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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
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.
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]:
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
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%.
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
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.
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
APPENDIX
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
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.
Table A4. Effects of the disturbances on the different response variables at 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