DISTILLATION OF ETHANOL

AND WATER MIXTURE

By:
Zed Daliela Zulkafli
Tracy Elizabeth Grant
Andrew Lossing

Advisors:
PROF. BRIDGET ROGERS
PROF. JULIE SHARP

ChBE 229w
Fall 2009
December 10, 2009
 Executive Summary

The binary distillation of ethanol and water is made possible due to the difference
in volatilities of the components in the boiling liquid mixture. In this experiment, a
continuous distillation unit consisting of a perforated-tray column filled with packing of
IMTP #15 together with a partial reboiler and a total condenser. This column was used to
find the specifications and optimum operating conditions needed to produce 100 barrels
of strong, 80% mole of ethanol blend beverage from an 8% mole of ethanol mixture
everyday.

In the experiment, all the feed, distillate, bottom, and reflux flow-meters were
calibrated, taking into consideration that the flow meters provide accurate measurements
only for water flows. The refractometer was calibrated to enable the determination of the
concentration of ethanol in any given ethanol and water mixture from the refractive
index. The relationship between the mole composition of ethanol, xEtOH in the mixture to
the density of the mixture, ρ was found to be: ρ = 155.3*exp(-3.1752* xEtOH) +
843.4*exp(-0.05741*xEtOH). The relationship between the density of the mixture and the
composition of ethanol is no longer linear once it reaches higher concentration.
V H O (22 Xs + 18 ) ρ H O
Therefore, the equation: Xs = X diluted [1 + (2
+ * 2
)] was used to
Vs 18 ρs
determine the initial ethanol composition of a diluted sample.

The experiment was done by varying the reflux ratio at 6.72 and 7.31, with having
the feed come in the middle stage. Then we kept the reflux ratio at 6.72 and varied the
feed stage which are the middle and the bottom stage. The actual number of stages of the
column used in the lab is 5 stages. To find the number of theoretical stages required for
the stage, the results from the distillation process was analyzed using the McCabe-Thiele
method. By comparing these values, the efficiency of the column was found from the
equation: Efficiency = (# Theoretical stages/# Actual stages). Once up-scaling calculation
was done, we used the new theoretical number of stages to run a simulation in Aspen for
the binary distillation process. Data from the experiment were used as process conditions
to find the heat duty of both the reboiler and the condenser.

When the reflux ratio was set to be 6.72, the purity of ethanol was extremely high,
which shows that the column has very high efficiency. However, because the value was
out of the range provided in the ethanol/water equilibrium curve, it was impossible to
determine the percent efficiency. This high purity gain might be due to the small amount
of the distillate produced. This occurred because it was difficult to maintain the flow rate
of the distillate at the specified value gained from Aspen.

The data from the experiment shows that the optimum specification for the
process is to have the feed enter the column from the middle and a reflux ratio of 7.31.
Even though a higher mole fraction of ethanol was obtained when the feed was at the
bottom, the amount of distillate produced was lower compared to the one when it is fed in
the middle. Moreover, the mole fraction gained from the latter was sufficient with what is
required. With this, the cost is saved, where we have a smaller amount of feed needed to
produce the same amount of the beverage.

In conclusion, a higher reflux ratio results in a higher production rate, and the
optimum stage feed is at the middle of the column. To obtain a concentration of 80%
mole ethanol in the distillate, the number of stages was found to be 8 stages, based on the
efficiency gained from the data (RR:7.31, feed stage: 3), which was 80%. The distillation
column was calculated to be 12.8 meters, which is an appropriate measurement for a real
time operating reactor.
Calibration curve for the 4 flow-meters and refractometer

Feed Calibration Curve

2.5
Actual Flow Rate (mL/s)

1.5

1 y = 0.0138x + 0.1248
R2 = 0.9985
0.5

0
0 20 40 60 80 100 120 140 160
Flowmeter Reading
Figure 1: Linear relationship between feed flow rate and the flow meter reading

Distillate Calibration Curve

0.8
0.7
Actual Flow Rate (mL/s)

0.6
0.5
0.4
0.3 y = 0.0052x + 0.0257
0.2 R2 = 0.9996

0.1
0
0 20 40 60 80 100 120 140
Flowmeter Reading
Figure 2: Linear relationship between distillate flow rate and the flow meter reading
 Bottoms Calibration Curve

8
7
Actual Flow Rate (mL/s)

6
5
4 y = 0.0607x - 0.5528
3 R2 = 0.999
2
1
0
0 20 40 60 80 100 120 140
Flowmeter Reading
Figure 3: Linear relationship between bottom flow rate and the flow meter reading

Total Flow Calibration Curve

4
3.5
Actual Flow Rate (mL/s)

3
2.5
2 y = 0.0246x - 0.0054
R2 = 0.9994
1.5
1
0.5
0
0 20 40 60 80 100 120 140 160
Flowmeter Reading
Figure 4: Linear relationship between total flow rate and the flow meter reading
 Refractometer Calibration Curve
refractometer reading (nD) 1.36

1.355

1.35 y = 0.0012x + 1.3337

R2 = 0.9896
1.345

1.34

1.335

1.33
0 5 10 15 20 25
mole percent of ethanol %
Figure 5: Linear relationship between refractometer reading and ethanol mole percent
 Density Calibration Curve

1000
980
960
Density (kg/m^3)

940
920
900
880
860
840
820
800
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
Ethanol Mole Fraction
Figure 6: Relationship between the density and the ethanol mole fraction in a binary
mixture

Sensitive analysis on Reflux Ratio (RR)

Sensitive Analysis on RR
0.68
Mole Fraction EtOH in Distillate

0.67
0.66
0.65
0.64
0.63
0.62

0.61
0.6
0 2 4 6 8 10 12 14 16
Reflux Ratio
Figure 7: Relationship between mole fraction of ethanol in the distillate and the specified
reflux ratio
Appendix

Table 1: Data for calibration curve of four flow-meters of streams entering and exiting column
Total
Feed Bottoms Distillate
Flow
Actual Actual Actual Actual
Flowmeter Volume Volume Volume Volume
Time (s) Flow Time (s) Flow Time (s) Flow Time (s) Flow
Reading (mL) (mL) (mL) (mL)
(mL/s) (mL/s) (mL/s) (mL/s)
10 30 131.5 0.228 26 182.97 0.142 26 343.13 0.076 26 111.07 0.234
40 30 43.94 0.683 50 27.5 1.818 26 110.45 0.235 70 74.25 0.943
70 140 124.03 1.129 70 19.19 3.648 30 78.62 0.382 70 39.94 1.753
100 130 85.15 1.527 110 20.28 5.424 60 109.41 0.548 110 44.03 2.498
130 90 47.09 1.911 150 20.16 7.440 50 72.13 0.693 110 34.66 3.174
150 90 41.56 2.166 130 35.5 3.662

Table 2: Data for calibration curve of refractor

mole percent refractometer reading (nD)
T (oC)
(EtOH) trial 1 trial 2 Average
5 1.3404 1.3402 1.3403 21.1
10 1.3477 1.3476 1.3477 21.1
15 1.3521 1.3514 1.3518 21.1
20 1.3582 1.358 1.3581 21.1
0 1.3327 1.3328 1.3328 21.1
Table 3: Data from Aspen for calibration curve of density of ethanol mixture

ETOH
ETOH mole flow [with 1 DENSITY
mole FIT
kmol/hr H2O] (kmol/hr) (kg/cum)
fraction
0 998.7672 0 998.7
0.25 915.78773 0.2 916.0672
0.5 881.55706 0.333333 881.3043
0.75 863.0296 0.428571 862.7295
1 851.47748 0.5 851.2801
1.25 843.61818 0.555556 843.5366
1.5 837.94343 0.6 837.9523
1.75 833.66438 0.636364 833.733
2 830.32907 0.666667 830.4308
2.25 827.66037 0.692308 827.7746
2.5 825.47918 0.714286 825.5906
2.75 823.66479 0.733333 823.7624
3 822.13297 0.75 822.209
3.25 820.82322 0.764706 820.8725
3.5 819.69102 0.777778 819.71
3.75 818.70291 0.789474 818.6895
4 817.83327 0.8 817.7864
4.25 817.06217 0.809524 816.9813
4.5 816.37388 0.818182 816.259
4.75 815.75583 0.826087 815.6074
5 815.19783 0.833333 815.0164

Table 4: Data from Aspen for sensitive analysis on Reflux Ratio (RR)
RR Mole Fraction ETOH in Distillate
0.5 0.60689154
1 0.63111669
1.5 0.64327581
2 0.65059548
2.5 0.65564087
3 0.65913983
3.5 0.6617769
4 0.66383625
4.5 0.66548926
5 0.66684557
5.5 0.66797773
6 0.66893856
6.5 0.66976362
7 0.67054299
7.5 0.67116715
8 0.67171735
8.5 0.6722068
9 0.67264508
 9.5 0.67303985
10 0.67339729
10.5 0.67372248
11 0.67401959
11.5 0.67429214
12 0.67454304
12.5 0.67477478
13 0.67498948
13.5 0.67518896
14 0.67537479
14.5 0.67536759
15 0.67555142

Data from distillation column until steady state was reached

Table 5.1: Distillate composition of ethanol when feed enters at stage 3 and RR is 4
distillate
samples EtOH mol % Xd refractometer reading (nD) Xud change
1 13.4167 0.1342 1.3498 0.7668 -
2 13.5833 0.1358 1.35 0.7835 0.017
3 13.2500 0.1325 1.3496 0.749 -0.035
4 13.4167 0.1342 1.3498 0.7668 0.018

Table 5.2: Distillate composition of ethanol when feed enters at stage 3 and RR is 8
distillate
samples EtOH mol % Xd refractometer reading (nD) Xud change
1 13.9167 0.1392 1.3504 0.822 -
2 13.8333 0.1383 1.3503 0.8127 -0.009
3 14.3333 0.1433 1.3509 0.8715 0.059
4 14.5833 0.1458 1.3512 0.9023 0.031
5 14.4167 0.1442 1.351 0.8814 -0.021
6 14.6667 0.1467 1.3513 0.913 0.032

Table 5.1: Distillate composition of ethanol when feed at stage 5 and RR is 8

distillate
samples EtOH mol % Xd refractometer reading (nD) Xud change
1 14.5833 0.1458 1.3512 0.9023 -
2 14.4167 0.1442 1.351 0.8814 -0.021
3 14.4167 0.1442 1.351 0.8814 0.000
4 14.7500 0.1475 1.3514 0.9235 0.042
5 14.7500 0.1475 1.3514 0.9235 0.000
Analysis

Design a process to concentrate a mash (8 mole% ethanol in water) to a very strong, but tasty, 80 mole% blend. Need to be able to
produce 100 barrels a day.

Design 1 Design 2 Design 3

Properties Feed Distillate Bottom Feed Distillate Bottom Feed Distillate Bottom
volumetric flow rate (L/day) 1.49E+05 1.19E+04 1.36E+05 1.36E+05 1.19E+04 1.22E+05 1.36E+05 1.19E+04 1.22E+05
mass flow rate (g/day) 1.43E+08 9.75E+06 1.33E+08 1.30E+08 9.75E+06 1.20E+08 1.30E+08 9.75E+06 1.21E+08
ethanol mass flow rate (g
EtOH/day) 2.61E+07 8.88E+06 1.72E+07 2.37E+07 8.88E+06 1.48E+07 2.37E+07 8.88E+06 1.48E+07
water mass flow rate (g
H2O/day) 1.17E+08 8.68E+05 1.16E+08 1.06E+08 8.68E+05 1.06E+08 1.07E+08 8.68E+05 1.06E+08
ethanol mass fraction (g
EtOH/g soln) 0.1820 0.9110 0.1287 0.1820 0.9110 0.1230 0.1820 0.9110 0.1230
water mass fraction (g H2O/g
soln) 0.8180 0.0890 0.8713 0.8180 0.0890 0.8770 0.8180 0.0890 0.8770
ethanol mole fraction (mol
EtOH/mol soln) 0.0800 0.8000 0.0274 0.0800 0.8000 0.0217 0.0800 0.8000 0.0218
water mole fraction (mol
H2O/mol soln) 0.9200 0.2000 0.9726 0.9200 0.2000 0.9783 0.9200 0.2000 0.9782
From Aspen:

Column Performance

Performance Condenser Reboiler

Temperature © 77.874 88.778
Heat Duty (kJ/day) -7.43E+07 8.60E+07
Distillate rate
(kmol/day) 242.56182 -
Reflux rate (kmol/day) 1630.0155 -
Reflux ratio 7.31 -
Bottom rate (kmol/day) - 6455.64967
Boilup rate (kmol/day) - 2071.01713
Boilup ratio - 0.32

Stream Properties

Temperature K 339.650 351.024 361.928

Pressure atm 1.000 0.987 0.987
Vapor Frac 0 0 0
Mole Flow kmol/hr 279.092 10.107 268.985
Mass Flow kg/hr 5654.290 406.304 5247.986
Mass Flow g/day 135702957 9751294 125951663
Volume Flow l/min 103.577 9.022 97.310
Volume Flow l/day 149152 12991 140126
Enthalpy
MMkcal/hr -18.783 -0.659 -18.009
Mole Flow kmol/hr
ETHANOL 22.327 7.993 14.335
WATER 256.765 2.114 254.651
Mole Frac
ETHANOL 0.08 0.791 0.053
WATER 0.92 0.209 0.947

Design specifications

Efficiency 80%
Theoretical number of
stages 6
Actual number of stages 8
Optimal Feed Stage middle
Column Diameter (m) 1.28

6) Calculation for diameter: use scale up value from experimental data

Diameter of column: 10.15 cm
Height of column: 110 cm
Scale up ratio (in volume): 2009.64
Ratio of Height to Diameter of column: 10.84

Use the equation of a cylinder:

V=Πr2h (I)

Where,

V = volume of column
r = radius of column
h = height of column

Volume of column: Π(5.075)2(110) = 8900.5 cm3 = 8.9 L

Volumn of actual reactor column: 8.9(2009.64) = 17886.81 L

From equation of cylinder and diameter to height ratio, equation II was obtained:

D2 (II)
V = π ⋅10 .837 D ⋅
4

4V 4(17886810 )
Therefore the actual diameter is: = 3 = 3 = 128.1 cm = 1.28 m
10 .837 π 10 .837 π
References

1) http://lorien.ncl.ac.uk/ming/distil/distilpri.htm
2) Seader, J.D, 2006, Separation Process Principles, 2nd edition, John Wiley & Sons,
Hoboken, pp 316-318.
3) Koch-Glitsch, 2003, “Intalox Packed Tower Systems, IMTP High Performance
Packing,” Koch-Glitsch, LP, pp.