Article

pubs.acs.org/IECR

Energy-Saving Design and Control of a Methyl Methacrylate

Separation Process
Wei-Lun Chang and I-Lung Chien*
Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan

ABSTRACT: An alternative design for the separation of a

mixture including methyl methacrylate, methanol, and water is
investigated as compared to a previous design using the same
process units. In this alternative design, top and bottom
products of the distillation column are designed to be at
unstable and stable nodes, respectively. Thus, signicant savings
in the steam cost (16.3%) can be realized as opposed to the
previous design of placing the bottom product at a saddle point.
Another benet is that the loss of methyl methacrylate product
through the water outlet stream is also less than that of the
previous design. This represents another 9.6% savings of the
operating cost for this alternative design. Furthermore, an
overall control structure for this alternative design is also devised
based on a novel way of using open-loop and closed-loop
sensitivity tests. By the control of a temperature dierence at two trays of the distillation column and another single-tray
temperature at the stripper, both MMA and water products can be maintained at high purities despite large variations in feed ow
rate and feed composition changes.

1. INTRODUCTION feed, such as pyridine in water or acetic acid in water.13,14 The

Heterogeneous azeotropic distillation (HAD) is a separation
method commonly used in industry to separate azeotropic
mixtures or close-boiling mixtures. By adding another light
component, a binary (or ternary) minimum boiling heteroge-
neous azeotrope can be formed. The top overhead of the HAD
column is usually designed to be near the heterogeneous
azeotrope, while the bottom is designed as high-purity product.
The overhead separates into two liquid phases in a decanter: an
organic phase sent back to the HAD column, and an aqueous
phase drawn out of the process or fed to a recovery column
depending on the desired purity. For example, ethanol
dehydration1,2 by HAD utilized another recovery column to
meet the specication on the aqueous outlet. On the other
hand, the ethylenediamine dehydration process3 was imple-
mented without any recovery column because of an already
high purity in the aqueous outlet from the decanter. In the
acetic acid dehydration process,4,5 the specication on the
aqueous outlet could be met by sending portions of the aque-
ous pahse back to the HAD column rather than using another
recovery column.
For the purpose of process intensication, the dividing-wall
column designs or thermally coupled techniques were
commonly incorporated into the HAD process with a recovery
column,610 showing the economic potential. Another savings
on the utility usage could be realized by vapor recompression or
heat pump.11,12 In addition, the recovery columns were further
combined with the preconcentrator for diluted feed.710 Some
authors even found good extraction solvents and proposed
hybrid extractiondistillation processes to separate the diluted
hybrid process could be viewed as a modication of HAD
process with an extractor, which was also shown to be
economically favorable. In the above HAD examples, decanters
were all designed at the top of the column so that the newly
formed lightest azeotrope could naturally separate into two
liquid phases.
However, for the studied system of separating methyl
methacrylate (MMA), methanol (MeOH), and water (H2O),
which is needed in the production of MMA processes, a hetero-
geneous MMA/H2O azeotrope at a saddle point is presented.
Wu et al.15 devised a two-column design with a bottom
decanter. The reproduced owsheet and the material balance
lines are shown in panels a and b of Figure 1, respectively. The
bottom composition of the distillation column was designed to
be near MMA/H2O azeotrope so that a decanter can be
designed to obtain aqueous and organic streams. The aqueous
stream is pure enough to draw out of the system while another
small stripper was needed to purify the organic stream to MMA
product specications. This design owsheet was further
simplied by combining two columns into one column with a
middle decanter.
The drawback of the above design is that the bottom
composition of the distillation column needs to be placed near
a saddle point (MMA/H2O azeotrope) of this ternary system.
Received: January 27, 2016
Revised: February 27, 2016
Accepted: February 29, 2016
Published: February 29, 2016

2016 American Chemical Society 3064 DOI: 10.1021/acs.iecr.6b00391

Ind. Eng. Chem. Res. 2016, 55, 30643074
Industrial & Engineering Chemistry Research Article

Figure 1. (a) Optimal design owsheet of original design. (b) Material balance lines of original design.

Also, the composition prole in the distillation column goes Table 1. UNIQUAC Model Parameters of the Studied
along the distillation boundary formed by two azeotropes (will Systemsa
be shown later). Thus, a larger reboiler duty was required at the
comp. i MeOH MeOH MMA
distillation column. Some contributions1620 mentioned a mix
with water in a decanter or extractor followed by distillation comp. j water MMA water
methods for this separation purpose, but they all lacked details aij 0 0 0
about the process and also the dynamic control of the process. aji 0 0 0
In this work, this concept will be implemented by simulations bij (K) 165.2623 44.6284 474.3300
and compared to the original design proposed by Wu et al.15 bji (K) 254.7308 411.6194 194.0000
a
Moreover, a feasible control structure will be developed and Aspen Plus UNIQUAC:
tested for the rejection of changes in feed composition or jij
i z
throughput. ln i = ln + qi ln i qiln ti qi + li + qi
xi 2 i j t j
2. ENERGY-SAVING DESIGN i
xjlj
2.1. Proposed Design Flowsheet. To correctly predict xi j
the thermodynamic behaviors of this ternary system, the
UNIQUAC model was selected as in previous work done by where
Wu et al.15 The UNIQUAC model and the binary parameters qixi qixi rx
i i
are shown in Table 1. The proposed conceptual design i = ; qT = qkxk ; i = ; qT = qkxk ; i = ; rT
qT qT rT
owsheet using the same process units by avoiding the saddle z
k k

point is shown in Figure 2a with the material balance lines = rkxk ; li = (ri qi) + 1 ri ; ti = kki ; ij
2
shown in Figure 2b. The fresh feed, containing 69.79 mol % k k

MeOH, 12.5 mol % water, and 17.71 mol % MMA, is rst bij
mixed with some water and condensed stripper overhead so = expaij + ; and z = 10
T
that the composition of this mixture is pulled within the liquid
liquid equilibrium (LLE) envelope. After liquidliquid
separation in the decanter at 50 C, the aqueous stream can mostly MeOH (MeOH/MMA azeotrope at the lowest
further be separated in a distillation column with top product of temperature in that distillation region) and the bottom product
3065 DOI: 10.1021/acs.iecr.6b00391
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Table 2. Basis of Economics and Equipment Sizing

column diameter (D): Aspen tray sizing
column length (L): NT trays with 2 ft spacing plus 20% extra length
column and other vessel (D and L are in meters)
capital cost = 17 640(D)1.066(L)0.802
condensers (area in m2)
heat-transfer coecient = 0.852 kW/Km2
dierential temperature = reux-drum temperature 315 K
capital cost = 7296(area)0.65
reboilers (area in m2)
heat-transfer coecient = 0.568 kW/K-m2
dierential temperature = steam temperature base temperature (T > 20 K)
capital cost = 7296(area)0.65
coolers (area in m2)
heat-transfer coecient = 0.852 kW/K-m2
dierential temperature = LMTD of (inlet or outlet temperature 315 K)
capital cost = 7296(area)0.65
energy cost
HP steam = $9.88/GJ (41 barg, 254 C)
MP steam = $8.22/GJ (10 barg, 184 C)
LP steam = $7.78/GJ (5 barg, 160 C)
cooling water = $0.354/GJ
electricity = $16.9/GJ
MMA price = $2/kg (approximated from ICIS indicative chemical price)
TAC = (capital cost/payback period) + energy cost
payback period = 3 yr

Figure 2. (a) Conceptual design owsheet of alternative design.

(b) Material balance lines of alternative design.

of pure water (at the highest temperature in the same

distillation region). The MMA product can be obtained from
further purifying the organic stream in a small stripper. Note
that in this alternative design, top and bottom products of the
distillation column are designed to be at the unstable and stable
nodes, respectively.
For an easy comparison of these two designs, the total
numbers of stages of the distillation column and the stripper are
assumed to be the same as in the previous design. The remaining
design variables considered in this study are only two, including
the recycled water ow rate (REC) and the feed stage of the
distillation column (NF1). The three product purity specica-
tions are set the same as in the previous design, which are
92.9946 mol % MeOH at distillate of the distillation column,
99.5 mol % H2O at the bottom of the distillation column, and
99.9 mol % MMA at the bottom of the small stripper.
A sequential iterative optimization procedure is performed
with REC as the outer iteration loop to minimize the total
annual cost (TAC) of this process and NF1 as the inner loop to
minimize total reboiler duty. The TAC includes total operating
cost and annualized total capital cost, where a three year
payback period is assumed. Operating cost includes the cost of
steam and cooling water, while the capital cost includes the cost
of columns and heat exchangers (reboilers and condensers).
Table 2 summarizes the formulas for the TAC calculation.21
Figure 3 shows the results of the optimization procedures. Note
that the recycled water ow rate is represented by the ratio of
recycled water ow rate to the water product ow rate (REC/
H 2 O) as a representative design variable during the Figure 3. Summary of TAC plots for this alternative design.

3066 DOI: 10.1021/acs.iecr.6b00391

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Figure 4. Optimal design owsheet of alternative design.

Table 3. Itemized TAC Terms of Various Systems

original alternative design
design (REC/H2O = 23)
C-1 column (1000 USD) 267.59 209.79
C-1 condenser (1000 USD) 164.48 128.69
C-1 reboiler (1000 USD) 104.96 109.01
C-2 column (1000 USD) 8.75 12.66
C-2 reboiler (1000 USD) 11.29 17.64
cooler (1000 USD) 18.24 59.38
capital cost (1000 USD) 575.31 537.18
LP steam cost (1000 USD/y) 567.80 475.63
cooling water cost (1000 USD/y) 24.37 20.02
operating cost (1000 USD/y) 592.17 495.65 (16.3%)
MMA lost from water outlet 57.10 (9.6%)
(1000 USD/y)
TAC (1000 USD/y) 783.94 617.61 (21.2%)

optimization. The optimal value of this ratio is 23 with the feed

on the 28th stage of the distillation column. The optimal
process owsheet is shown in Figure 4. Also, the itemized TAC
of these two designs is shown in Table 3. Despite large amount
of water recirculated in this system, a signicant saving in the
steam cost (16.3%) is realized by using this design. Another
benet is that the MMA product loss through the water
product stream is also less than previous design. This represents
another 9.6% savings of the operating cost.
2.2. Composition Proles in the Distillation Column.
Figure 5a,b shows the liquid-phase composition proles in the
distillation column for both designs. Two isovolatility curves
divide the ternary map into three regions where dierent
volatility rankings to these three components occur. For the
original design, not only is the bottom composition designed
near a saddle point, but also the composition prole goes along
the distillation boundary formed by two azeotropes. This
prole is located in a region where methanol is the most volatile
component followed by MMA and then water. Results show
that this prole has so close volatility that it requires a large
energy duty for separation.
However, for the alternative design, most of the prole is Figure 5. (a) Liquid-phase composition prole of C-1 column in
original design. (b) Liquid-phase composition prole of C-1 column in
located in another region where MMA is the most volatile alternative design.
component followed by methanol and then water. Results show
that it requires less energy duty because most of the stages are azeotrope. More accurately, as long as the MMA content in the
separating just methanol and water, a binary pair without feed to C-1 column all goes out from the top distillate with
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Table 4. Results in Process Variables from Closed-Loop Sensitivity Testsa

deviation
base case (kmol/h) (kW) MeOH + 10% MeOH 10% feed + 20% feed 20%
Process Variables
REC 286.11 12.34% 11.87% 21.70% 20.61%
R1 87.85 10.04% 10.03% 20.01% 20.00%
QR1 1991.76 10.44% 10.30% 20.88% 20.44%
QR2 131.00 36.89% 37.21% 19.60% 19.89%
QC1 1592.41 10.04% 10.04% 20.02% 20.00%
V1 162.82 10.04% 10.03% 20.01% 20.00%
D1 74.97 10.04% 10.03% 20.01% 20.00%
B1 298.55 10.84% 10.40% 21.62% 20.58%
H2O 12.44 23.54% 23.45% 19.70% 19.93%
AQ 373.52 10.68% 10.32% 21.30% 20.46%
OR 21.38 36.66% 36.71% 19.76% 19.91%
V2 8.79 36.86% 36.91% 19.09% 19.67%
B2 12.59 36.52% 36.57% 20.22% 20.08%
MIX 394.89 8.12% 7.78% 21.21% 20.43%
QC 371.24 3.31% 2.78% 24.32% 22.18%
Ratios
RR 1.172 0.00% 0.00% 0.00% 0.00%
R1/AQ 0.235 0.58% 0.32% 1.06% 0.58%
QR1/B1 6.672 0.36% 0.11% 0.61% 0.18%
QR1/AQ 5.332 0.22% 0.03% 0.34% 0.03%
QR2/OR 6.092 0.36% 0.37% 0.13% 0.03%
QR2/B2 10.405 0.58% 0.47% 0.52% 0.24%
a
[REC], recycled water ow rate; [R1], reux rate of C-1; [QR1], reboiler duty of C-1; [QR2], reboiler duty of C-2; [QC1], condenser duty of C-1;
[V1], overhead vapor ow rate of C-1; [D1], top distillate ow rate of C-1; [B1], bottom ow rate of C-1; [H2O], water product ow rate; [AQ],
aqueous phase ow rate; [OR], organic phase ow rate; [V2], overhead vapor ow rate of C-2; [B2], bottom ow rate of C-2; [MIX], mix stream
ow rate of fresh feed, REC, and V2; [QC], cooler duty.

methanol, the prole will be in that region where MMA is the
lightest component. Otherwise, if there is so much MMA fed to
the column that some of MMA should go out from the bottom,
MMA must be less volatile than methanol, which can be
achieved only with a high-energy-required composition prole
similar to that in the original design. The maximum MMA
content allowed for the prole as in Figure 5b depends on the
product specications and material balance. This is why the
TAC with REC/H2O = 21 in Figure 3 exceeds that of the
original design. The composition prole changes to the high-
energy-required one because the amount of recycled water is
not enough to separate out most of the MMA in the decanter.
3. OVERALL CONTROL STRATEGY DEVELOPMENT
In this section, a proper control strategy for this optimal design
in Figure 4 will be devised based on open-loop and closed-loop
sensitivity tests with Aspen Plus steady-state simulations. No
online composition measurement will be used in the quality
control loops for wider industrial applications. This control
strategy is expected to hold the product purities at speci-
cations despite any feed composition change or throughput
change.
The tray sizing option in Aspen Plus is utilized to calculate
the column diameters with the assumed tray spacing of 0.6096 m
and weir heights of 0.0508 m. The resulting column diameters
are 0.890 m for the distillation column and 0.327 m for the
stripper. Other equipment sizing follows the recommendations
by Luyben and Chien.22 Volumes of the column bases and the
reux drum are sized to provide 10 min holdup with 50% liquid
level. As for the decanter, it is sized bigger to allow the
separation of two liquid phases. The holdup time of 40 min
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with 50% total liquid level is used because of a smaller density
dierence in two liquid phases. Then this steady-state
simulation is exported to the dynamic simulations of Aspen
Plus Dynamics. Pressure-driven simulations in Aspen Plus
Dynamics is selected with the top stage pressures of every
column set at atmospheric pressure. Pressure drops inside the
columns will be automatically calculated by Aspen Plus
Dynamics.
3.1. Inventory Control Loops. The intuitive regulatory
control and inventory control loops are designed as follows.
Fresh feed ow rate is ow-controlled with a PI controller of
Kc = 0.5 and I = 0.3 min. Both column base levels are
controlled by manipulating their bottom ow rates separately.
Reux drum level is controlled by manipulating distillate ow
rate. As for the decanter, the aqueous phase level is controlled
by manipulating aqueous outlet ow, while the organic phase
level is controlled by manipulating organic outlet ow. P-only
controllers are used in level control loops. To speed up closed-
loop control behavior in the recycle loop, the settings Kc = 10
for the organic and aqueous phase level loops to manipulate
organic or aqueous ow and Kc = 5 for the base level loop of
distillation column to manipulate bottom ow rate are used.
Otherwise, Kc = 2 is used in the other level control loops. The
pressure of the distillation column is controlled by manipulat-
ing the condenser duty, while the pressure of the stripper is
controlled by manipulating the overhead vapor ow. In
addition, there are two temperature controllers controlling
temperature of the condensed overhead ow and the stream
entering the decanter at 50 C by manipulating the cooler duty.
These pressure and temperature PI controller parameters are
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set at default Kc = 20 and I = 10 min for the purpose of tight
control.
After the above regulatory control and inventory control
loops are established, there are four remaining degrees of
freedom in this system, including reboiler duty and reux rate
of the distillation column, reboiler duty of the stripper, and the
recycled water ow rate, which are related to quality control.
Thus, in sections 3.2 and 3.3, it will be illustrated how the
additional four control loops are determined for manipulating
these four remaining degrees of freedom.
3.2. Closed-Loop Sensitivity Test. A control strategy
is desirable if it is able to hold the product purities at
Figure 6. (a) Closed-loop sensitivity test on temperature prole in C-2
stripper. (b) Open-loop sensitivity test with reboiler duty (QR2) on
temperature prole in C-2 stripper.
Table 5. Results in Tray Temperatures from Closed-Loop Sensitivity Tests
base case (kmol/h) (kW) MeOH + 10%
Ratio and Temperatures
QR2/OR 6.092
T2 81.061
T36T33 11.126
T33T28 9.573
[T2], temperature on 2nd stage in C-2; [T36T33], temperature dierence between 36th and 33rd stages in C-1; [T33T28], temperature
dierence between 33rd and 28th stages in C-1.
Article
specications despite any disturbance. To save time, closed-
loop sensitivity test is a test that can help us understand what
kind of combinations of quality control loops will lead to better
performance in closed-loop control because this test can be
easily done with Aspen Plus steady-state simulation. This test
assumes that the overall process will nally achieve perfect
control after the anticipated disturbances are introduced to the
system. Thus, what we should do is to change the input data,
such as feed ow rate or feed composition, as disturbance and
then use the Design Spec option in Aspen Plus to vary the
degrees of freedom to hold the product purities at specication.
Finally, this process will go to a new steady-state equal to
perfect control if the Design Specs options all work successfully.
The last step is to identify any process variables or ratios of
process variables that remain almost unchanged before and
after the introduced disturbance, which are suitable to be
selected as controlled variables.
For this process shown in Figure 4, as mentioned in the
section 3.1, there are four remaining degrees of freedom.
However, the number of product purities of interest are just
three, which means there is still one degree of freedom
untreated if we hold all of the product purities. Thus, a quality
control loop for one of the degrees of freedom should be
guessed again and again until all Design Spec options work
successfully. The process is tested under two types of distur-
bances: one is 20% throughput changes (feed 20%), and
the other is 10% methanol changes in the fresh feed
composition (MeOH 10%). In the feed composition change,
MMA and water composition increase or decrease simul-
taneously and proportionally to each other. The successful
guessed control loop is to x the reux ratio in the distillation
column; then the remaining three degrees of freedom are varied
to hold the purities. Parts of the results of the closed-loop
sensitivity test are listed in Table 4, including process variables
and some important ratios. Base case represents the results
before any disturbance, while the deviation means the results of
perfect control compared to the base case. The other results of
the closed-loop sensitivity test, tray temperatures in the
columns, will be used in section 3.3.
Table 4 shows that every degree of freedom should change
for the sake of perfect control, but some of the ratios can
be xed. These ratios which change least are the reux ratio in
the distillation column (RR), ratio of reboiler duty in C-1 to the
aqueous phase ow rate (QR1/AQ), and ratio of reboiler duty
in the stripper to the organic phase ow rate (QR2/OR). Thus,
xing these three ratios is feasible for perfect control. The
remaining degree of freedom is the recycled water ow rate,
which must be manipulated with the aid of a tray temperature
controller.
deviation
MeOH 10% feed + 20% feed 20%
0.36% 0.37% 0.13% 0.03%
0.00% 0.06% 0.13% 0.08%
0.15% 0.05% 0.18% 0.13%
1.18% 1.12% 2.38% 2.12%
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3.3. Selection of Temperature Control Stage(s). Open-
loop and closed-loop sensitivity tests are used to determine the
tray temperature control point for both columns. The open-
loop sensitivity test is performed in which 0.1% changes in
one of the degrees of freedom is given when others are xed.
An appropriate temperature control point should have large
Figure 7. (a) Closed-loop sensitivity test on temperature prole in C-1
column. (b) Open-loop sensitivity test with recycled water ow rate
(REC) on temperature prole in C-1 column.
Figure 8. Overall proposed control structure for this alternative design.
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sensitivity (large temperature deviation in open-loop sensitivity
test) to the manipulated variables. On the other hand, as men-
tioned before, an appropriate temperature control point should
also be almost unchanged (small deviation in closed-loop
sensitivity test) for the sake of perfect control. Thus, the control
point is determined based on both open-loop and closed-loop
sensitivity tests.
For the C-2 stripper, the results of tray temperature deviation
in the closed-loop sensitivity test are shown in Figure 6a, and
the results in the open-loop sensitivity test are shown in Figure 6b.
Although temperature on the rst stage deviates the least under
perfect control, it has less sensitivity to the reboiler duty. The
best temperature control point is the second stage considering
both requirements discussed above. However, in section 3.2, we
know that the reboiler duty can also be manipulated with xed
ratio to the organic phase ow rate. In Table 5, deviations of
this ratio and the temperature on second stage (T2) in closed-
loop sensitivity test are compared. This temperature is better
as a controlled variable because of less deviation, while this ratio
can still be applied as an inner-loop ratio control for better
dynamic performance.
As for the C-1 distillation column, results of both tests are
shown in Figure 7a,b. The selection is not obvious because
stages with larger open-loop sensitivity all have much
temperature deviation under perfect control. Large deviation
in product purities is further conrmed after the introduction of
any disturbance by using either single-end or dual-end
temperature control. However, temperatures on stages 2836
have similar temperature deviations under perfect control. This
means that a smaller deviation in temperature dierence
between any two of these stages can be achieved. If the
temperature dierence between any two stages is selected as a
controlled variable, it should also have enough open-loop
sensitivity to the manipulated variables, which is the subtraction
of two sensitivities for these two stages. Thus, one of the stage
temperatures should have larger sensitivity, while the other one
should have smaller sensitivity. Figure 7b shows that temper-
ature dierence between stages 28 and 33 (T33 T28) has the
largest open-loop sensitivity. However, the nal selected tem-
perature dierence is that between stages 36 and 33 (T36
T33) for better closed-loop performance as listed in Table 5, at
the cost of just a little decrease in the open-loop sensitivity,
shown in Figure 7b. Here, controlling a temperature dierence
DOI: 10.1021/acs.iecr.6b00391
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Figure 9. Closed-loop dynamic responses to 10% methanol feed composition changes.

can also be viewed as a single-tray temperature control with a
oating set point from another tray.
3.4. Closed-Loop Dynamic Control Behaviors. In
summary of sections 3.2 and 3.3, the four quality control
loops are determined: xed reux ratio in C-1 column (RR),
3071
xed ratio of reboiler duty in C-1 column to aqueous
phase ow rate (QR1/AQ), controlling temperature on second
stage (T2) in C-2 stripper by manipulating the ratio of its
reboiler duty to organic phase ow rate (QR2/OR), and
controlling the temperature dierence between the 36th
DOI: 10.1021/acs.iecr.6b00391
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Industrial & Engineering Chemistry Research
Figure 10. Closed-loop dynamic responses to 20% throughput changes.
and 33rd stages (T36-T33) in C-1 column by manipulating
the recycled water ow rate. PI controllers are used in
these two temperature control loops with 1 min deadtime.
They are iteratively tuned by relay feedback test provided
in Aspen Plus Dynamics with TyreusLuyben tuning rules.23
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For the single-tray temperature controller, the resulting
parameters are Kc = 0.931 and I = 10.56 min with reverse
action. For the controller controlling temperature dierence,
the resulting parameters are Kc = 0.295 and I = 65.34 min with
direct action.
DOI: 10.1021/acs.iecr.6b00391
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The overall proposed control structure is shown in Figure 8.
Note that two inner-loop ratio controls are added for faster
dynamic response: ratio of recycled water ow rate to fresh feed
ow rate and ratio of reboiler duty in the stripper to organic
phase ow rate. Thus, both temperature controllers adjust these
two ratios separately, rather than directly manipulating recycled
water ow rate or the reboiler duty.
Two types of disturbances will be used to test the proposed
control strategy. The tough disturbance of unmeasurable fresh
feed composition changes is considered rst. Large variations
of 10% methanol changes (MeOH 10%) in the fresh
feed composition are tested, and MMA and water in feed
composition increase or decrease simultaneously and propor-
tionally to each other. For example, in the +10% MeOH case,
the feed composition changes from 69.79 mol % MeOH,
12.50 mol % H2O, and 17.71 mol % MMA to 76.77 mol %
MeOH, 9.61 mol % H2O, and 13.62 mol % MMA. Figure 9
shows the closed-loop dynamic responses to feed composition
changes. It is observed that the temperature in the C-2 stripper
and the temperature dierence in the C-1 column are
quickly controlled back to their set point values within 6 h.
Three product ow rates increase or decrease according to the
unmeasurable feed composition changes. Most importantly, all
three product purities are maintained near their specications
despite these unmeasurable disturbances.
The other tested disturbance is the 20% throughput
changes (feed 20%). Although throughput changes can be
considered as known disturbance, any set point in this control
strategy has no need to adjust with the throughput changes.
Figure 10 displays the dynamic responses of this disturbance.
All three product purities are also maintained near their
specications despite large throughput changes.
When the closed-loop performances of this proposed design
are comared with that of the original design in Wu et al.,15 the
ranges of feed composition and feed rate changes for the
closed-loop tests in this paper are almost doubled. In spite of
these larger disturbance changes, the product purities are still
kept very close to their original values even during transient
conditions.
4. CONCLUSIONS
In this work, an alternative design of a methyl methacrylate
separation process is rigorously studied and compared to the
original design. Both designs utilize a distillation column, a
stripper, and a decanter. In the alternative design, the fresh feed
is rst mixed with some water and condensed stripper overhead
so that the composition of this mixture is pulled within the LLE
envelope. After liquidliquid separation in a decanter, the
distillation column is used to separate the aqueous stream,
while the organic stream is puried in a stripper. It shows that
signicant saving in the steam cost (16.3%) is realized. Another
benet is that the MMA product loss through the water
product stream is also less than that of the original design. This
represents another 9.6% savings of the operating cost. Also, the
composition proles in the distillation column are compared. It
shows that these two proles are in dierent regions with
dierent volatility rankings, resulting in dierent relative
volatility as well as energy usage for separation.
An overall control structure is also devised based on a novel
way to use closed-loop and open-loop sensitivity tests. The four
controlled variables in quality control loops include the reux
ratio in the C-1 column, the ratio of reboiler duty in the C-1
column to aqueous phase ow rate, the temperature dierence
3073
Article
between the 36th and 33rd stages in the C-1 column, and the
temperature at the second stage in the C-2 stripper. Two inner-
loop ratio controls are added to enhance the dynamic
performance. Results show that with the aid of this control
strategy, the process quickly reaches another steady state within
6 h and all the product purities are still maintained near their
specications despite any disturbance, such as feed composition
changes or throughput changes.
AUTHOR INFORMATION
Corresponding Author
*Tel: +886-3-3366-3063. Fax: +886-2-2362-3040. E-mail:
ilungchien@ntu.edu.tw.
Notes
The authors declare no competing nancial interest.
ACKNOWLEDGMENTS
The research funding from the Ministry of Science and
Technology of R.O.C. under Grant MOST 104-2218-E-002-
006 is greatly appreciated.
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Ind. Eng. Chem. Res. 2016, 55, 30643074