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ASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING

Asia-Pac. J. Chem. Eng. 2016; 11: 958972


Published online 5 September 2016 in Wiley Online Library
(wileyonlinelibrary.com) DOI: 10.1002/apj.2030

Research article
Side draw optimisation of a high-purity, multi-component
distillation column
Michael A. Kraller,1 Isuru A. Udugama,2 Robert Kirkpatrick,2 Wei Yu2* and Brent R. Young2
1
Chemical Engineering Department, Technical University of Munich, Munich, Germany
2
Chemical and Materials Engineering Department, The University of Auckland, Auckland, New Zealand

Received 23 February 2016; Revised 12 July 2016; Accepted 2 August 2016

ABSTRACT: Distillation columns with side draws are widely used in the process industry to rene crude methanol into
high-purity methanol. Historically, industrial methanol manufacturers have concentrated on meeting strict product
specications, while methanol yield and reboiler duty optimisation has often been neglected. In this work, a steady-state
model of an industrial high-purity multi-component methanol distillation column was developed using a commercial process
simulator. To achieve higher recovery at optimal reboiler duty, the side draw location and side draw mass ow rates were
identied as two important factors. It was determined that a combination of lowering the side draw location while reducing
the side draw mass ow rate will lead to the most optimal outcome. A design of experiment was also carried out to evaluate
the stability of the column at recovery rates of 97.7% (current recovery) and 99.5% (proposed high recovery). Disturbances
in the feed stream were identied as having the greatest effect, while the product purity was observed to become more
sensitive towards all disturbances when operating at an enhanced recovery. 2016 Curtin University of Technology and
John Wiley & Sons, Ltd.

KEYWORDS: high-purity distillation column; side draw optimisation; methanol distillation

INTRODUCTION and isobutanol is distilled into federal AA grade


methanol, which should consist of <10 ppm of ethanol.
The global demand for methanol has grown markedly Moreover, the bottoms discharge from the column is
over the past decade, nearly doubling from 40 million required to have <10 ppm of methanol to avoid costly
tons in 2004 to 70 million tons in 2013. This growth bio treatment. To separate this multi-component
is predicted to continue into the future with current mixture and to make high-purity products as well as
estimates for global demand in 2016 exceeding 90 bottoms discharge, these columns employ a side stream.
million tons.[1] To satisfy both this growing global In addition, the column is operated above a recovery
demand and demand from new emerging markets, rate of 97.7% for more prot. In the oil and gas industry,
methanol plants with capacities of up to 10 000 metric distillation operations can use up to 40% of total energy
tons per day (MTPD) are considered and planned.[2] consumption in a plant.[3] Given this, optimising the
In order for these proposed plants to meet the future columns energy consumption and product methanol
demand for methanol while still increasing the prot yield is of great economic importance for operators.
margins for methanol producers, they must operate at Optimising this distillation process is challenging
higher methanol recovery rates and in a more energy because the mixture is highly non-ideal and high
efcient manner than current plants. In this paper, we purities need to be achieved at both top and bottom of
will investigate applying recovery enhancement the column. In the past, methanol product recovery
optimisation to a high-purity methanol distillation and the energy input into the distillation column have
column with a side draw. The operation effects that often been overlooked in favour of meeting the strict
inherently come with this kind of optimisation, such as <10 ppm of product ethanol specication.
increased disturbance sensitivity, will also be explored. The subject of rening crude methanol into federal
In industrial methanol production, crude methanol AA grade specication (<10 ppm ethanol), ultra-high-
consisting of methanol, water and trace levels of ethanol purity methanol is very scarcely discussed in published
literature. Zhang et al.[4] look at a crude methanol
rening and the feasibility of employing multiple
*Correspondence to: Wei Yu, Chemical and Materials Engineering
Department, The University of Auckland, Auckland, New Zealand. methanol rening columns to reduce the overall energy
E-mail: w.yu@auckland.ac.nz demand of the process. However, they do not consider
2016 Curtin University of Technology and John Wiley & Sons, Ltd.
Curtin University is a trademark of Curtin University of Technology
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 959

industrial and economic factors and do not investigate out optimisation work on a distillation column design
distillation columns with side draws. Columns with a on a benzenetoluene separation. In another study of
side draw are more complex in design than simple Shahandeh et al.,[15] the same authors carried out an
distillation columns, as they have more design variables optimisation case study on a methanol/water binary
ascribed to additional degrees of freedom. These types separation, where ve heat pump-assisted distillation
of columns were initially designed by hand; this meant column schemes were rst optimised and then
that the number of trays required and the side stream compared with each other. In the study of Shahandeh
location and ow rate may not be the optimal condition. et al.,[14,15] the authors represented the column using
In 1985, Glinos and Malone[5] proposed equations and a a mathematical model. In the study of You et al.,[16]
design algorithm for side stream columns, which the authors modelled an extractive distillation process
allowed accurate estimations for the fundamental of acetonemethanol with water using an industrial
parameters of these type columns. These equations only process simulation and minimised the total energy
apply on ideal mixtures, as they are based on the classic consumption. In the study of Palmeira et al.,[17] the
equations introduced by Underwood.[6] Bausa and authors also use an industrial process simulation to
Watzdorf presented shortcut calculation methods for simulate and optimise a methanol-water-glycol system.
non-ideal mixtures with up to three or four However, the authors in this instance carried out a
components.[7,8] These methods were also capable of sensitivity analysis rather than a true optimisation study
being applied to side stream columns. Modern process in order to optimise the operations of the column. In the
simulators allow a column design and optimisation with study of Tian et al.,[18] the authors use an
much higher accuracy. Many methanol distillation experimentally backed mathematical model and plot
columns were built several decades ago, when the data in a viable operating range to nd the optimal feed
distillation design methods were not as advanced as stage and reboiler duty usage. Despite being in the
today. Because of this fact, it is potentially benecial general area of optimisation of distillation columns,
to more closely examine existing columns with modern these works lack one/more of the following aspects:
engineering tools, allowing for both the product
methanol yield, column energy input and, hence, the The columns do not include a side draw.
overall efciency of the column to be optimised. The columns do not require a higher purity at the top
Modelling industrial chemical processes allows for and bottom of the column.
the study and optimisation of existing, large-scale, The columns do not require high recovery rates.
industrial processes without the need for eld trials. A The operation of each of the columns is not limited
recent study successfully modelled the Fischer by industrial and economic considerations.
Tropsch process to examine how a novel type of a
reactor can improve key operational parameters.[9] In In contrast to the columns studied in these previous
another study, a kinetic model of a methanol to olen works, the industrial methanol columns studied in this
plant was developed and employed to optimise the paper have multi-component feeds (consisting of
operating conditions.[10] In both studies, an appreciable methanol, water and ethanol), include a side draw and
level of agreement between the computational models need to produce product methanol with <10 ppm of
and experimental data was achieved. Using process ethanol. On top of all this, the results proposed in this
models to optimise a columns operational parameters work are easily implementable in an industrial setting.
is cost efcient and time saving. These models also In this paper, we have modelled a real life methanol
contribute to the general understanding of the process distillation column in Aspen HYSYS to optimise the
and helps highlight areas of potential research interest. methanol recovery and energy efciency of the
Conversely, plant trials and small scale pilot plants, in process. Employing this model, we also carried out a
addition to being costly and time consuming, do not design of experiment, to analyse the stability of the
allow process engineers to explore the entire range of model and its sensitivity to disturbances. Through this,
operating scenarios because of safety concerns and conclusions on the feasibility of the increase in
other practical limitations. recovery were made.
A literature search on methanol distillation does, This paper is organised as follows. In the section
however, turn up a handful of papers that investigate immediately following this, the basic operating
the high-purity separation of a water/methanol binary principles of columns with side draws are discussed,
mixture. In the study of Luyben[11,12] and Sadgehi and key concepts are dened. In the next section,
and Ahangar,[13] the authors carry out process control industrial distillation processes are described, allowing
and optimisation work on this type binary methanol for the input parameters for the process simulator to be
distillation process using dynamic process simulations specied. Following this, a qualitative analysis of
as well as mathematical models. The optimisation of efcient yield enhancement and the optimisation of an
distillation units in general has also been long studied. industrial distillation column are performed. Next, a
In the study of Shahandeh et al.,[14] the authors carry description and evaluation of the experimental
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
960 M. A. KRALLER ET AL. Asia-Pacic Journal of Chemical Engineering

procedure is given. Subsequent to this, the stability and the primary separation between X1 and X2/X3/X4 takes
feasibility of operating the column at increased place, and in Model Description section, the secondary
recovery rates is discussed. Finally, a summary of the separation between X2 and X3/X4. Generally, the
most important results found concludes this paper. column can be considered as two separate columns
with two denable boil-up ratios for each hypothetical
column. The boil-up ratio at the top of the column for
DISTILLATION COLUMNS WITH SIDE DRAWS the primary separation is given by Equation [1]:

Distillation columns with side draws can be used to M_ W


separate any nonazeotropic multicomponent mixture ; (1)
into three (or more) product streams. The high energy M_ B M_ S
input for the primary (more difcult) separation is also
used to carry out the secondary separation in addition. and the boil-up ratio at the bottom of the column for the
The design of side stream distillation columns was secondary separation is give by Equation [2]:
analysed in detail by Glinos and Malone.[5]
A columns side stream can be placed either above or M_ V
: (2)
below the feed point location; on a similar note, the M_ B
side stream can be drawn as either a liquid or a vapour.
Within this work, the side stream is located below the In reality, the separations within the column are
feed tray and is drawn as a liquid. The side stream never as sharp as what is assumed herethere are
location was chosen on the basis that a high fractional always impurities in each of the different streams.
recovery and high purity of the light key component
need to be achieved in the column. The quality of the Degrees of freedom
side stream was chosen to lower the vapour rate and,
therefore, lower the operational costs of the column. To understand the difculties of designing and
A nonazeotropic quaternary mixture with the optimising side stream distillation columns, it is
components (X1/X2/X3/X4) is considered. The boiling important to analyse the degrees of freedom (DOF).
point increases from X1 to X4. For a simple distillation column with one feed, no side
Figure 1 shows that a column with a side stream is draws and the other column parameters (number of
effectively divided into three sections. In Introduction stages, the feed plate location, etc.) remaining xed,
and Distillation Columns with Side Draws sections, there are usually ve DOF that need to be controlled.
Because the pressure and holdups in the condenser
and reux drum are assumed to be constant at steady-
state operation, only two DOF need to be controlled
for a simple column.[19] The presence of a side draw
means an additional DOF needs to adjusted, making
the design and optimisation of the column considerably
more complicated. In total, there are three DOF that
need to be controlled with a single side draw column.
These are the following:
reboiler duty;
distillate ow rate; and
side draw ow rate.
The remaining ow rate (bottoms) is determined by
an overall mass balance around the entire column.
The three DOF are used to adjust the following column
outputs:
ethanol mass fraction at the top;
methanol mass fraction at the bottom; and
recovery.

Optimise energy input

Figure 1. Different sections of a distillation column with As for simple distillation columns, the energy input
side draw. of a side stream column is a function of the number
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 961

of trays of the distillation column. The optimum MODEL DESCRIPTION


operating point is always a compromise between
investment costs and operational costs. To minimise For the analysis and optimisation of the side draw of
the required energy input for a column, the ideal the high-purity distillation column, the process
feed plate location needs to be found, as an improper simulator Aspen HYSYS was used. The basis for the
feed location can reduce the performance of the steady-state model is the real life distillation unit
column. This ideal location is found where the employed by an industrial methanol producer. The feed
composition of the feed is identical to the enters at the middle of the column and consists of a 4:1
composition of the internal ows at that point within methanol to water mass ratio. The feed contains
the column. Thus, the composition gradient between 150 ppm of ethanol; this must be reduced down to
feed stream and liquid in the feed tray is <10 ppm in the nal methanol product. A complete
minimised.[20] While there are accepted and description of the composition of each component in
commonly used engineering practices for estimating the feed is given Table 1. Failure to meet this
the optimum amount of trays and ideal feed tray specication will result in substandard products that
for simple columns as specied in the study of cannot be sold to customers. In addition to the strict
Kister,[21] the inuence of the side draw on the product ethanol specication, the bottoms methanol
energy input is not explored as well. concentration also needs to be monitored and managed
The right placement of the side draw is of major below 10 ppm. Failure to meet this limit will require
importance, as it denes the tray ratio between the costly bio-treatment of the bottoms stream prior to
primary and secondary separation. Also of great discharge. Unlike the product and bottoms streams,
interest is the mass ow rate of the side stream, as this the fusel side draw consists of a methanol, ethanol
affects the boil-up ratio of the primary separation and water mixture and allows for dual high-purity
(Equation [2]) and, therefore, the relationship between specications. To maximise the protability, it is
both boil-up ratios. If the primary and secondary important to recover as much of the methanol entering
separation sections of the column are not balanced the column as products. In general, the ratio of
accordingly by varying the side stream location and methanol in the feed to methanol in the product must
ow rate, the process will operate at a sub-optimal be at a high level (97.5%). Failing to meet this
efciency. recovery will also result in and off specication
bottoms methanol specication. Figure 2 shows the
Increasing the recovery rening column as implemented in the process
simulator Aspen HYSYS. The trays are numbered from
The protability of increasing a columns recovery is top to bottom, where the condenser is the rst stage and
dependent on the additional capital and operating costs the reboiler the last. All together, the column has 87
required to increase recovery and the market value of stages.
the produced product. The nancial benet from The key components in the Feed F are methanol,
selling the extra product has to outweigh the additional ethanol, water and isobutanol. All other components
nancial costs. in the real feed are not considered, because the
For a simple distillation column, there are two concentrations are negligibly low. The feed stream
possible ways to enhance the degree of separation enters the column at stage 53 with the composition
and, hence, the recovery: by increasing the energy shown in Table 1. The primary separation, which takes
input or by mounting additional trays into the column. place in the upper section of the column, is between
This becomes more complicated for side draw methanol and ethanol, as dened in Distillation
columns, as the mass ow and the location of the side Columns with Side Draws section. In the lower part
stream inuence the interaction of the primary and of the column, the secondary separation between
secondary separation and, therefore, must be ethanol and the remaining components is carried out.
determined for every operation point separately. For a The high-purity methanol, which is drawn at the top
higher yield, the primary separation needs to be (Distillate D), must not contain more than 10 ppm
enhanced accordingly.
For our situation, however, the recovery of the
column cannot be increased at will. This is because
Table 1. Mass fractions in feed.
any marginal increase in recovery leads to severe
sensitivity to disturbances. This reects the fact Symbol Component Mass fraction (kg/kg)
that, at high recoveries, the column is being
operated at a point close to the theoretical X1 Methanol 0.83
X2 Ethanol 150 ppm
limitations of separation, where almost 100% of X3 Water 0.17
the methanol is extracted as products at ultra-high- X4 Isobutanol 95 ppm
purity specications.
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
962 M. A. KRALLER ET AL. Asia-Pacic Journal of Chemical Engineering

VLE property package with the Virial equation of state


and the Poynting correction was used to model the
distillation unit. The Wilsons equation uses two
adjustable parameters that can be set depending on the
chemical characteristics of the mixture.[23] The Wilsons
equation is well suited to model methanol distillation, as
the mixture has a single liquid and gas phase. The Viral
equation of state and the Poynting correction factor was
employed to modify the gas phase calculations to better
reect non-idealities present in the separation.[23]
The binary interaction parameters for the Wilsons
equation can be taken from vapourliquid equilibrium
(VLE) data bases, which, in turn, are based on physical
experimental data. However, when modelling multi-
component mixtures, these experimental data, which
are determined by carrying out experiments on two
components at a time, can be incorrect. This is because
the interaction parameters do not consider the
interactions among all of the components when they
are all present in a single multi-component mixture.[24]
In industrial process simulators, the users have the
option to choose between the pure binary interaction
parameters (as determined by experimental data) or to
use a semi-empirical (UNIFAC) interaction parameters
Figure 2. Distillation column as implemented in Aspen Plus. that attempts to correct for interaction when in a
mixture.[24] As expected, the simulation with the semi-
ethanol to reach the desired product specications. For empirical (UNIFAC) interaction parameters yielded
control purposes and to ensure this specication is satisfactory results, while the pure binary interaction
met, the industrial distillation units are operated at a parameters provided a poor data match with the
distillate ethanol concentration of 7 ppm. For the industrial data.
removal of ethanol, a Side Draw S is installed on stage The semi-empirical interaction parameters, on the
73. The Bottoms Product B is mostly water. It is other hand, were able to match the ethanol, water and
important that the methanol fraction of the Bottoms methanol proles with industrial data provided. The
Product B does not exceed 10 ppm, because this would isobutanol prole of the simulated column, however,
cause the need for expensive waste water treatment, did not match well with the industrial data provided.
which requires access to facilities that many methanol In order to achieve a better match with the isobutanol
producers do not even have within their plant. The mass prole, we have changed the interaction parameter
ow rates of the Feed F and the product streams are between isobutanol and water. It is also important to
listed in Table 2. note that this change did not have any noticeable effect
on the other concentration proles. The Murphree
Modelling efciencies are assumed to be equal for all the trays in
the column and were iteratively determined to be
An initial process model was created on Aspen HYSYS 84.0%. The t between the provided industrial data
by the authors in previous work[22] and was used as a and the computational model is shown in Table 3.
starting point. The model was rst adjusted by choosing
the right property package and Murphree tray
efciencies to achieve the best match between the INCREASING THE METHANOL YIELD
simulation and data provided by industry. The Wilson
Because the methanol synthesis is highly energy
Table 2. Mass ow rates for column operating at and cost intensive, it is of major interest to minimise
97.7% recovery.
the amount of methanol lost during the purication
Stream Mass ow in kg/h process. As shown in Table 4, there is still a large
amount of methanol being drawn from the side stream
Feed F 142 000 (2639 kg/h) for the current operation point of 97.7%
Distillate D 114 600
Side draw S 3113 recovery.
Bottoms B 24 287 In this section, we will investigate the possibility of
increasing the methanol yield (methanol recovery) of
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 963
Table 3. Deviation of the Aspen Plus model from the data provided by industry.

Product Data Model Percentage error


Methanol kg/kg 0.9999 0.9999 0
Ethanol ppm 7.00 7.00 0
Isobutanol ppm 0 0
Water ppm 85 50 41.2
Mass ow kg/h 114 600 114 598 0.01
Side draw
Methanol kg/kg 0.8554 0.8478 0.89
Ethanol kg/kg 0.0066 0.00658 0.25
Isobutanol ppm 47 55.8 18.7
Water kg/kg 0.138 0.141 2.40
Mass ow kg/h 3113 3113 0.00
Bottoms
Methanol ppm 7.00 6.96 0.60
Ethanol ppm 7.00 4 48.26
Isobutanol ppm 500 500 0
Water kg/kg 0.9999 0.9999 0.01
Mass ow kg/h 24287 24264 0.09
Energy
Reboiler MW 87.2 86.3 1.04
Condenser MW 87.7 87.0 0.80

Table 4. Methanol mass ow rates for column top of the column is increased. This is a
operating at 97.7% recovery. consequence of the fact that the degree of primary
separation is inversely proportional to the side draw
Stream Methanol ow in kg/h
mass ow rate, as predicted by Equation [1]. With
Feed F 117 236 additional methanol to the top of the column, the
Distillate D 114 597 distillate ow rate is increased by 2073 kg/h (a
Side draw S 2639
Bottoms B <1 1.8% increase). This increased ow rate was able
to be maintained while still achieving a distillate
product specication of 7 ppm of ethanol. A list of
the key process parameters for the column operating
the column. From an economic point of view, higher at a standard recovery of 97.7% and the column
methanol recovery will result in higher revenue. operating at the highest achievable recovery rate of
However, from a plant stability point of view, 99.5% is shown in Table 5. It should also be noted
operating the column at high recoveries will result in that reducing the mass ow rate of the side draw
an increased sensitivity to disturbances (as discussed decreased the amount of methanol lost via the side
in Design of Experiment section). Based on these two draw by 77.8%
facts and input from plant management, we have
decided to investigate the possibility of operating the ii. Lowering side draw location
column at a recovery ratio of 99.5%. This recovery rate
represents a relatively high, yet realistic/achievable By lowering the side draw location, the number of
rate. To increase the methanol yield of the column, trays provided for the primary separation increases,
the separation capacity has to be increased. For a while the number of trays provided for the
simple distillation column without a side draw, this secondary separation decreases. Although
means that either the reboiler duty must be increased increasing the number of trays for the primary
or additional trays must be introduced into the column. separation favours the purication of methanol
For a distillation column with a side draw, it is also within the column, a greater amount of impurities
necessary to balance the primary and secondary are still observed at the bottom of the column. This
separation to achieve optimal yield at a new operation is illustrated in Fig. 3, where both the methanol and
point. There are two possible ways: ethanol proles are shifted down in the column as a
result of lowering the side draw position. In order to
i. By reducing mass ow of the side draw compensate for the reduced secondary separation,
the reboiler duty of the column must be increased.
By lowering the mass ow rate of the side draw to It was found that by lowering the side draw to stage
733 kg/h, the amount of methanol that reaches the 81 and keeping the mass ow rate of the side draw
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
964 M. A. KRALLER ET AL. Asia-Pacic Journal of Chemical Engineering
Table 5. Process parameters for 99.5% recovery rate. varied. This will allow for the column to operate at
the most efcient point possible for a given
By reducing By lowering
mass ow of side draw recovery rate.
Product the side draw location
Methanol kg/kg 0.9999 0.9999
Ethanol ppm 7 7 OPTIMISATION OF THE SIDE DRAW COLUMN
Isobutanol ppm 0 0
Water ppm 75 70 A previous study conducted by Udugama et al.[22] has
Mass ow kg/h 116 671 116 671 successfully shown that the side draw location can be
Side draw optimised to reduce the required energy input for a
Methanol kg/kg 0.79 0.275 certain yield. This study did not vary, however, the
Ethanol kg/kg 0.0277 0.0066
Isobutanol ppm 80 55.8 mass ow rate of the side drawn or the number of
Water kg/kg 0.181 0.725 stages in the column.
Mass ow kg/h 733 3113 To nd the most efcient operation point for a given
Bottoms recovery, both the side draw mass ow rate and the
Methanol ppm 7.2 6.9
Ethanol ppm 0.2 0 side draw location must be simultaneously optimised,
Isobutanol ppm 558 500 resulting in the lowest possible required energy input
Water kg/kg 0.9999 0.9999 being achieved. As previously explained in Distillation
Mass ow kg/h 24 586 22 216 Columns with Side Draws section, this optimisation
Reboiler MW 88.5 88.2 process is inherent complicated as a result of the fact
that changing either one of these variables results in a
corresponding change in numerous other variables.
In the following section, the mass ow rate and
location of the side stream will be optimised for both
the actual operation point at 97.7% recovery and for
an enhanced recovery of 99.5%.

Optimum side stream location

Before optimising the side draw parameters, the


dependence of the reboiler duty on the side draw
location needed to be determined. Although the effect
of the side draw location on the required reboiler duty
was the key relationship being observed here, the mass
ow rate of the side draw, which needs to be at a
certain level to maintain the desired recovery, was also
monitored to ensure that it did not exceed certain limits.
Figure 4 shows that, by lowering the side draw (the
feed plate location remained unchanged), the reboiler
Figure 3. Methanol and ethanol concentration proles in
duty can be reduced to a minima point. Unfortunately,
the column with different side draw positions. by reducing the side draw location, the side draw mass
ow rate is also increased. This is because the
secondary separation is handicapped by reducing the
unchanged, a reboiler duty of 88.1 MW was height of the bottom section of the column. Based on
sufcient to achieve a recovery rate of 99.5% as plant experience, a side draw mass ow rate between
shown in Table 5. Compared with changing the 3000 and 5000 kg/h can be tolerated; a ow rate greater
mass ow rate of the side draw, the relative impact
of changing the side draw location is greater than
that of changing the side draw mass ow rate on
the balance between the primary and secondary
separations.In order to change the recovery of the
column while still achieving on-specication
products, the correct balance between the primary
and secondary separations must be maintained.
Achieving this perfect balance between the two
separations requires both the mass ow rate and Figure 4. Reboiler duties for different side draw locations
position of the side draw to be simultaneously for an operation with 99.5% recovery.
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 965

than this range can never be tolerated, however. This increasing the top pressure by 100 mbar remedies this
acceptable range is coloured red in Fig. 4. increase in the f-factor. Consequently, the effect of
For a recovery of 99.5%, the minimum reboiler duty optimising the side draw parameters on the columns
is achieved with a side draw at stage 79 (Fig. 4). Given f-factor can be neglected.
that the mass ow rate of the side draw at this stage is
1100 kg/h and, thus, does not fall above the acceptable Increase number of trays
side draw mass ow rate range, this ow rate is not of
concern. The optimum feed tray and the required If ultra-high levels of product recovery are desired at
reboiler duty were found to be stage 54 and 87.8 MW, the design phase of a production facility, the plant
respectively. This represents an energy saving of management has the option of installing additional
0.5% due to side draw optimisation. Compared with a trays in the main rening column. Figure 6 illustrates
column with an optimised side stream operating at a how the required reboiler duty varies with the number
recovery of 97.7%, a column with an optimised side of trays in the column. The feed and side draw location
stream operating at a recovery of 99.5% demands for each point has been optimised. The red standard
2.3% more reboiler duty. line indicates the reboiler duty of the current operation
point with a recovery of 97.7%. Looking at Fig. 6, it is
Flooding factor apparent that by operating the column at 99.5%
recovery and leaving the reboiler duty unchanged, 27
As the reboiler rate increases to increase recovery, the extra trays are required, resulting in a column with
vapour trafc in the column increases. Eventually, the 115 stages. To determine the most economically
column reaches a point where the liquid can no longer optimal number of trays, a nancial optimisation
ow down the column properly because of the higher process that considers both the increased operational
vapour ow and tray pressure drop. This leads to liquid costs associated with increasing reboiler duty and the
accumulating within the column. This situation is increased capital costs associated with installing
known as ooding. The ooding factor (f-factor) additional trays must be performed.
numerically quanties the likelihood of a single tray
to ood. In order to calculate the f-factor of each tray,
the speed of the upward travelling vapour in the DESIGN OF EXPERIMENT
column must be determined.[25] This was able to be
determined in Aspen HYSYS by providing the process It is an established concept that, for distillation, columns
simulator with the sizing of the trays used in an actual are more sensitive to process disturbances at increased
methanol plant. To achieve a higher recovery, an levels of product recovery. However, operating a
increase in reboiler duty is necessary. By having the column at ultra-high rates of recovery rates (99.5%)
reboiler produce more steam and by increasing the might illustrate interesting observations in comparison
column trafc while the dimensions of the column with operating the column at high rates of recovery
remain unchanged, the column operates closer to its (97.5%). The objective of this section is to use the
ooding point, as illustrated in Fig. 5. Although the steady-state model to quantify the increased sensitivity
optimisation of the side stream eases this ooding of the column as a result of increasing recovery. The
issue, the resulting maximum f-factor is still implications of this increased sensitivity on
 0:5 implementing ultra-high-purity distillation operations
kg
0:999ms 3 , which is 2% higher than that at in an industrial setting will also be explored. To
m
 0:5 examine the steady-state models performance and
kg
standard operation 0:98ms 3 . However, a slight stability at an increased recovery (compared with the
m
change in the operating pressure of the column can current operation), a Design of Experiment (DOE)
counteract this increase in f-factor.[22] In this case, was executed. The way in which the steady-state model

Figure 5. F-factor prole of the column at different Figure 6. Reboiler duties with operation at 99.5% recovery
operation points. for different column heights.
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
966 M. A. KRALLER ET AL. Asia-Pacic Journal of Chemical Engineering

reacted to certain input disturbances and, by extension, Table 7. Response variables for standard and
the process variables that most greatly inuenced this increased recovery without disturbance.
transient response, was investigated. a XD,Eth 7.00E06 7.00E06
b XB,Meth 7.26E06 6.99E06
c XD,Meth 0.999993 0.999993
Experimental set-up and specications d Rec 97.7 99.5

Within the DOE method, a higher recovery is achieved


without changing the distillation set-up by adjusting the
mass ow rate of the distillate and the side draw, as The results of the 24 factorial design for operation at
well as by varying the reboiler duty. For the analysis, 97.7% recovery and for operation at 99.5% recovery
changes in feed ow M_ F , reboiler duty Q_ Reb, methanol are shown in Tables A1 and A2, respectively, in the
XF,Meth and ethanol fraction XF,Eth in the feed were Appendix. Once the changes in the response variables
considered. Since the experiment is run at two levels to different process disturbances were determined, the
of disturbance (high and low), this results in a 24 effects e on the response variables could be calculated.
factorial design. The effects are shown in Table A3 (for a recovery of
The values for the disturbances are based on the 97.7%) and in Table A4 (for a recovery of 99.5%) in
experience of the real life plant and are as follows: the Appendix.
2.5% in feed ow M_ F
5% in reboiler duty Q_ Reb Analysis and acceptance of the results
1% in methanol fraction XF,Meth of the feed
To judge the signicance of the different disturbances,
50% in ethanol fraction XF,Eth of the feed.
Q-Q plots were generated in MATLAB for the two
For the execution of the DOE, the distillate and side operation points. The plots can be found in Figs. 7
draw mass ow rates are kept constant. As a result, a and 8. Insignicant effects almost behave like a random
change in feed ow rate only affects the bottoms ow sample drawn from a normal distribution with zero
rate. To balance the changes in XF,Meth and XF,Eth for mean, which implies the plotted effects will lie
the different runs, the water content of the feed XF, approximately on a straight line. The effects that
H2O was adjusted accordingly. deviate from the line are those of concern.
Table 6 gives the high and low levels of the input It can be seen in Fig. 7 that the ethanol concentration
variables for the DOEs. For both DOEs, the feed ow XD,Eth is barely affected by the disturbances for a
and composition are the same, but the reboiler duty is recovery of 97.7%, as the plotted effects almost form
higher in the case of the column running at a higher a straight line. The other three response variables XB,
recovery. This is because a greater amount of reux is Meth, XD,Meth and Rec seem to be affected most by the
required to achieve the desired separation. feed ow (A), followed by the methanol concentration
The response variables for this setup were ethanol in the feed (C). The interaction (AC) of both effects is
XD,Eth and methanol XD,Meth concentrations in the also distinctive.
distillate, as well as the methanol concentration in the Figure 8 shows that, for a recovery of 99.5%, the
bottoms XB,Meth and the recovery Rec. The values of ethanol concentration XD,Eth is affected by disturbances
these variables were monitored during the disturbance in the feed ow (A) and the ethanol concentration in the
tests. The response variables for the two different feed (D), where at the effect of the feed ow dominates.
modes of operation without any disturbance are shown The effect of the interaction (AD) is visible, too. XB,Meth,
in Table 7. XD,Meth and Rec are, again, disturbed severely by the
feed ow (A) and the methanol concentration in the
feed (C), with the interaction (AC) of both.
Table 6. Values of the input variables for both points The Q-Q plots demonstrate clearly that, for an
of operation. operation at increased recovery, the variable XD,Eth
develops a distinct sensitivity towards changes in feed
Main effect Standard +  ow and the ethanol concentration in the feed. The
A 141 976 145 525 138 426 disturbances in feed ow become perceptible, because
M_ F at 99.5% recovery, the column is operating very close
B [97.7] % 86.20 90.50 81.89 to the absolute methanol recovery. As the methanol feed
Q_ Reb
ow rate drops (while keeping the distillate ow rate
B [99.5] % 88.53 92.95 84.10
Q_ Reb and reboiler duty constant), a larger fraction of the
C XF,Meth 0.8258 0.8340 0.8175 methanol entering the column top of the tower in the
D XF,Eth 1.50E04 2.25E04 7.50E05 distillate. As the methanol feed ow rate drops (while
keeping the distillate ow rate and reboiler duty
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 967

Figure 7. Q-Q plots of the effect for 97.7%.

Figure 8. Q-Q plots of the effect for 99.5%.


2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
968 M. A. KRALLER ET AL. Asia-Pacic Journal of Chemical Engineering

constant), a larger fraction of the methanol entering the methanol content XF,Meth and the interaction of both
column will be drawn at the top. This can go above disturbances. All the remaining effects on XB,Meth, XD,
100% recovery. In such a situation, the methanol Meth and Rec are insignicantly small. At a higher
entering the column via the feed is, temporarily, lower recovery, the product purity seems to be affected more
than that leaving the column via the distillate. Thus, by an increase of the feed ow rate or methanol fraction
the impurities in the product will increase severely, as of the feed. The column is operating at a higher boil-up
the lack of methanol needs to be balanced with other ratio, and the lower side draw ow rate at increased
components. recovery favours the primary separation more.
The larger the fraction of methanol that is drawn at Therefore, the column is able to accumulate a larger
the top of the column as distillate and, therefore, the fraction of the additional methanol in the distillate. As
greater the sensitivity of the column to even small a consequence, the recovery is affected less.
disturbances (which can be sufcient to cause a To understand the directions of the effects, the
methanol decit). An under-supply of methanol can process must be analysed more closely. With an
force all of the ethanol in the column (as there is only increase in feed ow, more methanol enters the column
approximately 10 kg/h in the feed) and even water into along with the other components. As more methanol is
the distillate. At this point, XD,Eth becomes more fed to the column (while keeping the distillate ow rate
sensitive for changes in the ethanol content of the feed, constant), the product purity improves. But, with the
as the changes are passed on to the distillate reboiler duty being steady and the distillate ow being
composition to the full extent. limited, most of the excess methanol is drawn at the
For further analysis, all of the effects of the other bottom. This leads to a higher methanol concentration
three variables are displayed in the bar chart in Fig. 9, at the bottom and a lower methanol recovery.
to allow a convenient comparison between the two Figure 9 shows that the effects on the bottoms
operation points for these variables. methanol composition are fairly high for both
The responses of the variables XB,Meth, XD,Meth and recoveries. Changes in the methanol content of the feed
Rec resemble one another for the two different have a similar impact. When the methanol content in
operation points, as already observed in the Q-Q plots. the feed increases, the methanol purity of the distillate
All three show the highest sensitivity towards changes improves because the separation becomes easier.
in the feed ow M_ F , followed by disturbances in the However, the constant distillate rate means the product
recovery would be lower while the bottoms purity will
also be worse.
The main observation made for both of the recovery
cases is that both M_ F and XF,Meth have a noticeable
effect on the column performance. M_ F and XF,Meth
affect the columns performance by changing the
amount of methanol entering the column.
Consequently, achieving stable on-specication
operations requires the distillate and bottoms ow rates
to be changed such that a feasible mass balance is
reached. This effect is more apparent in the 99.5%
recovery scenario, where the effect on the product
methanol is higher for these two disturbances. A similar
observation is reported in the study of Fruehauf and
Mahoney,[26] where the author concludes that from a
control point of view, having the correct feed split (mass
balance) is a key aspect in achieving on-specication
operations when operating a column at ultra-high
recovery at dual high purity.

COLUMN SENSITIVITY TOWARDS


DISTURBANCES AT INCREASED RECOVERY

Operational stability

Figure 9. Effects of the different disturbances on the In order to evaluate a distillation columns stability
response variables. towards disturbances, short-term changes have to be
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 969

distinguished from long-term changes. Short-term however, it is also of interest to ensure that the bottoms
disturbances occur suddenly and unexpected, while composition does not contain excessive amounts of
long-term variations are usually known in advance or methanol such that costly waste water treatments are
happen over a longer period of time. Examples of said required. The effect of disturbances on the methanol
long-term changes include intended changes to the concentration at the bottom is very distinctive, which
methanol production or the bit by bit loss of activity makes a dual composition control highly advisable
of the catalyst in the reactor, both affecting the feed for both operation points.
of the distillation column. Because these disturbances For an operation at 99.5% recovery, the column is
are known and predictable, the parameters of the operating close to the theoretical limit of separation,
distillation can be pre-emptively adjusted to account as determined by a mass balance around the entire
for these disturbances. For this reason, these kinds of column. In any case, the difference between the
changes are of little concern. methanol mass ow entering the column and the
It becomes apparent that, for a higher recovery, the distillate mass ow is still higher than 500 kg/h.
product quality is affected more by disturbances, as Although this difference is not that great relative to
the risk of disturbances causing a lack of methanol the total mass ow rate of the feed, it does leave
for a certain distillate stream increases. Additionally, enough room for the feed forward controller to react
the ethanol prole along the column sharpens for to disturbances. Looking at an enhanced recovery of
higher recoveries, as the ethanol content in the side over 2000 kg/h of methanol, the higher control effort
draw increases. This affects the controllability and is denitely worth considering.
stability of the column heavily, as only a small upward
or downward shift of the prole has a major impact on
the performance of the column. CONCLUSION
Nevertheless, the effects of the disturbances
experiences by real columns are not as severe as those Feasibility of increasing the product recovery rate of a
observed in the steady-state model. The uctuations of high-purity methanol distillation column was studied
concern are mostly of short duration, and it, therefore, by employing a validated steady-state process
partly buffered by the column itself, which is simulation. In initial studies, it was established that
essentially a large mass and energy storage unit. location and the mass of the side draw are two critically
important factors in achieving high product recovery.
Control With the steady-state model, the side draw location
and mass ow have been optimised to achieve a
In order to achieve an increase in recovery, the effects minimum energy input for columns operating at a
of the disturbances with the biggest inuence must be standard recovery rate of 97.7%; these location and
reduced. As identied in the DOE, the product side draw adjustments represent an energy saving of
composition has the highest sensitivity to changes in 0.5%. If a methanol production facility is in the design
the feed ow. To improve the performance of the phase, an addition of 27 extra trays would also result in
column, a feed forward control can be applied. By an enhanced recovery of 99.5% without the need to
measuring the actual feed ow and adjusting the increase reboiler duty. Deciding between these two
column distillate ow rate, side draw ow rate and options requires comparing the relative energy and
reboiler duty accordingly, more stability and a more investment costs associated with each option. This
consistent product quality should be achieved as a nancial optimisation process will need to be
result of nullifying the disturbance. The inertia of the conducted on a case by case basis for each column. It
column towards interruptions buys additional response is often the case that a combination of both solutions
time. The controller must prevent the column from is the most protable course of action. Finally, the
experiencing a methanol decit while the distillate ow design of experiment showed that the feed ow,
rate remains unchanged. Such a situation would result followed by the feed composition, has the highest
in the concentration of impurities in the distillate impact on the essential column output parameters. It
product greatly exceeding product specication. Feed was also concluded that the effects of disturbances
forward control is also applicable for disturbances in become more signicant at higher rates of recovery.
feed composition, as this is the disturbance with the
second highest effect. NOMENCLATURE:
The DOE shows that for both operation points, a B Bottoms Product (-)
signicant effect of the disturbances on the bottoms D Distillate (-)
composition. Naturally, the ethanol concentration at E Effect (-)
the top of the column is of the greatest interest, as this F Feed (-)
determines the product quality and, hence, the market Mass ow rate of the bottoms
value of the nal product. With that being said, M_ B (kg/h)
2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
970 M. A. KRALLER ET AL. Asia-Pacic Journal of Chemical Engineering

Mass ow rate of the distillate Rec Recovery (%)


M_ D (kg/h) S Side Draw (-)
Mass ow rate of the feed (kg/h) V Boil-up column (-)
M_ F W Boil-up primary separation (-)
Methanol Mass ow rate in the XB,Meth Methanol mass fraction at the
M_ F;Meth feed (kg/h) bottom (-)
Mass ow rate of the side draw XD,Eth Ethanol mass fraction at the top
M_ S (kg/h) (-)
Methanol Mass ow rate in the XD,Meth Methanol mass fraction at the
M_ S;Meth feed (kg/h) top (-)
Boil-up rate primary separation XF,Eth Ethanol mass fraction in the
M_ V (kg/h) feed (-)
Boil-up rate seconcary XF,H2O Water mass fraction in the feed
M_ W separation (kg = h) (-)
Q_ Reb Reboiler duty (MW) XF,Meth Methanol mass fraction in the
R Reux Ratio (-) feed (-)

APPENDIX

Table A1. Results of the 24 factorial design for 97.7% recovery.

A B C D a b c d
1     9.06E05 3.61E24 0.987967 100.0
2 +    8.75E06 6.15E02 0.999991 96.3
3  +   9.06E05 1.35E24 0.987967 100.0
4   +  9.39E06 1.26E10 0.999991 99.2
5    + 2.72E04 3.62E24 0.987967 100.0
6 + +   1.33E06 6.01E02 0.999999 96.3
7 +  +  7.08E06 1.46E01 0.999993 94.4
8 +   + 2.63E05 6.17E02 0.999974 96.3
9  + +  1.45E06 1.05E10 0.999999 99.2
10  +  + 2.72E04 1.35E24 0.987967 100.0
11   + + 2.80E05 1.28E10 0.999972 99.2
12 + + +  1.07E06 1.45E01 0.999999 94.4
13 + +  + 4.00E06 6.02E02 0.999996 96.3
14 +  + + 2.11E05 1.46E01 0.999979 94.4
15  + + + 4.31E06 1.06E10 0.999996 99.2
16 + + + + 3.18E06 1.45E01 0.999997 94.4

Table A2. Results of the 24 factorial design for 99.5% recovery.

A B C D a b c d
1     8.90E05 1.90E24 0.970094 100.0
2 +    7.67E06 6.00E02 0.999992 98.1
3  +   8.90E05 8.80E25 0.970094 100.0
4   +  8.90E05 2.09E24 0.989692 100.0
5    + 2.67E04 1.90E24 0.970094 100.0
6 + +   1.12E06 5.97E02 0.999999 98.1
7 +  +  6.18E06 1.45E01 0.999994 96.1
8 +   + 2.30E05 6.01E02 0.999977 98.1
9  + +  8.90E05 9.41E25 0.989692 100.0
10  +  + 2.67E04 8.80E25 0.970094 100.0
11   + + 2.67E04 2.08E24 0.989692 100.0
12 + + +  9.01E07 1.45E01 0.999999 96.1
13 + +  + 3.36E06 5.97E02 0.999997 98.1
14 +  + + 1.84E05 1.45E01 0.999982 96.1
15  + + + 2.67E04 9.40E25 0.989692 100.0
16 + + + + 2.70E06 1.45E01 0.999997 96.1

2016 Curtin University of Technology and John Wiley & Sons, Ltd. Asia-Pac. J. Chem. Eng. 2016; 11: 958972
DOI: 10.1002/apj
SIDE DRAW OPTIMISATION OF A MULTI-COMPONENT
Asia-Pacic Journal of Chemical Engineering DISTILLATION COLUMN 971
Table A3. Effects of the disturbances on the different response variables at 97.7% recovery.

XD,Eth XB,Meth XD,Meth Rec


A 8.69E05 1.03E01 6.01E03 4.28E02
B 1.07E05 6.86E04 1.07E05 1.16E05
C 8.62E05 4.24E02 6.01E03 1.35E02
D 5.25E05 4.71E05 7.22E06 5.30E06
AB 2.75E06 6.86E04 2.75E06 2.96E06
AC 8.43E05 4.24E02 6.01E03 5.59E03
AD 4.35E05 4.70E05 1.85E06 9.66E07
BC 3.23E06 3.34E05 3.22E06 3.22E06
BD 5.31E06 1.33E05 5.30E06 5.30E06
CD 4.31E05 1.70E05 2.17E06 1.09E06
ABC 4.68E06 3.34E05 4.70E06 5.44E06
ABD 1.38E06 1.33E05 1.37E06 9.66E07
ACD 4.21E05 1.70E05 3.20E06 3.24E06
BCD 1.60E06 1.95E06 1.60E06 1.09E06
ABCD 2.34E06 1.95E06 2.33E06 3.24E06

Table A4. Effects of the disturbances on the different response variables at 99.5% recovery.

XD,Eth XB,Meth XD,Meth Rec


A 1.70E04 1.02E01 2.01E02 2.92E02
B 5.90E06 1.75E04 5.90E06 5.21E06
C 8.71E07 4.25E02 9.80E03 9.71E03
D 9.30E05 2.29E05 3.95E06 3.11E06
AB 5.90E06 1.75E04 5.90E06 5.21E06
AC 8.71E07 4.25E02 9.80E03 9.71E03
AD 8.50E05 2.29E05 3.95E06 3.11E06
BC 6.51E07 1.02E05 6.50E07 1.09E06
BD 2.94E06 1.20E05 2.93E06 3.11E06
CD 4.44E07 5.15E06 4.50E07 1.01E06
ABC 6.51E07 1.02E05 6.50E07 1.09E06
ABD 2.94E06 1.20E05 2.93E06 3.11E06
ACD 4.44E07 5.15E06 4.50E07 1.01E06
BCD 3.33E07 1.40E06 3.25E07 1.01E06
ABCD 3.33E07 1.40E06 3.25E07 1.01E06

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DOI: 10.1002/apj

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