6], for instance, the concern that the benefits
The wall construction is different for tray and packed columns. of DWCs are obtained at the cost of lack of controllability and con-
Generally, tray DWCs are easier to build and the dividing wall that sequently flexibility in operation.
is welded on the column can strengthen the shell stability. The Although much of the existing literature focuses on the control
construction of a packed DWC is more complex, the welding of of binary distillation columns, there are only a limited number of
the wall being especially difficult. During the installation, it must studies on the control of DWCs. Here we give a critical overview
of the most important DWC control studies up to date. It should
be mentioned that various authors have selected different ternary
chemical systems to be separated and have explored many control
structures. The selection and pairing of manipulated and controlled
variables – with different control objectives and different control
algorithms – vary from the classical proportional integral deriva-
tive (PID) to model predictive control (MPC). Some authors control
only two compositions, while others control three or even four
compositions. Several papers look at inferential temperature con-
trol instead of (or in combination with) composition control. Nev-
ertheless, the main conclusion is that DWCs have good
controllability properties, providing that an appropriate control
structure is implemented [19].

3.1. Degrees of freedom

The dividing-wall distillation system has seven degrees of free-


dom. Six degrees of freedom are usual for a distillation column
with side stream, namely: the condenser duty (QC), the product
Fig. 8. Top view of triangular wall structures.
rates (distillate D, side stream S, bottoms B), the reflux (L) and

A B B C A B C A B

ABCD
ABCD ABCD
C A

ABCD C

D D D D

A B B C A B
ABCD

ABCD
C A

ABCD C

D D D

Fig. 9. Possible DWC configurations for the separation of a four-component mixture according to the synthesis procedure of Rong [16].
Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417 407

the reboiler duty (QR) or, equivalently, the vapour boilup (V). These energy savings, but lack good controllability [20–22]. Rong and
variables can be also combined, for example, instead of the reflux Turunen [23] reported a reliable synthesis method, whereas
rate L the reflux ratio R = L/D could be manipulated. Gómez-Castro et al. [24] proposed a robust method for the design
The additional degree of freedom arises from the flow of liquid of distillation sequences with dividing walls and recommended an
between the two sections of the column: at the top of the divided- analysis of both thermodynamic and controllability properties.
wall section, the liquid coming down from the rectifying section Accordingly, it was concluded that the distillation arrangements
can be split, in a controlled manner, between the two sides of (e.g. DWC), other than conventional Petlyuk configurations, pre-
the wall by using a total liquid trap-out tray and sending part of sented the best values for condition number and minimum singu-
the total liquid to the prefractionator side and the rest to the side- lar value. As a result, good dynamic closed-loop performance could
stream side. Thus, this internal liquid split (bL) is available for con- be expected for these types of thermally coupled distillation sys-
trol purposes. At the bottom of the dividing wall section, the tems [24]. Moreover, it was found that thermally coupled distilla-
vapour flow is split in accordance with the hydrodynamic condi- tion systems (TCDS) are not only well controllable, but they
tions (above all, pressure drop and flow resistance). It is worth not- sometimes exhibit dynamic responses that are easier to manage
ing that the vapour split is fixed by the stage-reflux requirements than in the case of conventional distillation sequences [21,24,25].
consideration and it needs to be physically established during Recently, Kiss and Rewagad [26] performed a comparison of sev-
the design of the partitioned part of the column. Consequently, eral conventional control structures based on PID control loops
the cross-sectional area of each side is fixed by the physical loca- enhanced by using the liquid split as an additional manipulated
tion of the wall, and this is already set at the design stage. There- variable, thus implicitly achieving minimal energy requirements.
fore, it cannot be changed when the column is operated [7]; Their reported dynamic results show good DWC controllability,
moreover, the vapour split (bV) variable cannot be adjusted for relatively short settling times and low overshooting.
control purposes during the column operation. Table 1 gives an overview of the DWC control structures re-
Typically the distillate (D) and bottoms flow rates (B) are used ported so far in the open literature, while the next paragraphs pro-
to maintain liquid levels in the reflux drum and column base, vide a more detailed analysis of most important ones.
respectively. Moreover, the condenser duty QC controls the pres-
sure. Therefore, the four degrees of freedom left (L, S, QC, bL) can 3.2.1. Three-point control structure
be used to control four variables. It should be remarked that, in The simplest control structure that can be imagined is just an
some control structures, the roles of the flow rates D and B can extension of the control of a regular distillation column with a side
be exchanged with that of the flow rates R and QC, respectively. stream. This is known as the three-point control structure. The dis-
Ideally, the purities of all three product streams should be con- tillate purity (xD1) is controlled by manipulating the reflux rate
trolled: the amount of mid-boiler component in distillate and bot- (L), the sidestream purity (xS2) is controlled by manipulating the
tom streams (xD2 and xB2, respectively) and the amounts of light sidestream flow rate (S) and the bottom purity (xB3) is controlled
and heavy components in the side stream (xS1 and xS3). However, by manipulating the vapour boilup (V). The three-point structure
the last set of specifications is usually replaced by the purity of was suggested by Wolff and Skogestad [27]. They studied the sep-
the side stream (xS2), which means that one degree of freedom aration of an ethanol/propanol/butanol system in a configuration
can be used to achieve some other objective, as, for example, to with 40-tray main column and 20-tray prefractionator. The
minimise the energy requirements. authors analysed the controllability of the system by using linear
tools, concluding that the system is easy to control. Moreover, they
3.2. DWC control structures also performed dynamic simulations of the nonlinear model, show-
ing that the column handles well the disturbances and some set-
All the control structures described hereafter could use or make point changes. However, sometimes small changes in the purity
use of an additional optimisation loop that manipulates the liquid setpoints (for example xS2, from 0.994 to 0.996) cannot be handled,
split in order to control the heavy component composition at the changes of 100% in L and V being required. Although this does not
top of fractionator, and implicitly achieving minimisation of the appear to be a problem in a practical implementation, the authors
energy requirements. Many authors analysed the effect of mini- tried to find a solution by using the remaining available degree of
mising the energy requirements on the controllability properties freedom (bL), hence adding another point to the control structure.
of the system, because an optimal design might give the highest Note that the mole fraction xS2 does not define the composition of

Table 1
Overview of various DWC control structures.

DWC control structure Ternary system Reference

Three-point control structure Ethanol/propanol/butanol [27]


Four-point control structure
Three-point control structure with nested loops
Three-point control structure with nested loops Methanol/2-propanol/butanol [31]
Three-point control structure with alternative pairing Hypothetical system with constant relative volatilities: 1:2.15:4.65 [28–30]
Performance control of prefractionator sub-system using the liquid split Hypothetical system with constant relative volatilities: 1:2:4, Boiling points 100, 50, 0 °C [32,33]
Butanol/pentanol/hexanol
Control of the temperature in the top of the prefractionator Butanol/pentanol/hexanol [34]
Model Predictive Control (MPC)
Control of the temperature in the bottom of the prefractionator Ethanol/1-propanol/1-butanol [35]
Temperature-composition cascade
Null space method Hypothetical system with constant relative volatilities: 1:3:9 [38]
Self-optimising control
Feedforward control to reject frequent measurable disturbances Benzene/toluene/xylene [36]
Feedforward and differential temperature control loops Benzene/toluene/xylene [37]
LQG/LQR, higher order controllers based on H1 norm l-synthesis Benzene/toluene/xylene [39]
408 Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417

the side stream, as it can correspond to several levels of the con- the liquid split is used to control the level of the heavy impurity
centration of impurities xS1 and xS3. in the top of the prefractionator. Note that the mixture considered
for separation was a hypothetical constant relative volatility sys-
3.2.2. Three-point control structure with alternative pairing tem. The relative volatilities were assigned the values of 1, 2, 4,
Serra et al. [28–30] performed a comprehensive study concern- whereas the boiling points were 100, 50, 0 °C, respectively.
ing the operation and controllability of DWCs. They studied a
hypothetical system with constant relative volatilities (a = 1: 3.2.6. Control structures based on inferential temperature
2.15: 4.65). Different controllability indices were used to select measurements
the pairing in a three-point control structure. However, the liquid The control structures make use of controlling the temperature
split was not varied. The results showed that the best structure in the top or bottom of the prefractionator.
was the one previously introduced by Wolff and Skogestad [27].
Moreover, Serra et al. [28–30] compared the performance of the 3.2.6.1. Controlling the temperature in the top of the prefractiona-
PI control with Dynamic Matrix Control (DMC), revealing the better tor. Adrian et al. [34] reported experimental results concerning the
performance of the PI control and the limitations of the DMC. The control of a butanol/pentanol/hexanol system. Compared to the
authors also pointed out that the performance depends on the de- previous studies, temperature control was used instead of concen-
sign of the column, but did not elaborate further on this tration control. The location of the controlled temperatures in-
conclusion. cluded the top of the prefractionator, a point above the side draw
and the lower part of the column. It should also be remarked that
3.2.3. Four-point control structure the heat input was fixed. Model Predictive Control (MPC) was em-
In addition to the reflux, sidestream and boilup that control the ployed by a second control structure, where the heat input was
concentration of the main components in the product streams, the added for a total of four manipulated variables used to control
liquid split ratio bL can be added to the set of manipulated vari- three temperatures. The MPC controller showed better perfor-
ables with the goal of controlling the levels of both impurities in mance for disturbances, not only in the feed flowrate, but also in
the side stream. Wolff and Skogestad [27] tested this structure the feed composition. Nevertheless, the additional manipulated
with the separation of the same system as previously described. variable cast some doubt on the conclusion of Adrian et al. [34]
Both linear and nonlinear tools predicted difficult control. Beside that MPC alone is generally better than a multi-SISO control (i.e.
small gain from the manipulated variables toward the controlled multiple SISO loops).
variables, the steady state feasibility space shows regions where
no steady states exists. 3.2.6.2. Controlling the temperature in the bottom of the prefractio-
nator. Wang and Wong [35] studied a high-purity ethanol/1-pro-
3.2.4. Three-point control structure with nested loops panol/1-butanol column. Proportional-Integral-Derivative (PID)
Wolff and Skogestad [27] have switched the V – xB3 and S – xS2 algorithms and temperature control were used instead of composi-
loops to the alternative pairing V – xS2 and S – xB3. Although the lin- tion control. A temperature in the prefractionator and two temper-
ear controllability tool did not predict control difficulties, the atures in the main column were selected. The pairing was
structure proved unworkable under mild disturbances. The authors completely different than that previously proposed by Adrian
attributed this to the strong nonlinearity link between V and xS2. et al. [34]. A temperature in the bottom section of the prefractiona-
However, it should be stated that the loops V – xS2 and S – xB3 are tor was controlled by manipulating reboiler heat input, while a
nested: a change of the side stream flow rate is expected to affect, temperature in the rectifying section was controlled by manipulat-
first, the side stream purity xS2, and only later the bottom purity ing the reflux flow rate. Moreover, a temperature near the base of
xB3. Therefore, strong interactions between the loops are expected. the column was controlled by manipulating the sidestream flow
The same control structure was also considered by Mutalib and rate. The liquid split was again not manipulated. Stable control
Smith [31]. They presented a simulation study of the methanol/2- was achieved and products returned to their desired purity levels
propanol/butanol system. In contrast to the results of Wolff and for feed flow rate changes. However, large product purity devia-
Skogestad [27], it was found that the pairing V – xS2 and S – xB3 tions were reported for feed composition disturbances. The authors
worked well in the three-composition control structure. Moreover, recommended a temperature/composition cascade control struc-
they switched the reflux and distillate in the level and distillate- ture to solve this problem.
concentration loops. The performance comparison of the two con-
trol structures made for setpoint changes and feed disturbances 3.2.7. Feedforward control to reject frequent measurable disturbances
showed that the system is indeed controllable. Ling and Luyben [36] proposed to control the impurity levels in
the three product streams and one composition in the prefractio-
3.2.5. Performance control of prefractionator sub-system using the nator. This implicitly helps to achieve also the minimisation of
liquid split the energy requirements. The four manipulated variables are liquid
Halvorsen and Skogestad [32,33] formulated two key tasks that split, reflux flow rate, sidestream flow rate, and vapour boilup. This
should be achieved by the prefractionator when the whole system four-point control structure uses combined feedback and feedfor-
faces disturbances or setpoint changes are required: (1) keep the ward to account for feed flow disturbances. Dynamic simulations
heaviest component from going out to the top of the prefractiona- demonstrated the improved performance.
tor section, and (2) keep the lightest component from going out to In a more recent paper, Ling and Luyben [37] explored also the
the bottom of the prefractionator section. use of temperatures in order to avoid expensive and high-mainte-
A portion of the heaviest component that enters the rectifying nance composition analysers. Two types of temperature control
section will flow down through the sidestream side of the wall structures were studied. In the first one, three temperatures lo-
and it will adversely affect the purity of the liquid sidestream. Sim- cated in the main column and one temperature on the prefractio-
ilarly, a portion of the lightest component that goes out to the bot- nator side were used to adjust the four manipulated variables.
tom of the prefractionator section will flow up through the Feed flow rate disturbances are well handled with this structure,
sidestream section, mostly in the vapour phase, with a reduced ef- but product purities start to deviate significantly from their desired
fect on the composition of the liquid sidestream. Based on these values for feed composition changes greater than 10%. In the sec-
considerations, the authors added a fourth control loop in which ond control structure, four differential temperature control loops
Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417 409

were used. The performance is improved and disturbances of 20%


in the feed composition are well handled with only small devia-
tions in product purities. This second structure also handles large
changes in the column operating pressure.

3.2.8. Advanced control techniques


The null space method is a self-optimising control method that
selects the control variables as combinations of measurements
[38]. For the case of a Petlyuk distillation setup, this resulted into
the following candidate measurements: temperature at all stages
and all flow rates. Using the null space method, a subset of six mea-
surements was obtained, resulting in a practical implementation.
Van Diggelen et al. [39] applied more advanced controllers such
as Linear Quadratic Gaussian (LQG/LQR) control, Generic Model
Control (GMC) and higher order controllers based on H1 loop
shaping design procedure (LSDP) and the l-synthesis procedure. Fig. 10. Decomposition of DWCs into simple column sequences.
The controllers were applied to a DWC used in an industrial case
study – the ternary separation of benzene/toluene/xylene. The per-
formance was compared to several structures involving multi-loop called decomposition method developed by Triantafyllou and
PID controllers. Amongst the multi-loop PID strategies, the LSV Smith [41] simplifies the design problem. The existing DWC config-
(using reflux/side-stream/vapour for purity control) and DSV (dis- uration is replaced by a sequence of conventional distillation col-
tillate/side-stream/vapour) structures were the best, being able to umns. Possible decomposition variants are shown in Fig. 10.
handle persistent disturbances in reasonably short times. Obvi- For the initial design of a DWC, the shortcut method suggested
ously, shorter times means better control performance. These re- by Triantafyllou and Smith [41] can be applied. This method is
sults agree with those of Mutalib and Smith [31], although Wolff based on the equations introduced by Fenske, Underwood, Gilli-
and Skogestad [27] reported the lack of controllability for this con- land and Kirkbride. The calculations are relatively simple and can
trol structure- this was attributed to the nonlinearity of the re- be used for mixtures of any number of components [42]. Another
sponse from V towards xS2. While PI control structures were also simple method for the conceptual design of DWCs is suggested
able to control the DWC, significantly shorter settling times and by Halvorsen and Skogestad [43–45]. This method is based on a
faster control were achieved using multi-input multi-output graphical treatment of the minimum energy represented by nor-
(MIMO) controllers. malised vapour flow.
Meanwhile, Aspen Plus suggests a routine for the design of Pet-
3.3. Guidelines for DWC control lyuk configurations. The latter are thermodynamically equivalent
to a DWC if the heat transfer across the wall is neglected. Rangaiah
Kim et al. [40] recommended general guidelines and rules for et al. [46] developed a procedure for a quick design of DWCs using
the DWC design and standards for selecting control structures for AspenTech. This tool is based on the equilibrium stage model,
DWCs. These were used in a several studies, described previously. which assumes that the streams leaving a column segment (stage)
Hereby, the following rules can be recommended in order to select are in thermodynamic equilibrium. This is an idealised description
the appropriate control strategy for DWCs [19]: that requires experimental parameters, such as efficiency factors
for tray columns or HETP values for packed columns. A more con-
 Use the reflux and boilup to control the distillate and bottom sistent alternative is given by the rate-based approach that takes
compositions. the process kinetics and specifics of column internals directly into
 Use the sidestream flow rate to control the sidestream account. In this case, the rates of mass and heat transfer between
composition. the liquid and vapour phases are determined explicitly [47,48].
 Alternatively, use the distillate and bottoms flow rates for com- For the rate-based model, adequate correlations describing pres-
position control. sure drop, liquid hold-up, mass and heat transfer coefficients are
 Use the liquid split to control the amount of heavy component necessary.
leaving in the top of the prefractionator. The reader will find a detailed description of the modelling and
 Use (inferential) temperature measurements for controlling design methods of DWC in the review by Dejanović et al. [7].
DWCs.
 Use temperature – cascade loops.
5. DWC applications
 Combine feedback with feedforward control.
 Apply MPC and MIMO control strategies when single-input sin-
Dividing wall columns are applied for separation of mixtures
gle-output (SISO) loops are not sufficient.
with three and more components. Initially, they found application
for systems with low fractions of the light and heavy boiling com-
It is worthy of note that information about control structures for
ponents. Currently, DWCs are used for a broad spectrum of sys-
industrial applications described in the open literature is very
tems, e.g. hydrocarbons, alcohols, aldehydes, ketones, acetals,
scarce. It is thus desirable that column manufactures make such
amines and others [11].
information available.
Further, DWCs can be used to conduct azeotropic, extractive
and reactive distillation. Despite that the DWC technology prom-
4. Design and modelling of DWCs ises significant reduction in operating and capital cost, its indus-
trial applications are still limited. Moreover, the information on
An optimal design of a DWC requires adequate models and the particular application of DWCs is mostly scarce.
computer-based simulations. However, commercial process simu- Table 2 shows the number of implemented DWCs reported in
lators do not include particular subroutines for DWCs. The so- the literature. It can be seen that most of them (more than 116)
410 Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417

Table 2 technology was applied more than 116 times for the separation
Overview of industrial applications reported in the literature. of ternary mixtures. Most industrial columns are exploited by BASF
System Number SE (more than 70 units). Almost all these columns have been built
Ternary mixtures >116 by Montz GmbH; they are filled with packings. Information on the
Mixtures with more than three components 2 systems or on the specifics of these DWCs is not available. The
Reactive system – reader can find more information in the corresponding patents
Azeotropic system 1 which are summarised in the review published by Dejanović
Extractive system 2
Revamps 4
et al. [7]. Further, they have mentioned that, Bayer AG has recently
started employing DWC, too.
The world largest column with 107 m height is constructed by
are applied for the separation of three-component mixtures. In to-
Linde AG for Sasol in Johannesburg, South Africa. This tray column
tal, there exist more than 125 applications. In Fig. 11, the number
recovers hydrocarbons from the Fischer–Tropsch synthesis. Fur-
of industrial applications is plotted against the corresponding year.
thermore, Uhde has built two DWCs in Germany and Saudi Arabia
An exponential increase in the number over the years can be ob-
and applied an extractive DWC (cf. Section 5.5). Sumitomo Heavy
served. If this increase is assumed for the next five years, about
Industries and Kyowa Yuka designed six DWCs for undisclosed
350 DWCs can be expected by 2015.
companies (they refer to DWCs as ‘‘column in column’’). Further
constructors are Sulzer Chemtech Ltd. and Koch-Glitsch. Sulzer
5.1. Separation of ternary mixtures has installed more than 20 DWCs and Koch-Glitsch more than 10
[5].
The industrially available DWC applications for three-compo- In the last years, UOP has also built DWCs. One application is
nent mixtures are summarised in Table 3. Accordingly, the DWC realised for the optimisation of the process shown in Fig. 12. It con-
sists of a sequence of three reaction/separation units. A reagent A
and an inert I are fed to a reactor, where A reacts to B. Afterwards,
the heavy product B is separated from the mixture by distillation.
Number of industrial DWCs

Since the bottom products of all columns are similar, the separa-
100
tion of B can be carried out within one shell (Fig. 13).
The DWC is also applied for the UOP Pacol Enhancement Pro-
This study cess (PEP) shown in Fig. 14a. Fig. 14b shows the developed DWC
for the same separation problem. In this process, A is pentane, B
10 is benzene, C consists of C7 + olefins and D comprises C7 + aromat-
ics [3,12]. In order to prevent mixing of C and D, a novel trap tray is
applied and excessive B is added. According to Schultz et al. [12],
the DWC shown in Fig. 14b has found more than five applications
in industry. Energy savings of approximately 50% and capital sav-
1 ings of approximately 35% could be achieved compared to the
1985 1990 1995 2000 2005 2010 2015
Year two-column design (Fig. 14a).
It appears probable that most of the future implementations of
Fig. 11. Number of reported industrial DWCs over the years. the DWC technology will be realised in developing countries with

Table 3
Industrial applications of DWCs for ternary systems.

Company System Constructor and year Features Reference


BASF SE, diverse sites Mostly undisclosed Majority of the columns are built  More than 70 DWCs [75–77]
by Montz GmbH  Diameter 0,6–4 m
First commercial DWC in 1985  Operating pressure 2 mbar to 10 bar
Sasol Separation of hydrocarbons from Linde AG  World largest DWC [3,49]
Johannesburg, South Africa Fischer–Tropsch synthesis unit In 1999  Height 107 m
 Diameter 5 m
 Tray column
Veba Oel Ag, Separation of benzene from Uhde  170,000 mt/year feed capacity [3,69]
Münchs münster, Germany pyrolysis gasoline In 1999
Saudi Chevron Petrochemical Undisclosed Uhde  140,000 mt/year feed capacity [69]
Al Jubail, Saudi Arabia In 2000
ExxonMobil Benzene-toluene-xylene ExxonMobil  No data available [5]
Rotterdam, Netherland fractionation Was planned for 2008
Undisclosed Undisclosed Sumitomo Heavy Industries and  Six DWCs [78]
Kyowa Yuka  No data available
Undisclosed Separation of C7 + aromatics UOP  Five DWCs [3,12]
from  Trap tray
C7 + olefin/paraffin
Undisclosed Undisclosed reactive system UOP  Split shell column with two walls [12]
consisting of two reactive
components and an inert
component
Undisclosed Undisclosed Sulzer Chemtech Ltd.  20 DWCs [5]
 No data available
Undisclosed Undisclosed Koch Glitsch  10 DWCs [78]
 No data available
Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417 411

A, I A, I A, I

A, A, A,
I, I, I,
A, I Reaction B Reaction B Reaction B
Stage 1 Stage 2 Stage 3

B B B
B

Fig. 12. Multistage reaction/separation flow scheme with three distillation columns [12].

emerging markets (e.g. India, Brasil), rather than in countries with


Reaction established distillation networks.
Stage 2

5.2. Separation of mixtures with more than three components


A, A,
I I,
B There are only two applications of DWCs for the separation of
mixtures with more than three components (Table 4). According
A, I to Parkinson [49], in 2002 BASF SE started with the development
of DWCs separating quaternary mixtures. The columns are in-
tended to recover fine chemical intermediates. Another DWC for
A, A, the separation of mixtures with more than three components
I, I,
A, I Reaction B
was developed by UOP. In this process, a split shell column (shown
B Reaction
Stage 1 Stage 3 in Fig. 15) was introduced for the separation of two streams into
five components. The first stream was from a hydrocracking pro-
cess that contained different hydrocarbons, such as naphta, kero-
sene, diesel and oil. The second stream was from the reactor
section of a plant that contained heavy polynuclear aromatic
dividing walls (HPNA) and light components. This column was built at an undis-
closed company in the far east [5,12].
Recently, Dejanović et al. [50] have given a theoretical analysis
B of the DWC configurations shown in Fig. 6 and replaced a usual
three-column sequence. In their study, an aromatic mixture is used
Fig. 13. Multistage reaction/separation flow scheme with single split shell column
[12].
as a test system. The analysis shows that considerable energy and
cost savings can be achieved with the DWC technology.

(a) Two Column Design (b) PEP DWC


A,B
A A

A,B,C A,B,C

B
A.B,D

B,C

A.B,D
B

D B,C D

Fig. 14. PEP fractionation in a two column design (a) and in DWC (b) [3,12].
412 Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417

Table 4
Industrial applications of DWCs for mixtures with more than three components.

Company System Constructor and year Features Reference


BASF SE Recovery of four-component mixtures of fine chemical BASF SE/Montz GmbH  Single wall [49,76]
intermediates since 2002  Height 34 m
 Diameter 3.6 m
 Column works under deep vacuum
Undisclosed customer in the Integration of a product separator and an HPNA stripper Designed by UOP  5 product streams [5,12]
Far East

To naphtha stripper reactive distillation

To kerosene stripper

To diesel stripper

Mixture of Product
hydrocarbons fractionator

HPNA stripper feed distillation reactive


dividing wall column

dividing wall column

HPNA rich Fig. 16. Schematic showing the path from a distillation column to a reactive
Stream dividing wall column (grey area represents the reactive zone).

Recycle oil R-DWCs were also shown to yield considerable energy and cost
to reactor savings. Some other groups investigated R-DWCs using standard
routines available in commercial software tools, e.g. Aspen Plus.
Fig. 15. UOPs split shell column.
Experimental investigations of R-DWC configurations are still very
scarce [53,56,57].
The application of DWC for the separation of mixtures with The application and investigation of DWCs for reactive distilla-
more than three components is still very scarce. This is presumably tion processes is also very limited. This situation can be explained
because it is considered to be a more complex technology than for by the clear niche character of the R-DWC technology. In the mean-
three-component separations. However, due to the clear advanta- time, the DWC concept is rapidly evolving to become a standard
ges, we believe, that also for these systems, further DWC applica- distillation tool and, thus, further applications for reactive systems
tions can be expected, especially, as far as developing countries can be expected. Interestingly, R-DWC studies are rather popular
are concerned. as compared to other integrated DWC applications. This can be ex-
plained by the general interest to reactive distillation itself.

5.3. Reactive DWC


5.4. Azeotropic DWC
Reactive DWC (R-DWC) represents a combination of a reactor
and a separation unit in one DWC (Fig. 16). It is a highly integrated In some cases, it is difficult or impossible to separate two com-
operation which is already mentioned in some patents [51,52]. In ponents (A and B) by distillation, due to similar boiling points or
such columns, reactive systems with more than two products, due to the occurrence of an azeotropic point. In such cases different
non-reacting components or excessive reagents can be separated methods can help, e.g. pressure swing distillation or azeotropic dis-
[48]. tillation [58]. The latter process uses an additional component
Up to now, just very few industrial applications of R-DWC have (entrainer E) that forms an azeotrope with the components to be
been reported [53,54]. However, this process has been analysed separated [59,60]. Preferable are entrainers forming heterogeneous
theoretically (see Table 5). The first comprehensive papers on azeotropes, since they can be easily separated in a decanter [61].
R-DWC modelling were published by the group of Kenig By using a two-column sequence (shown in Fig. 17), a separation
[42,47,48,55]. They also introduced the name R-DWC into use. of an azeotropic mixture A-B can be realised. A detailed description
The modelling was realised with the rate-based approach and the of this process can be found in [62].
performance of R-DWCs was theoretically studied for different In principle, it is possible to combine azeotropic distillation
systems. The advantages of this integrated process, i.e. high con- with the DWC concept according to the scheme shown in Fig. 17.
version, selectivity and product purity were demonstrated. The Up to now, only few papers have been published in which
Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417 413

Table 5
Works published on reactive DWCs.

Reaction Simulation Reference


methanol + butanol + acetic acid M methyl acetate + butyl acetate + water Rate-based model / Aspen Custom Modeller [42,47,48,79]
dimethyl carbonate + ethanol M diethyl carbonate + methanol
methyl acetate + water M methanol + acetic acid
methyl acetate + water M methanol + acetic acid Aspen PlusÒ or PRO/II [80]
isoamylenes + ethanol M tertiary amyl ethyl ether Aspen DISTILTM, Aspen HYSYSTM, CSTR [81]
Isoamylenes are:
2-methyl butene-1 and 2-methyl butene-2
methyl acetate + water M methanol + acetic acid Aspen PlusÒ or PRO/II [56]
ethanol + acetic acid M ethyl acetate + water Aspen PlusÒ Aspen Dynamics [57,82]
reactive distillation with 10 species Aspen Plus RADFRAC [53]
TM
isobutane + ethanol M ethyl tertiary butyl ether (ETBE) Aspen HYSYS [83]
ethanol + acetic acid M ethyl acetate + water Aspen PlusÒ [84]
methanol + isobutylene M methyl tertiary butyl ether
ethanol + ethylene M ethoxyethanol

theoretical analysis of azeotropic DWCs (A-DWC) is presented. ity of one of the components, for instance of the heavy boiling com-
Midori et al. [63] simulated an A-DWC with Aspen Plus. The test ponent B, decreases. In this case, A can be withdrawn at the top of
system was the separation of ethanol and water using cyclohexane the first column, whereas S and B can be separated in a second col-
as entrainer. Briones-Ramírez et al. [64] also performed theoretical umn [59,61,65,66].
investigations using Aspen Plus. In their study, isopropanol-water– The two-column configuration can also be integrated into one
acetone and isopropanol-water–methanol were used as test sys- column. The integration scheme of an extractive DWC (E-DWC)
tems. Furthermore, they applied an optimisation procedure using is illustrated in Fig. 18. The mixture of A and B and the solvent S
a multiobjective genetic algorithm in order to find the optimal de- are fed to the E-DWC (Fig. 18, right). The heavy boiling product B
sign. The results of this study show that energy savings of up to interacts with S, which reduces the vapour pressure of B. The light
50% can be achieved using an A-DWC instead of a two-column se- boiling component A is obtained in the left part of the column. B
quence. Industrial application of the A-DWC technology was men- and S are separated in the right part of the column and S is fed back
tioned in the literature only once by Kaibel et al. [11], without any into the left part.
specific information. Table 6 shows the main industrial applications of E-DWCs. Uhde
applied the DWC technology for the Morphylane process, initially
5.5. Extractive DWC based on a two-column configuration for the recovery of benzene,
toluene or xylenes from various feed stocks [67,68]. The integrated
Azeotropic or narrow boiling mixtures (A, B) can also be sepa- column solution (Fig. 19) was applied in 2004 at the Arsol Aromat-
rated using extractive distillation. In this process, an additional ics GmbH (formerly Aral Aromatics) in Gelsenkirchen, with a feed
substance (solvent S), with a boiling point much higher than that capacity of 28,000 mt/year [69]. Another E-DWC was implemented
of A and B is added [58]. By adding this solvent the relative volatil- by BASF SE for the production of butadiene from a C-cut [7,9,70].

azeotropic distillation

azeotrop E-rich
phase

azeotrop

E-rich
A,B B-rich
phase
phase

B A A,B
B-rich
phase

B A

distillation azeotropic dividing wall column

dividing wall column

Fig. 17. Schematic showing the path from a distillation column to an azeotropic dividing wall column.
414 Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417

extractive distillation

A B
S

B,S

A,B
A B

B,S
A,B

distillation extractive dividing wall column

dividing wall column

Fig. 18. Schematic showing the path from a distillation column to an extractive dividing wall column.

Table 6
Industrial applications of E-DWCs.

Company System Constructor and Features Reference


year
Arsol Aromatics GmbH (formerly Aral Aromatics) Separation of toluene and non-aromatics Constructed by  28,000 mt/year feed capacity [5,67,69]
Gelsenkirchen, Germany with N-formyl-morpholine Uhde in 2004
BASF SE Crude butadiene from a crude C4 using BASF SE  Both trays and packings [17,70]
Ludwigshafen, Germany N-methyl-pyrrolidone (NMP) as solvent

The extraction/distillation part of the classic butadiene process is obtained. In their study, acetone-methanol–water was used as a
shown in Fig. 20 a. At BASF SE, this part of the plant was replaced test system and the simulations were carried out using Aspen Plus.
by the dividing wall technology shown in Fig. 20b [17,70]. Bravo-Bravo et al. [72] applied a stochastic multiobjective proce-
Although E-DWC has already found industrial application, only dure in order to find the optimal design for three different chemical
few studies have been published in the open literature. Midori systems. Ruffert and Olf [73] reported on the recent process devel-
et al. [71] investigated theoretically the application of E-DWCs opment at Bayer Technology Services with respect to the applica-
and the results revealed that energy savings about 36% could be tion of extractive distillation. For the separation of a mixture of
isomers, they applied a two-column extractive distillation technol-
ogy instead of the former crystallisation-based process. They also
mentioned the possibility of applying the DWC configuration.
According to the authors, this technology would have been pre-
ferred, if the process could be realised with new equipment.
Solvent

Nonaromatics 5.6. Revamping to DWC

Feed The revamping of conventional columns to DWCs is a relatively


straightforward opportunity to reduce the operating costs. Accord-
ing to Parkinson [5], the reduction of one column can save up to
30% of the energy costs and the revamping can pay back within
one or two years. Table 7 summarises retrofitted DWCs that are re-
ported in the literature. Koch-Glitsch and MW Kellogg are the only
Aromatics suppliers that performed retrofits. Koch-Glitsch converted two col-
umns of Exxon-Mobil Refineries to DWCs. For instance, the
revamping of the Fawley Refinery in England took 30 days, but
energy savings of up to 53% were achieved [5]. This revamp includ-
ing process and mechanical design is described in detail by Slade
et al. [74]. Another revamp by Koch-Glitsch was made for a CEPSA
refinery in Spain. The operating costs dropped by 40% comparing to
a conventional two-column system. In academia, the revamp of
Fig. 19. E-DWC by Uhde. conventional columns was analysed so far only by Rangaiah et al.
Ö. Yildirim et al. / Separation and Purification Technology 80 (2011) 403–417 415

(a) Extraction/distillation part of the (b) Application of the dividing wall technology
classic butadiene extraction process
Raffinate Raffinate

Crude
butadien

Lean
Crude solvent
Lean butadien
solvent Lean
solvent

Crude Rich
Crude Rich C4 solvent
C4 solvent

Fig. 20. Production of butadiene by BASF SE: classic extraction/distillation (a); dividing wall technology (b).

Table 7
Performed retrofits of conventional columns reported in the literature.

Company System Constructor and year Features Reference


ExxonMobil Fawley Refinery Recovers mixed xylenes from reformate Conversion by Koch-Glitsch  3.8/4.3 m diameter [5,74]
Southampton, England motor gasoline in 2005  Tray column
 Energy savings up to 53%
ExxonMobil Refinery Recovers mixed xylenes from reformate Conversion by Koch-Glitsch  Reduction of the operating cost [5]
Port Jerome, France motor gasoline up to 40%
CEPSA Refinery Separation of paraffins and isoparaffins Conversion by Koch-Glitsch  No data available [5]
Algeciras, Spain Production of Isohexane
BP (now BP Amoco) Petroleum Undisclosed Constructed by MW Kellogg  No data available [75]
refinery
Coryton, Great Britain

[46]. In this study, six industrially important three-component structured controllers, DB/LSV and LB/DSV are the best control
mixtures were chosen. For these systems, a two-column distilla- structures capable of handling persistent disturbances in reason-
tion configuration and a DWC were designed. According to the re- ably short times, with low overshooting.
sults, considerable energy and cost savings can be obtained using The DWCs are exploited for the separation of a broad spectrum
DWCs. of chemicals, e.g. hydrocarbons, alcohols, aldehydes, ketones, ace-
The design of revamped columns appears generally simpler as tals and amines. In principle, DWCs are realised in both tray and
compared to the design of new DWCs, due to the lower degree of packed columns. However, up to now, the majority have been con-
freedom. We may expect more columns revamped to DWCs in structed by Montz and used by BASF SE as packed columns. The
the future. However, it remains questionable whether their effi- details on the specific features of existing DWCs is mostly
ciency is superior to new DWCs. undisclosed. The DWCs are usually larger than common distillation
columns, their diameters reaching up to 5 m. For the separation of
mixtures with more than three components, only two industrial
6. Conclusions applications are reported.
The integration of the DWC concept with azeotropic, extractive
This paper provides a review on industrial DWC configurations and reactive distillation principles shows a remarkable reduction
including those with different dividing wall positions. For three- in terms of investment and operation costs. Currently, industrial
component separations, the dividing wall is usually located close applications exist only in the field of extractive distillation (BASF
to the geometrical centre of a column. With increasing number SE and UOP). The literature on azeotropic and extractive DWCs is
of components to be separated, the number of possible configura- scarce. A few investigations have been performed, both experimen-
tions also grows. Such systems reveal a higher order of complexity, tally and theoretically, for reactive DWCs. Some models have been
and, thus, more than one wall is required for an efficient separa- developed, but no industrial application is available yet.
tion. The influence of the wall location, however, has not been Compared to conventional distillation towers, DWCs are consid-
investigated sufficiently yet, especially for the cases with more erably more energy efficient and require less capital investments.
than one wall. The experimental and theoretical investigations of The recent rapid expansion of the DWC applications allows us to
quaternary and higher-order systems in DWCs with more than estimate that about 350 industrial applications could be expected
one wall represent an interesting topic for future research. by 2015.
In terms of control strategies available for DWCs, the overview
given here clearly shows that DWCs are not difficult to control pro-
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