Extractive Distillation of Acetone/Methanol Mixture Using Water As Entrainer
Extractive Distillation of Acetone/Methanol Mixture Using Water As Entrainer
Extractive Distillation of Acetone/Methanol Mixture Using Water As Entrainer
The acetone-methanol extractive distillation using water as an entrainer was simulated on Aspen Plus software
package using rigorous methods. Calculation of the vapor-liquid equilibrium for the ternary system was
done by the UNIQUAC model according to the experimental results obtained in a previous work. The effects
of the solvent to feed molar ratio, reflux ratio, feed stage, feed solvent stage, and solvent feed temperature
were studied to obtain the best design of the extractive distillation column with minimal energy requirements.
The most appropriate configuration is 52 theoretical stages. The best binary mixture and entrainer feeding
stages were obtained at 48 and 22 respectively with a solvent to feed molar and reflux ratio of 2.0 and 5.0,
respectively. The simulation results show the effect of the main variables on the extractive distillation process.
Figure 3. Pseudo-binary x-y plot for the acetone (1)-methanol (2) system
with an entrainer to feed molar ratio 3. Solid and dashed lines predicted by
UNIQUAC model for the pseudo-binary and binary systems, respectively.
Figure 5. Number of stages and reflux ratio influence on the distillate Figure 7. Number of stages and reflux ratio influence on the reboiler duty.
acetone mole composition. Operational conditions: BFS 48, EFS 22, EFT Operating conditions: BFS 48, EFS 22, EFT 47 C, and E/F 2.0. Evaluated
47 C, and E/F 2.0. Evaluated refluxes: 3.0 ( ), 4.0 (), 5.0 (), 6.0 (]), refluxes: 3.0 ( ), 4.0 (), 5.0 (), 6.0 (]), and 7.0 (0).
and 7.0 (0).
Figure 6. Number of stages and reflux ratio influence on the condenser Figure 8. Binary feed stage and reflux ratio influence on the distillate acetone
duty. Operating conditions: BFS 48, EFS 22, EFT 47 C, and E/F 2.0. mole composition. Operating conditions: NS 52, EFS 22, EFT 47 C, and
Evaluated refluxes: 3.0 ( ), 4.0 (), 5.0 (), 6.0 (]), and 7.0 (0). E/F 2.0. Evaluated refluxes: 3.0 ( ), 4.0 (), 5.0 (), 6.0 (]), and 7.0 (0).
binary feed stage (BFS), entrainer feed stage (EFS), entrainer Figure 8 shows the results of the reflux ratio and the binary
feed temperature (EFT), and entrainer to feed molar ratio (E/ feed stage analysis. As can be seen, at reflux rates between 3.0
F). The binary mixture was fed in the extractive distillation and 5.0 were obtained the greatest distillate compositions, with
column at azeotropic composition. a difference among them no higher than 0.02. However,
Figure 5 shows the influence of the reflux ratio and the differences on distillate acetone mole composition at reflux ratios
number of stages on the distillate mole composition (xD). higher than 5.0 were around 0.10. The highest distillate acetone
According to the ASTM purity standard specification for acetone composition was reached when the binary mixture was fed
is 99.5% mass (99.0% mol), this specification can be achieved between the 46 and 48 stages. Because of longer contact time
using refluxes among 3.0 and 5.0. The highest xD was obtained between the azeotropic mixture and the solvent, higher purity
at a reflux of 4.0. It is observed that an increase of reflux causes in the distillate, the azeotropic mixture was fed near to the
a decrease in the distillate. This is because high reflux causes column bottoms.
the dilution of the liquid phase, which should be rich in solvent. Figure 9 presents the influence of the binary feed stage on
From Figure 5, is also possible to observe that with a number the distillate composition and energy duty. From the above
analysis, the reflux ratio was kept constant (5.0). At stages
of stages greater than 52 the composition of the distillate does
greater than 42, the condenser and reboiler duties and distillate
not change significantly. Results show that the column may have
composition did not change significantly (Figure 9). Hence, a
52 stages and be operated at a reflux rate between 3.0 and 5.0.
feasible binary feed location is at stage 48 because the binary
The effect of reflux ratio and number of stages on the mixture-entrainer contact time is kept long. It is also possible
condenser (QC) and reboiler (QR) duties is presented in Figures to observe that reboiler duty was greater than condenser duty.
6 and 7, respectively. For both cases, duties did not change with The increased energy consumption is produced when the binary
the number of stages. Nevertheless, reflux rate had an important mixture is fed as a saturated liquid near to the reboiler. At stage
influence on the column energy consumption. Heating and 22, the reboiler and condenser duties decline; this is caused by
cooling requirements presented a direct proportional relationship the entrainer feeding.
with the reflux ratio. From the sensitivity analysis, it is possible The reflux ratio and the entrainer feed stage effect on distillate
to conclude that at a reflux ratio of 5 the energy consumption acetone composition are presented in Figure 10. It is noticed
and distillate composition requirements are satisfied. that the highest acetone compositions in the distillate were
Ind. Eng. Chem. Res., Vol. 48, No. 10, 2009 4861
Figure 11. Entrainer feed stage effect on distillate composition (), and
Figure 9. Binary feed stage effect on distillate composition () and energy
energy duty (condenser O, and reboiler 0). Operating conditions: NS 52,
duty (condenser O, reboiler 0). Operating conditions: NS 52, EFS 25, EFT
BFS 48, EFT 47 C, R 5.0, and E/F 2.0.
47 C, R 5.0, and E/F 2.0.
Figure 12. Entrainer to feed molar ratio and reflux ratio influence on the
Figure 10. Entrainer feed stage and reflux ratio influence on the distillate distillate acetone mole composition. Operating conditions: NS 52, BFS 48,
acetone mole composition. Operating conditions: NS 52, BFS 48, EFT 47 EFS 22, and EFT 47 C. Evaluated refluxes: 3.0 ( ), 4.0 (), 5.0 (), 6.0
C, and E/F 2.0. Evaluated refluxes: 3.0 ( ), 4.0 (), 5.0 (), 6.0 (]), and (]), and 7.0 (0).
7.0 (0).
obtained at reflux ratios of 4.0 and 5.0, and that, at greater values Because of higher E/F ratios, the entrainer dilution caused by
of entrainer feed stage, acetone composition in the distillate was the reflux is small and the purity of distillate increases.
lower. This is due to the interaction between entrainer and At entrainer to feed molar ratios of 2.5 or higher, the distillate
azeotropic mixture components that occur predominantly in the composition remained constant (Figure 12). For all of the
liquid phase. When the solvent is fed in the top, it is possible evaluated E/F range, the condenser duty remained constant.
to guarantee that the entrainer is present in the liquid phase in However, the reboiler duty presented significant changes with
all of the stages below. From these results, at stage 22 was the increased E/F. This is associated with higher E/F values
obtained the highest acetone concentration, and then this is a owing to larger liquid volumes needed for vaporization;
feasible stage to feed the solvent. therefore the energy consumption in the reboiler is increased.
The energy consumption was less when the solvent was fed An optimal value could be 2.0 because with this value it was
at stages near to the top of the column (Figure 11). This could possible to obtain high acetone purity and lower energy
be owed to the higher entrainer contact with the vapor phase consumptions (Figure 13). Also, a rise of the inlet entrainer
that caused a higher methanol transferred to the liquid phase. temperature increased acetone composition in distillate when
Therefore, the flow to the reboiler is greater. If the solvent is the reflux ratio was higher than 4.0 (Figure 14). However, at
fed near to the bottoms, a minimal quantity of methanol leaves temperatures higher than 50 C the increase of the distillate
the vapor phase so the flow to the condenser and the energy composition was not significant. With respect to reflux ratio, it
consumption increases. Binary mixture feeding caused an was observed that the highest distillate acetone composition was
increase on reboiler and condenser duties. For that reason, in obtained at reflux rates of 4.0 and 5.0 (Figure 10), whereas at
proximity to stage 48 an increase on reboiler and condenser higher reflux rates acetone concentration in distillate decreases.
duties was observed. The influence of the entrainer feed stage This could be associated with the solvent feed stage. When it
on the distillation composition showed that acetone composition is fed near to the top of the column, it is mixed with the reflux,
in the distillate is higher with the decrease of the entrainer feed which causes the dilution of the entrainer and, therefore, the
stage. At stage 22, the composition of the distillate had a effectiveness decreases.
maximum value. This result agrees with those results presented When the entrainer feed temperature was varied in the range
in Figure 10. As can be seen on Figure 12, at high reflux rates of 20 to 100 C, no effect on the distillate composition and
and E/F ratio the distillate acetone composition was greater. condenser duty was observed (Figure 15). Nevertheless, the
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Figure 13. Entrainer to feed molar ratio effect on distillate composition Figure 16. Reflux ratio effect on distillate composition (), and energy
(), and energy duty (condenser O, and reboiler 0). Operating conditions: duty (condenser O, and reboiler 0). Operating conditions: NS 52, BFS 48,
NS 52, BFS 48, EFT 47 C, and R 5.0. EFS 22, EFT 47 C, and E/F 2.0.
Figure 15. Entrainer feed temperature influence on distillate composition liquid phase and the liquid flow to the bottoms is lower. Figure
(), and energy duty (condenser O, and reboiler 0). Operating conditions: 16 shows the effect of reflux ratio on distillate composition,
NS 52, BFS 48, EFS 22, EFT 47 C, R 5.0, and E/F 2.0. and condenser and reboiler duties.
Finally, the pressure drop effect on acetone final composition
reboiler energy consumption was significantly affected by the is presented in Figure 17. The plot shows how the liquid profile
inlet entrainer temperature. The reboiler duty decreased with composition in the extractive column was affected by a pressure
the increase of the entrainer feed temperature because if entrainer drop neglected and P ) 0.01 atm. The other operating
is fed at low temperatures more energy is required to vaporize conditions were established above. When P ) 0 psi, distillate
the liquid in the bottoms. When the solvent is fed at higher acetone composition was higher than the obtained when the
temperatures, small amounts of methanol are transferred to the column had a P of 0.01 atm per stage. This is because when
Ind. Eng. Chem. Res., Vol. 48, No. 10, 2009 4863
Figure 18. Process flow-sheet for extractive distillation of acetone-methanol using water as an entrainer.
Table 4. Feed Streams Conditions Table 7. Condenser and Reboiler Heat Duties on the Columns
stream 1 4 extractive column recovery column
feed mole flow (kmol/h) 100 1 condenser (kW) -3748 -975
temperature (C) 20 47 reboiler (kW) 3858 987
pressure (atm) 1 1
mole fraction the same conditions of energy supply the separation efficiency
acetone 0.7775 0 will be lower when a pressure drop is not neglected.
methanol 0.2225 0
water 0 1
Configuration and operating conditions of the primary column
was established from results obtained with the sensitivity
Table 5. Configuration of Extractive and Recovery Columns
parameter extractive column recovery column
number of stages 52 26
feed stage 48 14
entrainer feed stage 22
reflux ratio 5 3
condenser total total
top stage pressure (atm) 1 1
pressure drop per stage (atm) 0.01 0.01
distillate mole flow (kmol h-1) 76 25
a pressure drop is present in the column more energy is required Figure 20. Liquid () and vapor (0) molar flow profiles in the extractive
to drive the vapor up through the distillation column, thus at column.
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