Luyben 2008 Comparison of Extractive Distillation and Pressure Swing Distillation For Acetone Methanol Separation
Luyben 2008 Comparison of Extractive Distillation and Pressure Swing Distillation For Acetone Methanol Separation
Two of the most common methods for separating a binary homogeneous azeotrope are pressure-swing
distillation and extractive distillation. The former is effective if the composition of the azeotrope changes
significantly with pressure. The latter method is effective if a suitable solvent can be found. This paper compares
the steady-state design and the dynamic control of these two methods when applied to the acetone-methanol
binary system. The minimum-boiling azeotrope at 1 atm contains 77.6 mol % acetone at 328 K. At 10 atm
the azeotropic composition is 37.5 mol % acetone at 408 K, so pressure-swing separation is feasible. Extractive
distillation is also feasible using water as the solvent. Both systems require two distillation columns. Purities
of the two products are set at 99.5 mol %. Results show that the extractive distillation system has a 15%
See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.
lower total annual cost. However, a third component (water) is introduced that appears as trace impurities in
both the acetone and methanol products. It is also much more difficult to attain higher purities in the extractive
distillation system than in the pressure-swing system because of ternary vapor-liquid equilibrium constraints.
The dynamic controllabilities of the two alternative processes are quite similar. Steady-state designs and
Downloaded via FH FRANKFURT on July 30, 2025 at 13:21:42 (UTC).
control structures are also developed for the two methods when the columns are heat integrated. Heat integration
is straightforward in the pressure-swing system because the condenser temperature in the high-pressure column
is 60 K higher than the base temperature in the low-pressure column. In the extractive distillation system, the
pressure in the second solvent recovery column must be increased from 1 to 5 atm to provide the necessary
temperature differential driving force.
Figure 1. (A) Txy diagrams for acetone-methanol at 1 and 10 atm. (B) Residue curve map for acetone-methanol-water.
composition specification is 99.5 mol % methanol, and the high-pressure column. The optimum feed stage locations are
distillate composition specification is 75 mol % acetone (2.5 determined by finding the feed trays that minimized reboiler
mol % lower than the azeotrope at 1 atm). In the high-pressure heat input. Figures 3 and 4 give temperature and composition
column, the bottoms composition specification is 99.4 mol % profiles in the two columns.
actone and the distillate composition specification is 40 mol % The first column in Table 1 gives design parameters and
acetone (2.5 mol % higher than the azeotrope at 10 atm). economic data for this pressure-swing distillation system.
The minimum reflux ratios are found with 103 stages to be Column diameters are found using Aspen Tray Sizing. The
2.3 and 3.08 in the low- and high-pressure columns, respectively. relationships given in Luyben11 are used for sizing condensers
The number of stages required for reflux ratios about 1.2 times and reboilers and for calculating capital cost of equipment.
these minima are 52 in the low-pressure column and 62 in the Temperature differentials are 34.8 K in reboilers. In condensers,
2698 Ind. Eng. Chem. Res., Vol. 47, No. 8, 2008
3. Acetone-Methanol Separation Using Extractive 3.1 Steady-State Design. The Knapp-Doherty optimum
Distillation design had a 57-stage extractive column and a 26-stage methanol
column, both operating at 1 atm. They do not provide informa-
Knapp and Doherty9 present the economic optimum design
tion about feed tray locations, so these were found empirically
of an acetone-methanol separation using water as the extractive
solvent. The design used in this paper is based on their work. by finding what locations give minimum energy consumption.
Using extractive distillation has the inherent disadvantage of Note that the solvent is fed to the extractive column on a tray
introducing a third component into the system that will appear above the feed tray and below the top of the column so that
as impurity in the product streams. So the extractive system high-purity acetone can be produced in the distillate.
must show significant economic and/or control advantages over Figure 7 shows the flowsheet used in this paper with stream
the pressure-swing system to make it the process of choice. information, heat duties, equipment sizes, and operating condi-
2700 Ind. Eng. Chem. Res., Vol. 47, No. 8, 2008
Table 3. Design Results for Heat-Integrated Systems In this section we compare the steady-state design and the
pressure swing extractive dynamic control of heat-integrated extractive and pressure-swing
with heat with heat processes. The same numbers of trays used in the base-case
integration integration designs are used in both systems. The systems have not been
C1 Nstage 52 57 re-optimized for heat integration.
ID (m) 3.30 2.79 3.1. Heat-Integrated Extractive Distillation Process. 3.1.1.
QCR (MW) 5.86 9.31
QAUX (MW) 8.93 2.10
Design. Figure 15 gives the flowsheet for the revised extractive
QC (MW) 15.1 9.87 distillation process in which the pressure in the methanol column
QHX (MW) - 1.35 is increased from 1 to 5 atm. This raises the reflux-drum
Treflux (K) 328 329 temperature to 385 K with the 99.5 mol % methanol distillate.
ARC (m2) 110 514 The base of the extractive column is 364 K, so there is a
AC (m2) 982 609
AHX (m2) - 52.7 reasonable 21 K differential temperature driving force to size
AAUX (m2) 450 106 the reboiler/condenser heat exchanger.
shell (106 $) 1.13 1.02 The higher pressure in the methanol column requires a higher
condenser (106 $) 0.643 0.567 reflux ratio and more heat input than the low-pressure operation
condenser/reboiler (106 $) 0.155 0.421
aux reboiler (106 $) 0.388 0.151 because the higher pressure makes the separation more difficult.
cooler HX (106 $) - 0.096 The reflux ratio increases from 1.61 to 2.91, and the reboiler
aux condenser (106 $) - ? heat input increases from 7.1 to 11.4 MW.
total capital (106 $) 1.58 2.26 The condenser duty in the methanol column is now 9.31 MW,
energy ($106/yr) 1.32 0.311
C2 Nstage 62 26 which can be used to produce vapor in the base of the extractive
ID (m) 1.89 1.61 column. The total energy needed in the extractive column is
QR (MW) 7.59 11.3 11.4 MW, so an auxiliary steam-driven reboiler is required with
AC (m2) - - a duty of 2.1 MW. The extractive column itself is unchanged
AR (m2) 383 570
shell (106 $) 0.722 0.292
except it has two reboilers.
condenser (106 $) - - The reboiler/condenser is sized by using an overall heat
reboiler (106 $) 0.349 0.451 transfer coefficient of 0.00306 GJ h-1 m-2 K-1. The heat transfer
total capital (106 $) 1.07 0.743 rate is 33.53 GJ/h (9.31 MW) and the temperature difference is
energy ($106/yr) 1.13 1.67
total total capital (106 $) 2.65 3.00
21.2 K, giving an area of 514 m2.
system The second column in Table 3 gives sizing and cost
total energy ($106/yr) 2.45 1.98 information. Notice that the diameter of the methanol column
TAC ($106/yr) 3.33 2.98 (1.61 m), which is operating at 5 atm, is smaller than the
diameter in the non-heat-integrated case at 1 atm (1.89 m),
3. Heat-Integrated Systems despite having a larger reboiler heat input (11.3 versus 7.59
The studies reported above have considered systems with MW). The larger vapor density at higher pressure results in a
independent reboilers and condensers on both columns. The smaller diameter column.
large differences in the temperature between the high- and low- The TAC of the heat-integrated extractive system is $2,980,-
pressure columns in the pressure-swing process make heat 000 per year. This should be compared with the base-case TAC
integration a natural. In the extractive process, Knapp and of $3,750,000 per year. Total capital investment is essentially
Doherty9 suggest raising the pressure in the methanol column the same in the base and heat-integrated designs ($3,000,000),
so that its overhead vapor can be condensed in the reboiler of while energy cost is reduced from $2,720,000 to $1,980,000.
the extractive column. They point of that the alternative of 3.1.2. Control. Implementing heat integration in Aspen
raising the pressure in the extractive column is infeasible because Dynamics requires the used of Flowsheet Equations. The method
of distillation boundaries that occur in the ternary diagram at for simulating heat integration in distillation systems is discussed
higher pressures. in detail in a recent paper.8
Figure 16. Aspen Dynamics flowsheet equations for heat integration and pressure-compensated temperature in high-pressure column.
Ind. Eng. Chem. Res., Vol. 47, No. 8, 2008 2705
Figure 17. Control structure for extractive distillation system with heat integration.
Figure 18. Control structure for pressure-swing distillation system with heat integration.
There are two conditions that must be satisfied at each point in the reboiler/condenser QRC must be equal to the product of
in time during the dynamic simulation: (1) The heat transfer the fixed area ARC, the fixed heat-transfer coefficient U and the
2706 Ind. Eng. Chem. Res., Vol. 47, No. 8, 2008
Figure 19. (A) Comparison of extractive distillation and pressure-swing systems with heat integration; feed flowrate disturbances. (B) Comparison of
extractive distillation and pressure-swing systems with heat integration; feed composition disturbances.
temperature difference between the condenser temperature in that have been made from the base-case control structure: (1)
the methanol column and the base temperature in the extractive The output signal from the TC1 controller in the extractive
column. This heat transfer rate is the heat removed in the column is the auxiliary heat input QAUX, which is 7.61 GJ/h
condenser of the methanol column. (2) The total heat transfer (note Aspen uses metric units). (2) The PC2 pressure controller
in the base of the extractive column is the sum of the heat in the methanol column has no input signal and is on manual.
removed in the condenser of the methanol column QRC and the (3) The deadtime element “dead2” has no input shown in Figure
heat added in the auxiliary reboiler QAUX in the extractive 17, but its input signal is the pressure-compensated temperature
column. signal as defined in the flowsheet equation given in Figure 16A.
These conditions correspond to the first and second laws of The temperature and pressure on Stage 21 in the methanol
thermodynamics. Figure 16A shows the flowsheet equations for column are measured, and a “pressure-compensated” temper-
the extractive heat-integrated system. The two conditions listed ature13 TPC is fed into the deadtime element as its input signal.
above are specified in the top two equations in the Text Editor The design pressure on Stage 21 is 5.136 atm with a composition
window. of 45 mol % methanol and a temperature of 396.19 K.
The third equation is used to provide a “pressure-compen- Generating a Txy diagram at 6 atm gives a temperature of
sated” temperature13 measurement in the methanol column. This 401.66 K at the same composition. The following equation is
is needed because in the heat-integrated system the pressure in used to calculate the signal fed to the deadtime element
the methanol column is not controlled. It floats with operating and subsequently into the temperature controller as the PV
conditions. If more heat transfer is required in the reboiler/ signal.
condenser, a larger temperature difference is required, and this
- 396.19
is achieved by the pressure in the methanol column increasing,
which raises the bubblepoint temperature in the reflux drum.
TPC ) T21 - (P21 - 5.136) (401.66
6 - 5.136 )
Figure 17 shows the control structure for the heat-integrated The two temperature controllers are tuned using the methods
extractive system. The three block arrows point to the changes discussed above. Tuning parameters are given in Table 2.
Ind. Eng. Chem. Res., Vol. 47, No. 8, 2008 2707
Remember that the temperature controller in the extractive handle this disturbance. In the Aspen Dynamics simulation this
column is manipulating the energy input QAUX from the auxiliary is easily achieved by specifying the minimum controller output
reboiler (2.10 MW or 7.6 GJ‚h as given in the TC1 faceplate signal of TC1 to have a negative value (-30 GJ/h as shown in
in Figure 17). Table 2). The additional capital cost of an auxiliary condenser
The effectiveness of this control structure on the heat- is not included in the economic data shown in Table 3.
integrated extractive distillation system is compared with that
of the heat-integrated pressure-swing distillation system in the 4. Conclusion
following section.
Steady-state and dynamic comparisons have been presented
3.2. Heat-Integrated Pressure Swing Process. The heat-
of an extractive distillation process and a pressure-swing
integrated flowsheet in the pressure-swing system is essentially
distillation process. The extractive system has lower costs and
the same as without heat integration. The only change is that
equivalent dynamics compared to the pressure-swing process.
there is a reboiler/condenser and an auxiliary steam-heated
However, it is more difficult to achieve high product purities.
reboiler on the low-pressure column. The temperature difference
In addition, the introduction of a third component can lead to
between the condenser of the high-pressure column and the base
impurity issues in the products.
of the low-pressure column is quite large (407.5 - 345.3 )
Using heat integration reduces energy costs. Capital costs in
62.2 K). The heat duty in the condenser of the high-pressure
the extractive system are essentially the same with and without
column is 5.86 MW, which gives a heat-transfer area of 110
heat integration. In the pressure-swing system, the capital cost
m2.
of the heat-integrated process is actually lower than the base-
The first column in Table 3 gives process and economic data
case process. This is the result of lower reboiler capital cost
for this process. The TAC of the heat-integrated pressure-swing
because of the smaller areas that result from the large temper-
system is $3,330,000 per year. This should be compared with
ature difference between the top of the high-pressure column
the base-case TAC of $4,520,000 per year and the heat-
and the base of the low-pressure column.
integrated extractive process of $2,980,000 per year. Total
In the heat-integrated system, the pressure in the high-pressure
capital investment is unexpectedly smaller than for the base
column changes with operating conditions, so a pressure-
design ($3,330,000 instead of $3,510,000). This is the result of
compensated temperature control structure is required to main-
the small reboiler/condenser due to the large temperature driving
tain product specification in these columns.
force. The energy cost is reduced from $3,350,000 to $2,450,000
per year.
The energy requirement in the low-pressure column is 14.79 Literature Cited
MW, so the auxiliary reboiler must provide 14.79 - 5.86 ) (1) Grassi, V. G. Process design and control of extractive distillation,
8.93 MW (32 GJ/h, as shown in the TC1 faceplate in Figure Practical Distillation Control; Van Nostrand Reinhold: New York, 1992;
18). Similar flowsheet equations are needed in this system and p 370.
are given in Figure 16B. The pressure-compensated temperature (2) Chien, I. L.; Wang, C. J.; Wong, D. S. H.; Lee, C. H.; Cheng, S. H.;
Shih, R. F.; Liu, W. T.; Tsai, C. S. Experimental investigation of
measurement uses the temperature (412.9 K) and pressure conventional control strategies for a heterogeneous azeotropic distillation
(10.354 atm) on Stage 53. column. J. Process Control 2000, 10, 333.
(3) Chien, I. L.; Zeng, K. L.; Choa, H. Y. Design and control of a
- 411.51
TPC ) T53 - (P53 - 10.354) (414.26
11 - 10.354 )
complete heterogeneous azeotropic distillation column system. Ind. Eng.
Chem. Res. 2004, 43, 2160-2174.
(4) Arifin, S.; Chien, I. L. Design and control of an isopropyl alcohol
dehydration procee via extractive distillation using dimethyl sulfoxide as
Figure 18 gives the control structure developed for the heat- an entrainer. Ind. Eng. Chem. Res. 2008, 47, 790-803.
integrated pressure-swing process. (5) Luyben, W. L. Control of a multi-unit heterogeneous azeotropic
Figure 19 gives a direct comparison of the two alternative distillation process. AIChE J. 2006, 52, 623-637.
heat-integrated processes for feed flowrate and feed composition (6) Luyben, W. L. Plantwide control of an isopropyl alcohol dehydration
process. AIChE J. 2006, 52, 2290-2296.
disturbances. The solid lines are for the pressure-swing system. (7) Abu-Eishah, S. I.; Luyben, W. L. Design and control of a two-column
The dashed lines are for the extractive system. Both systems azeotropic system. Ind. Eng. Chem. Process Des. DeV. 1985, 24, 132-
provide stable base-level regulatory control. The results are quite 140.
similar to those found in the non-heat-integrated systems. (8) Luyben, W. L. Design and control of a fully heat-integrated pressure-
swing azeotropic distillation system, Tuning of PI controllers for integrator/
These results show that there is no control penalty for going deadtime processes. Ind. Eng. Chem. Res. 2008, 41, 2681-2695.
to the heat-integrated systems. This result is to be expected (9) Knapp, J. P., Doherty, M. F. Thermal integration of homogeneous
because only partial heat integration is used so there is no loss azeotropic distillation sequences. AIChE J. 1990, 36, 969-984.
of control degrees of freedom. Similar results were found in a (10) Kossack, S.; Kraemer, K.; Gani, R.; Marquardt, W. A systematic
previous paper.8 synthesis framework for extractive distillation processes. Chem. Eng. Res.
Des. 2008, submitted.
One comment should be made about the extractive heat- (11) Luyben, W. L. Distillation Design and Control using Aspen
integrated system. A close look at the flowsheet in Figure 15 Simulation; Wiley: New York, 2006; p 88.
will disclose an auxiliary condenser on the extractive column (12) Tyreus, B. D.; Luyben, W. L. Tuning of PI controllers for integrator/
in addition to an auxiliary reboiler. When the feed composition deadtime processes. Ind. Eng. Chem. Res. 1992, 31, 2625-2628.
(13) Buckley, P. S.; Luyben, W. L.; Shunta, J. P. Design of Distillation
disturbance from 50 to 40 mol % acetone is introduced into the Column Control Systems; Instrument Society of America: Research Triangle
system, the large production rate of methanol increases the Park, NC, 1985; p 234.
reboiler heat input in the methanol column, causing the heat
input in the auxiliary reboiler in the extractive column to be ReceiVed for reView December 11, 2007
driven to zero. The system is unable to maintain acetone product ReVised manuscript receiVed February 8, 2008
Accepted February 13, 2008
purity because the temperature in the extractive column becomes
too high. Thus, an auxiliary condenser would be needed to IE701695U