Beruflich Dokumente
Kultur Dokumente
319-335 (2006)
319
ABSTRACT
This work explores the feasibility of recovery of acetic acid from aqueous solutions with different acid concentrations. Instead of separating acid from water using
azeotropic distillation, acetic acid is converted to acetate via esterification. A range of
acetic acid concentrations is explored, varying from 100 wt%, to 75 wt%, to 50 wt%,
and then to 30 wt%. The TAC analysis shows that a standalone reactive distillation is
more economical than a flowsheet with a pre-treatment unit. Process characteristics
have been explored and the results show significant nonlinearity associated with reactive distillation columns for all four different acid concentrations. A systematic design
procedure is devised to control reactive distillation columns by temperature control.
Reasonable control performance can be achieved. A further improvement can be made
by incorporating feedforward control for feed flow disturbance. Finally, one-temperature-one composition control structure is also examined. Acceptable control performance can be obtained while maintaining acetate composition.
Key Words: reactive distillation, esterification, acetic acid recovery, process control,
temperature control, nonlinearity measure.
I. INTRODUCTION
Dilute acetic acid solutions are often produced
in many chemical processes, manufacturing of terephthalic acid, dimethyl terephthalate, cellulose ester, and
acetate rayon (Xu et al., 1999a, 1999b; Saha et al.,
2000; Chien et al., 2004; Hung et al., 2005b).
Typically, the acetic acid concentration ranges from
70 wt% to 35 wt% and possibly down to 2-6 wt% for
wood distillation. Generally, two approaches can be
taken to treat the dilute acid. One approach is the
acetic acid dehydration using simple distillation or
heterogeneous azeotropic distillation as discussed in
detail by Chien et al. (2004). A different route is to
convert dilute acetic acid into useful chemicals such
*Corresponding author. (Tel: 886-2-3365-1759; Fax: 886-23366-3037; Email: ccyu@ntu.edu.tw)
W. J. Hung, I. K. Lai, H. P. Huang, and C. C. Yu are with the
Department of Chemical Engineering, National Taiwan University
Taipei 106, Taiwan.
S. B. Hung and M. J. Lee are with the Department of Chemical
Engineering, National Taiwan University of Science and Technology
Taipei 106, Taiwan.
as acetates, which has been explored by several researchers (Xu et al., 1999a, 1999b; Saha et al., 2000;
Hung et al., 2005b). Generally, reactive distillation
is used for converting dilute acid into acetate and the
conversion of the acid ranges from 60-80% as shown
in the studies of Saha et al. (2000) and Xu et al.
(1999a; 1999b). Hung et al. (2005b) explore the process chemistries based on the total annual cost (TAC)
and they conclude that amyl alcohol is an ideal solvent for converting the dilute acid to amyl acetate and
this offers great economic potential as compared to
the cost of acetic acid. Amyl acetate has been used
in industries as a solvent, an extractant, a polishing
agent etc. Design and control of amyl acetate using
pure acetic acid has been studied by Chiang et al.
(2002) and Huang and Yu (2003). The above mentioned amyl acetate reactive distillation columns have
been designed for neat operation. That is an exact
stoichiometric amount of alcohol and acid is processed in one column such that high purity product
can be obtained with an almost 100% conversion, as
opposed to excess reactant design. This imposes stringent requirements on the control system design.
320
Despite the great economic potential of a steadystate perspective, the operability of four reactive distillation columns with 100wt%, 75 wt%, 50wt%, and
30wt% is explored. First, process characteristics, such
as nonlinearity measure and possible output
multiplicities, are studied. Next, a systematic design
procedure is devised for dual-temperature control and
potential advantage of feedforward control is also shown.
In order to maintain acetate product specification, composition control is also explored. The results indicate
that acceptable control performance can be obtained
for all different purity levels of acetic acid.
II. PROCESS ANALYSIS
1. Optimal Steady-State Design
Hung et al. (2005b) examines the process chemistry for dilute acetic acid recovery using alcohols
ranging from methanol to n-pentanol (C1 to C5 ). The
results indicate that amyl alcohol is the best solvent
for recovery of dilute acetic acid using a single reactive distillation column (without pretreatment) based
on steady-state economics. Following the steady-state
design procedure of Tang et al. (2005), the optimum
results are shown in Fig. 1. Table 1 summarizes the
optimal steady-state design for four different acid
purity levels: 30 wt%, 50 wt%, 75 wt%, and 100 wt%.
Product specification for the acetates is set to 99
mol% with a production rate of 50 kmol/hr.
It is interesting to note that the column diameter increases as HAc becomes more and more dilute.
The reason for that is the column diameter is set by
the vapor rate. That implies that as HAc concentration decreases, a reactive distillation with larger reactors with fewer equilibrium stages is preferred from
a steady-state economic perspective for the amyl acetate system. But the Damkhler number (Da) actually drops from 9.8 to 2, because of a larger vapor/
liquid traffic.
2. Nonlinearity and Output Multiplicity
The manipulated variables are determined to
evaluate process nonlinearity for the amyl acetate
process. The tray temperatures are treated as state
variables. The manipulated variables are the heat
input Q R and feed ratio FR, respectively. First, the
upper and lower bounds of the steady-state gains between the tray temperatures and the manipulated variables (Q R and FR) are obtained for a range of input
variations. In this work, 5% to +5% changes in the
heat input (Q R) and 1% to +1% changes in the feed
ratio are made. Note that, for a truly linear system,
the upper and lower bounds should coincide with each
other. Fig. 2 clearly shows that dilute acetic acid
concentrations of 75 wt% and 50 wt% are more nonlinear than the other two cases of 100 wt% and 30
wt%. Moreover, the sign reversal is also observed
for the four cases under either QR or FR change. The
results presented here are rather unconventional, because chemical processes are known to be quite
nonlinear, but not to this degree in such a consistent
manner. Two measures are used to differentiate the
degree of nonlinearity. One obvious choice is the
fraction of sign reversal for all tray temperatures. In
this regard, the case of 75 wt% HAc composition indicates that more than half of the trays show sign reversal in which almost half of the tray temperatures
exhibit the sign reversal. Table 2 summarizes the
fraction of sign changes for all four cases. The second nonlinearity indicator is N which was first proposed by Allgower for dynamic systems and further
studied by Hernjak and Doyle (2003) under feedback.
Schweickhardt and Allgower (2004; 2005) give an
updated summary on nonlinearity measures. The
measure ranges from 0 to 1, N = 0 implies a linear
process and N = 1 means a highly nonlinear system.
Following Hung et al. (2005a), we only consider
steady-state (e.g., can be viewed as the nonlinearity
measure for a static function) and the upper bound of
the nonlinear measure can be computed from:
N =
G G+
G+ 2
G G
G 2
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
Condenser
Condenser
Pure AmOH
FAmOH = 50 (kmol/hr)
14
Impure HAc 12
FHAc = 438.98
(kmol/hr)
Pure AmOH
FAmOH = 50 (kmol/hr)
15
RD
Column
321
26
25
24
Organic
Reflux
RD
Column
Impure HAc
FHAc = 105.55
(kmol/hr)
2
1
Reboiler
0
1
Reboiler
0
(A) 30 wt%
Condenser
Pure AmOH
FAmOH = 50 (kmol/hr)
Pure AmOH
FAmOH = 50 (kmol/hr)
19
18
17
Impure HAc
FHAc = 216.64
(kmol/hr)
Condenser
RD
Column
40
Organic
Reflux
39
36
Pure HAc
RD
Column
FHAc = 50
(kmol/hr)
2
Reboiler
Reboiler
1
HAc = 0.8 mol%
AmOH = 0.2 mol%
AmAc = 99 mol%
H2O = 8.11E-8 mol%
(B) 50 wt%
0
HAc = 0.8 mol%
AmOH = 0.2 mol%
AmAc = 99 mol%
H2O = 5.66E-14 mol%
(D) 100 wt%
Fig. 1 Optimized process flowsheets for aqueous acetic acid recovery via single reactive distillation column using amyl alcohol
322
Table 1 Optimal steady-state operating conditions and total annual cost (TAC) for recovery acetic acid
with reactive distillation
100wt%
(100 mol%)
75wt%
(47.4 mol%)
50wt%
(23.1 mol%)
30wt%
(11.4 mol%)
41
6
33
1
7~39
36
39
50
50
49.96
50.03
52.23
122.62
27
3
22
1
4~25
24
25
50
50
105.91
49.64
48.16
175.01
20
1
17
1
2~18
17
18
50
50
217.43
49.21
71.79
323.13
16
1
13
1
2~14
12
14
50
50
440.63
48.35
139.26
651.62
0.0010
0.00711
0.00011
0.99178
0.00459
0.00645
0.00023
0.98873
0.00385
0.00506
0.00032
0.99076
0.00372
0.00411
0.00038
0.99179
0.00805
0.00195
0.99000
5.66e-16
-1283.00
-186.67
1295.15
1.225
23.85
21.86
36.49
0.00697
0.00302
0.99000
4.22e-12
-1845.36
-226.86
1840.41
1.454
35.70
26.74
51.86
0.00765
0.00232
0.99000
8.11e-10
-3396.69
-416.42
3405.30
2.018
71.21
52.42
95.95
0.00676
0.00323
0.99000
1.04e-09
-6789.01
-830.79
6876.45
2.957
144.22
105.88
193.76
9.58
3.64
2.88
1.98
790.24
404.26
69.44
316.54
794.00
343.39
58.83
391.79
1048.71
378.66
71.45
598.61
1518.65
470.85
102.01
945.79
167.51
20.81
146.70
227.93
19.53
208.41
414.61
29.06
385.54
826.01
47.74
778.27
430.92
492.60
764.18
1332.23
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
323
0.4
8
0.2
AmAc
6
dT/dFR
dT/dQR
0.0
-0.2
AmAc
-0.4
upper
lower
linear
-0.6
-0.8
upper
lower
linear
4
2
0
-1.0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40
stages
0 2 4 6 8 10 1214 16 18 20 22 24 26 28 30 32 34 36 3840
stages
(a) 100 wt%
6
5
AmAc
upper
lower
linear
dT/dFR
dT/dQR
2
1
0
-1
0
2 4
13
12
11
10
9
8
7
6
5
4
3
2
1
0
-1
8 10 12 14 16 18 20 22 24 26
stages
AmAc
upper
lower
linear
2 4
8 10 12 14 16 18 20 22 24 26
stages
15
11
10
9
8
7
6
5
4
3
2
1
0
AmAc
AmAc
10
upper
lower
linear
dT/dFR
dT/dQR
(b) 75 wt%
upper
lower
linear
10 12
stages
14 16
18
10 12
stages
14
16
18
(c) 50 wt%
25
AmAc
upper
lower
linear
15
10
dT/dFR
dT/dQR
20
5
0
0
8
10
stages
12
14
45
40
35
30
25
20
15
10
5
0
-5
AmAc
upper
lower
linear
8
stages
10
12
14
(d) 30 wt%
Fig. 2
Upper and lower bounds of steady-state gains of all tray temperatures for 5% reboiler duty and 1% feed ratio changes and the
sign reversal indicated as shaded areas
324
Table 2. Fractions of sign reversal and nonlinearity measures for AmAc esterification with different feed
compositions of acetic acid
System
HAc
composition
in the feed
AmAc
100 wt%
75 wt%
50 wt%
30 wt%
Fraction of sign
reversal
QR
0.10
0.41
0.21
0
FR
0.07
0.67
0.37
0
Overall*
0.17
0.67
0.42
0
Nonlinearity measure
(Schweickhardt and
Allgower)
QR
0.84
0.90
0.91
0.69
FR
0.66
0.75
0.69
0.84
Overall**
0.76
0.83
0.81
0.77
Overall
Assessment***
M
H
H
M
fast dynamics are attainable with a much smaller transient deviation (maximum deviation of less than 0.02
m.f.) as shown in Fig. 5. Furthermore, the process
settles in 5 hours. Fig. 5 also shows asymmetrical
responses in the product compositions (X B,acetate and
XD, H2O).
Because of large transient deviation for the cases
of 100 wt% and 30 wt% HAc feed, the feedforward
control is incorporated for, possibly, improved control performance. In the feedforward configuration,
Fig. 6, the feed flow rate is fed forward to the heat
input via a ratio control. Thus, the heat input can be
adjusted in advance to prevent large deviations in the
temperature as well as composition. Again, feed flow
disturbance is also used for comparing the performance of these two control configurations (with and
without feedforward control). Fig. 7 compares the
dynamic responses for these two control structures
for the cases of 100 wt% and 30 wt% HAc feed. The
results show that the peak errors are reduced by factors of 3 and 10, respectively, as shown in Fig. 7.
That implies that feedforward control is very effective for these highly nonlinear reactive distillation
systems. Before leaving the section, it should be
emphasized that, despite reasonable control
performance, steady-state offsets in the acetate composition can be observed in the dual temperature
control. The steady-state offsets range from 0.013
m.f. for 75 wt% HAc feed to 0.0075 m.f. for 50 wt%
HAc feed. In order to maintain product quality, composition control is explored next.
IV. COMPOSITION CONTROL
Because of the steady-state offsets in the dualtemperature control, one may seek offset-free composition control for amyl acetate production using
dilute acetic acid. Here, we choose to control the
acetate product quality via composition control while
325
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
1.00
126
AmAc
124
Mole fraction
125
0.99
0.98
140
0.94
AmAc
0.92
0.97
1275
141
0.96
123
1260
142
0.98
T34 (C)
Mole fraction
T34
T16 (C)
1.00
0.90
0.990
1335
139
T16
0.995
1.000
FR
138
1.010
1.005
125
0.995
0.99
0.97
115
AmAc
Mole fraction
0.98
0.96
T21
0.95
0.94
1800
110
0.990
142
0.985
140
0.980
138
0.975
136
0.970
0.990
105
1880
1820
1840
1860
Heat input (KW)
144
T15
120
T21 (C)
Mole fraction
146
AmAc
0.995
1.000
FR
T15 (C)
1.00
134
1.010
1.005
(b) 75 wt%
1.00
135
0.995
AmAc
120
0.98
T15
0.990
140
AmAc
0.985
135
T11
115
0.97
3390
Mole fraction
125
T15 (C)
Mole fraction
0.99
0.980
0.990
3465
0.995
1.000
FR
1.005
T11 (C)
145
130
1.010
(c) 50 wt%
1.000
0.995
0.990
105.2
0.985
AmAc
0.980
105.0
T13
0.975
T13 (C)
Mole fraction
Mole fraction
105.4
0.990
135
0.987
130
AmAc
125
0.984
T10
104.8
0.970
6840
6855
6870
6885
Heat input (KW)
6900
6915
T10 (C)
105.6
120
0.981
0.990
0.995
1.000
FR
1.005
1.010
(d) 30 wt%
Fig. 3
Trends of product compositions and temperature responses for a range of changes in the manipulated variables (heat input and feed
ratio) and nominal design indicated by the dashed line
326
PC1
X
TC1
FC
Organic
Reflux
FT
AmOH Feed
LC1
LC2
Decanter
HAc Feed
FT
Water
RD
column
FC
TC2
TC3
LC3
Steam
Reboiler
Product
dynamic performance of one- temperature- one- composition control for recovery of dilute acetic acid. Fig.
9 shows the dynamic responses for 20% feed flow
rate changes. Asymmetric responses can be clearly
seen for all four cases and they take, at least, 15 hours
to reach steady-state. Despite offset free performance,
the closed-loop performance is generally poorer than
that of the dual-temperature control counterpart. This
is especially true for the cases of 75 wt% and 50 wt%
HAc feed where fast transient is replaced by slow
dynamics, in order to eliminate steady-state offset.
The results presented here clearly indicate the importance of rapid response to disturbance of a control
system for these highly nonlinear processes. Once
the controlled variables drift away from set point, it
takes a great effort to bring them back to set point.
This is quite similar to what we have seen in extremely
high-purity distillation columns.
V. CONCLUSIONS
This work explores the dynamics and control for
the recovery of dilute acetic acid (ranging from 100
wt% to 30 wt%) via esterification using reactive
distillation. Despite great economic incentives, it is
not clear whether these reactive distillation systems
possess good operability. First, two measures are used
to analyze the degree of nonlinearity for all four cases.
One is the fraction of sign reversal for all tray temperatures and the other is the Allgowers nonlinearity
measure, N. Results show that significant nonlinearity
and possible steady-state sign reversal are observed
for all four systems. A systematic design procedure
is used to design the control structures. Simulation
T 15
T 21
T 11
T 15
T 10
T 13
AmAc
(75 wt%)
AmAc
(50 wt%)
AmAc
(30 wt%)
FR = F AmOH /F Acid
QR
FR = F AmOH /F Acid
QR
FR = F AmOH /F Acid
QR
FR = F AmOH /F Acid
QR
Manipulated
variables
T10
= 37.399 15.720
T13
0.785 0.217
T11
= 18.605 16.429
T15
3.899 0.663
T15
0.115
= 3.3
T21
5.485 20.295
T16
= 0.018 14.980
T34
0.595 0.656
T 16
T 34
AmAc
(100 wt%)
Controlled
variables
Q R, S
FR
Q R, S
FR
Q R, S
FR
Q R, S
FR
FR
0.396 0.604 T 10
= 0.604
0.396 T 13
Q R FR
0.239 1.239 T 11
= 1.239
0.239 T 15
Q R FR
0.009 0.991 T 15
= 0.991
0.009 T 21
Q R FR
0.001 1.001 T 16
= 1.001
0.001 T 34
QR
RGA
QR T 13:
Kc: 0.31 I: 1.128 (min)
FR T 10:
Kc = 0.337 I: 71.49 (min)
QR T 15:
Kc: 1.656 I: 8.76 (min)
FR T 11:
Kc = 1.86 I: 62.296 (min)
QR T 21:
Kc: 0.561 I: 3.67 (min)
FR T 15:
Kc = 1.2 I: 65 (min)
QR T 34:
Kc: 0.237 I : 8 (min)
FR T 16:
Kc = 0.1 I: 38.467 (min)
Tuning parameter
Table 3 Controlled variables, manipulated variables, process gain matrices, relative gain array, and tuning parameters for these five systems
under temperature control
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
327
328
0.04
0.96
10
20
30
40
0
10
20
10
20
10
20
Time (hr)
10
20
R (kmol/hr)
B (kmol/hr)
60
40
0
10
20
30
10
20
30
Fpentanol (kmol/hr)
0
10
20
10
20
30
40
30
80
60
40
20
Feed +20%
Feed 20%
4
0
10
20
Time (hr)
(a) 100 wt%
30
XD,H2O (m.f.)
0.02
10
20
10
20
40
0
10
20
20
30
10
20
30
110
0
10
20
30
10
20
30
80
60
40
20
10
QR (GJ/hr)
0.6
10
100
50
30
120
100
30
150
130
140
0.99
0.98
30
60
20
30
T21 (C)
T15 (C)
20
60
20
30
80
150
ratio
20
120
30
80
Fig. 5
10
0.04
0.96
0.5
0.4
130
30
XB,acid (m.f.)
XB,acetaet (m.f.)
1
0.99
130
10
QR (GJ/hr)
ratio
1.05
20
40
110
30
80
D (kmol/hr)
T16 (C)
T34 (C)
0
0.99
0.98
30
140
150
0.93
20
60
20
30
160
0.95
10
D (kmol/hr)
60
140
80
R (kmol/hr)
B (kmol/hr)
80
20
0.02
Fpentanol (kmol/hr)
0.93
XD,H2O (m.f.)
1
0.99
XB,acid (m.f.)
XB,acetaet (m.f.)
10
20
Time (hr)
30
Feed +20%
Feed 20%
6
4
10
20
Time (hr)
(b) 75 wt%
30
Temperature control responses for 20% production rate changes for AmAc esterificaiton with different feed compositions of
acetic acid
329
0.04
0.96
10
20
30
40
20
10
20
10
20
0.24
0.22
0.2
10
20
Time (hr)
10
20
30
10
20
30
250
200
30
110
0
10
20
30
80
60
40
20
Feed +20%
15
Feed 20%
10
30
1
0.99
10
20
Time (hr)
(c) 50 wt%
30
0.96
10
20
0.02
30
10
20
40
0
10
20
150
100
30
160
10
20
T13 (C)
120
100
0
10
20
110
105
100
30
20
30
10
20
30
10
20
30
10
20
30
400
80
60
40
20
40
QR (GJ/hr)
0.13
10
500
300
30
115
140
600
D (kmol/hr)
60
0.99
0.98
30
200
R (kmol/hr)
80
1
XD,H2O (m.f.)
0.04
XB,acid (m.f.)
XB,acetaet (m.f.)
30
5
0
B (kmol/hr)
20
20
QR (GJ/hr)
ratio
0.26
T10 (C)
20
115
105
30
10
150
10
Fpentanol (kmol/hr)
130
ratio
60
0
T15 (C)
T11 (C)
135
300
120
140
0.99
0.98
30
80
30
145
Fig. 5
20
40
0
0.12
0.11
0.1
10
D (kmol/hr)
60
20
100
R (kmol/hr)
B (kmol/hr)
80
0.93
0.02
Fpentanol (kmol/hr)
0.93
1
XD,H2O (m.f.)
1
0.99
XB,acid (m.f.)
XB,acetaet (m.f.)
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
10
20
Time (hr)
30
Feed +20%
30
Feed 20%
20
10
10
20
Time (hr)
(d) 30 wt%
30
Temperature control responses for 20% production rate changes for AmAc esterificaiton with different feed compositions of
acetic acid (Continue)
330
PC1
X
TC1
FC
Organic
reflux
FT
AmOH feed
LC1
LC2
Decanter
RD
column
HAc feed
FT
Water
TC2
FC
F(x)
TC3
LC3
Steam
Reboiler
Product
331
0.04
0.96
10
20
30
40
50
20
30
20
30
QR (GJ/hr)
30
10
20
30
40
10
20
30
40
10
20
30
10
20
30
40
60
50
40
40
70
60
50
40
40
10
20
Time (hr)
30
40
5.5
10
20
Time (hr)
(a) 100 wt%
30
40
XB,acid (m.f.)
0.04
0.95
10
20
0.02
30
1
XD,H2O (m.f.)
ratio
XB,acetaet (m.f.)
10
20
R (kmol/hr)
60
50
0
10
20
10
20
T13 (C)
140
120
105
100
0
10
20
30
20
30
10
20
30
10
20
30
10
20
30
70
60
50
35
QR (GJ/hr)
0.14
10
500
400
30
110
160
600
150
100
30
0.99
0.98
30
200
70
B (kmol/hr)
20
120
110
40
T10 (C)
10
D (kmol/hr)
T16 (C)
T34 (C)
10
1.02
ratio
55
130
0.13
0.12
Fig. 7
0.99
40
70
140
0.11
30
60
40
145
100
20
Fpentanol (kmol/hr)
10
150
40
10
50
0
155
0.9
D (kmol/hr)
R (kmol/hr)
B (kmol/hr)
60
0.98
0.992
65
70
40
0.02
Fpentanol (kmol/hr)
0.94
0.994
XD,H2O (m.f.)
1
0.98
XB,acid (m.f.)
XB,acetaet (m.f.)
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
10
20
Time (hr)
30
30
10
20
Time (hr)
(b) 30 wt%
30
Feedforward control responses for 20% production rate changes for AmAc esterification with different feed compositions of
acetic acid
332
PC1
X
TC1
FC
Organic
Reflux
FT
LC1
AmOH Feed
LC2
Decanter
Water
RD
column
HAc Feed
FT
FC
TC2
LC3
Steam
Product
CC
T 15
XB, acetate
T 11
XB, acetate
T 10
XB, acetate
AmAc
(75 wt%)
AmAc
(50 wt%)
AmAc
(30 wt%)
FR =
F AmOH /F Acid
QR
FR =
F AmOH /F Acid
QR
FR =
F AmOH /F Acid
QR
FR =
FAmOH /F Acid
QR
Manipulated
variables
X B, acetate
T10
X B, acetate
T11
X B, acetate
T15
X B, acetate
T16
= 37.399 15.720
17.498 6.422
= 18.605 16.429
20.547 16.027
= 5.49 20.30
5.38 11.73
= 0.018 14.98
1.000 19.02
Q R, S
FR
Q R, S
FR
Q R, S
FR
Q R, S
FR
*Transmitter spans: twice steady-state value of temperature and 1 for mole fraction
**Valve gains: twice steady-state value for Q R and FR
T 16
XB, acetate
AmAc
(100 wt%)
Controlled
variables
FR
FR
FR
FR
6.882 7.882
= 7.882
6.882
QR
7.570 8.570
= 8.570
7.570
QR
0.371 0.629
= 0.629
0.371
QR
0.022 0.978
= 0.978
0.022
QR
RGA
T 10
X B, acetate
T 11
X B, acetate
T 15
X B, acetate
T 16
X B, acetate
Q R X B, acetate:
Kc: 1.244 I: 49.8 (min)
FR T 10:
Kc = 0.274 I: 925 (min)
Q R X B, acetate:
Kc: 0.171 I: 66 (min)
FR T 11:
Kc = 0.884 I: 979 (min)
Q R X B, acetate:
Kc: 1.561 I: 53.67 (min)
FR T 15:
Kc = 1.2 I: 422 (min)
QR XB, acetate:
Kc: 1.54 I : 54.36 (min)
FR T 16:
Kc = 0.86 I: 109.45 (min)
Tuning parameter
Table 4. Controlled variables, manipulated variables, process gain matrices, relative gain array, and tuning parameters for these five systems
under one-temperature-one-composition control.
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
333
334
0.9
10
20
30
40
0
10
20
20
150
140
0
10
20
30
0.95
0.9
30
10
20
30
10
20
30
10
20
30
80
50
40
30
30
160
T16 (C)
10
D (kmol/hr)
R (kmol/hr)
60
130
60
Fpentanol (kmol/hr)
B (kmol/hr)
80
20
0.05
10
20
60
40
20
30
80
1.2
60
ratio
0.8
1
XD,H2O (m.f.)
0.1
XB,acid (m.f.)
XB,acetaet (m.f.)
40
20
10
20
0.8
30
QR (GJ/hr)
6
5
Feed +20%
4
3
Feed 20%
0
10
20
Time (hr)
30
(a) 100 wt%
XB,acid (m.f.)
10
20
30
40
50
60
40
20
10
20
30
40
160
T15 (C)
20
30
40
140
120
0
10
20
30
40
50
0.95
0.9
50
10
20
30
40
50
10
20
30
40
50
10
20
30
40
50
150
60
40
20
50
Fpentanol (kmol/hr)
100
10
80
R (kmol/hr)
B (kmol/hr)
80
D (kmol/hr)
0.8
0.05
10
20
30
40
100
50
50
80
0.7
60
0.6
ratio
XB,acetaet (m.f.)
0.9
1
XD,H2O (m.f.)
0.1
40
0.5
20
0.4
0
10
20
30
40
50
QR (GJ/hr)
10
8
Feed +20%
Feed 20%
10
20
30
Time (hr)
40
50
(b) 75 wt%
Fig. 9
Composition control responses for 20% production rate changes for AmAc esterificaiton with different feed compositions of
acetic acid
335
W. J. Hung et al.: Control of Reactive Distillation Columns for Amyl Acetate Production Using Dilute Acetic Acid
0.9
10
20
30
40
50
10
20
30
40
0.9
50
40
20
10
20
30
40
160
140
120
0
10
20
30
40
80
60
40
50
Fpentanol (kmol/hr)
10
20
30
40
50
10
20
30
40
10
20
30
40
50
10
20
30
40
50
20
40
60
80
100
20
40
60
80
100
20
40
60
80
100
250
200
150
50
80
0.26
60
0.24
40
0.22
20
0.2
0
50
300
D (kmol/hr)
60
T11 (C)
0.95
100
R (kmol/hr)
B (kmol/hr)
80
100
0.05
ratio
0.8
1
XD,H2O (m.f.)
0.1
XB,acid (m.f.)
XB,acetaet (m.f.)
10
20
30
40
50
QR (GJ/hr)
20
Feed +20%
15
Feed 20%
10
5
10
20
30
Time (hr)
40
50
(c) 50 wt%
0.9
20
40
60
80
100
40
20
40
60
80
40
60
80
0.9
100
140
120
0
20
40
60
80
100
600
150
100
100
Fpentanol (kmol/hr)
160
T10 (C)
20
D (kmol/hr)
60
100
0.95
200
R (kmol/hr)
B (kmol/hr)
80
20
0.05
20
40
60
80
500
400
300
100
80
0.13
60
0.12
ratio
0.8
1
XD,H2O (m.f.)
0.1
XB,acid (m.f.)
XB,acetaet (m.f.)
40
20
0.11
0
20
40
60
80
100
0.1
QR (GJ/hr)
40
30
Feed +20%
Feed 20%
20
10
20
40
60
Time (hr)
80
100
(d) 30 wt%
Fig. 9
Composition control responses for 20% production rate changes for AmAc esterificaiton with different feed compositions of
acetic acid (Continue)