Coloso, Ma. Jinelle V.

Date Performed: September 5, 2017

5ChE-B Date Submitted: September 26, 2017
Group No. 1

Experiment No. 1
Computing for the Efficiency of the Distillation Column

Introduction

Distillation is one the most common unit operations used in the industries. It is a
process wherein the desired component is separated from the initial mixture by
selective condensation or evaporation. This separation process could be in partial or
complete depending on the type of distillation use [1].

Flash distillation, also known as equilibrium distillation, happens when a definite

fraction of the liquid feed is vaporized and is in equilibrium with the residual liquid. The
process also involves reducing the pressure suddenly to lower the boiling point of the
component (hence, it is called flash distillation). While in batch or differential distillation,
the total vapor formed is not in equilibrium with the residual liquid, therefore removing
the bottoms product [2].

Batch distillation will be the focus of this experiment, wherein vapor from the
reboiler rises up the trays in the column and is finally liquefied in the condenser. This
condensed liquid could be either drawn off or reintroduced, also known as reflux, into
the top of the column. Reflux are mostly done to increase the efficiency of the column
[2].

Efficiencies of the column can be calculated using several approaches namely

graphical methods like Mc-Cabe thiele, shortcut methods like Fenske-Underwood-
Gilligand, and rigorous plate-plate calculations using computer softwares [3].

The most conventional and accurate way to get the theoretical concentration is by
using the Mc-Cabe Thiele method. This method is mostly used in binary distillation with
constant molar overflow, which in this case, an ethanol-water mixture [4].
 For ideal mixtures in thermodynamic vapour-liquid-equilibrium, it follows Equation 1
[5].

1
= Equation 1

Where: = . For real mixtures, = (y= activity coefficient)

For binary mixtures, the most common method to find the concentration of a
certain component is by the Rayleigh Equation [5].

ln ( ) =

Equation 2

Where B = bottoms product

xB = mole fraction of the bottoms product

xD = mole fraction of the distillate product

F = Feed

For this experiment, it will focus on getting the best combination of temperature
and reflux ratio under constant time which will give the highest efficiency of the distillate.
The optimization process will be done once all other groups are finish doing the
experiment. The experiment will also focus on getting the final conversion, the efficiency
of the distillation column and the percentage error by finding the theoretical distillate
concentration at a certain temperature using the McCabe-Thiele method.
Methodology

Figure 1 shows the set-up for the Distillation experiment while in Figure 2, a close-

up of the main controller of the set-up is seen.

*Fig. 1 Distillation Set-up **Fig. 2 Main controller of the Set-up

*See Appendix A for the schematic diagram of the Distillation set-up

** 1: Heater Switch. 2: Temperature Controller. 3: Temperature Indicator per column. 4: Reflux Switch. 5:
Main Switch

A 5L ethanol-water mixture was prepared by mixing 20% ethanol by weight and 80%
water by weight. The specific gravity of the mixture (0.3733) was then computed using a
pycnometer. The ethanol-water mixture was poured into the evaporator. The distillate drain
valve in the reflux divider was made close to avoid spillage. The reflux ratio was then set to 0
and the water inlet was connected to the faucet. Flow rate was then set to 150L/hr. The
students measured the specific gravity of the distillate every 3 minutes at 80oC (See Table 1.1
for the data). After collecting the data, the master switch and water supply was turned off.
Lastly, the system was cooled down before draining the evaporator.
Results and Discussions
After obtaining the data the students record the initial mixture which is seen in
Table 1.1.

Table 1.1 Initial Mixture

*Mass of the feed + *Density of the feed *Specific Gravity of
pycnometer (g) (g/mL) the Distillate
Feed 51.125 0.3722 0.3733
*See Appendix B for the sample calculations.

In finding the composition of the feed (xf), the table provided in the laboratory
manual was used (according to Windisch). By the method of interpolation, at
0.3722g/mL, the percent composition by weight of the feed is 39.607%.

Table 1.2 At T=80oC, Reflux ratio=0

Mass of empty pycnometer: 32.4921g
**%
Volume of the Mass of the *Density of
Time Composition *%
Distillate Distillate + the Distillate
(min) by Mass of Recovery
collected (mL) pycnometer (g) (g/mL)
Distillate (xD)
3 40.38 42.6344 0.2512 26.10% 65.90%
6 44.80 42.5886 0.2257 23.39% 59.06%
9 45.55 42.4654 0.2190 22.70% 57.31%
12 47.32 42.4146 0.2097 21.69% 54.76%
15 51.25 42.6215 0.1976 20.41% 51.53%
18 55.65 42.7543 0.1844 19.01% 48.00%
21 58.35 42.9019 0.1784 18.37% 46.38%
24 58.75 42.8186 0.1758 18.10% 45.70%
27 65.25 43.0841 0.1623 16.66% 42.06%
30 66.80 42.7035 0.1586 16.27% 41.08%
Total 488.55mL 426.986g 0.2089 21.618% 51.18%
*See Appendix B for the sample calculations
**Data was obtained using interpolation using the table in the Laboratory manual.
 In Figure 3, plotting the time vs. xD, the students obtained a graph showing the
distillation time increasing while the composition of the distillate is decreasing. This is
due to the fact that as the distillation time increases, the temperature of the top most
column increases too such that it may reach the boiling point of the second component,
making the desired distillate not pure [6].

Time vs. Xd
0.3

0.25
Composition

0.2
y = -0.0034x + 0.2593
0.15 R = 0.9659
0.1

0.05

0
0 5 10 15 20 25 30 35
Time

Fig. 3 Plot of time vs. xD using a linear trendline

Getting the trendline of the graph from Figure 3, the students could estimate the
composition of the distillate at T=80oC and Rd = 0.

Y = -0.0034x + 0.2593 Equation 3

As seen in Figure 3, a linear trendline generates a 0.9659 R2 making it not

accurate for getting the composition of the distillate.
 Time vs. Xd
0.3

0.25
Composition y = 0.2647e-0.017x
0.2 R = 0.9822
0.15

0.1

0.05

0
0 5 10 15 20 25 30 35
Time

Fig. 4 Plot of time vs. xD using exponential trendline

Hence, using an exponential trendline (Figure 4), the students obtained a 0.9822
R2 making it more accurate than the linear trendline.

y = 0.2647 0.017 Equation 4

The theoretical composition of the distillate can be estimated using the

equilibrium curve (See Appendix C). XD has a value of 75% by volume while the actual
xD is at 26.392% by volume. This concludes that at T=80OC and t=30mins, not all of the
distillate was distilled.

Lastly, using the Mc-Cabe thiele method, it would not be efficient because xf
(39.607%) is greater than xD (26.392%). Some errors that may had contribute to the
error would be the column was not properly set-up and not all the distillate at a certain
time was collected, making the volume and density not accurate.

The Mc-Cabe Thiele method is mostly used for binary mixtures and assumes
constant pressure throughout the system. Also, Mc-Cabe Thiele is only applicable when
both components have equal and constant molar enthalpies and overflow [7].
Answers to Questions

The use of reflux is widely used in industries that uses distillation columns as
their main separation process like in petroleum refineries and natural gas
processing plants. The more reflux is done by the system, the better is the column's
separation (difference in boiling points) [8]. Therefore, reflux is the term used to express
the amount of top product, which is put back into the tower. Having a 100% reflux
means that all distillate will be return to the column and no distillate will be collected. It
will be an endless cycle or loop.

One reason that the students had encountered during the experiment is when the
temperature could not increase even though it was set to 80 oC (highest temperature
was 30oC). This was due to the fact that air bubbles are trapped inside the tubes,
hindering the heat to go up the column. To fix this, the valve connecting to the distillate
tank should be opened minimally to let the pressure inside the tubes be released
therefore removing the air bubbles.

The temperature of the column will vary depending on what will be the desired
distillate. For an ethanol-water mixture, the ideal temperature should be higher than the
boiling point of ethanol which is 78oC but lower than the boiling point of water which is
100oC. If the columns temperature is higher than 100 oC, the distillate will now contain a
small amount of water for it already boiled too. While the higher the reflux ratio, the
more vapor-liquid contact will be. Therefore, a higher reflux ratio means higher purity of
the distillate but also means that the collection rate(volume) for the distillate will be
slower [8]. In the case of this experiment, if the time is limited, a high reflux ratio is not
recommended if a company wants a higher volume and a negligible purity
concentration.

The common difference between batch distillation and continuous or flash

distillation is that in flash distillation the feed is continuously entering the column, while
in batch distillation the feed is charged into the evaporator at the beginning of the
operation. The evaporator in batch distillation gets empty over time, therefore giving the
process an unsteady-state nature [9].
Conclusion and Recommendation

It was seen that having a high reflux ratio, the more the purity of the product will
be although it also means that the collection rate for the distillate will require a more
extended time. It was also concluded the concentration and purity of the distillate will
depend on the temperature of the column. The temperature should not exceed the
boiling point of the second component for it will also be distilled and will be mixed with
the first component.

The students obtained a value of 26.392% (xD). This tells that the not all of the
ethanol was distilled at 30 minutes making it not effective for a successful separation of
the components. Lastly, the column was also not efficient for xf is greater than xD.
Some factors that may had affect the distillate concentration is that while getting
the distillate every 3-minute intervals, the students did not cool down the mixture to the
indicated temperature written in the table in the laboratory manual. With this, the weight
of the distillate was not constant throughout the process. Also, it should be noted that if
distillate production is too slow to generate, it is because of the air pressure inside.
Make sure to open the pressure valve that will release the trapped air and that will
release the distillate.

References

[1] Distillation. (2017, September 19). Retrieved September 22, 2017, from
https://en.wikipedia.org/wiki/Distillation

[2] Jaffar, N. (1970, January 01). Chemical Engineering Knowledge. Retrieved

September 22, 2017, from http://chemknowhow.blogspot.com/2014/10/differential-
distillation-flash.html

[3] Sapp, K., Lawson, J. (2007). Batch Distillation Theory. USA. University of Florida.
Retrieved September 22, 2017, from
http://www.che.ufl.edu/ren/course/4404L/BD/BD%20Theory%20Handout.pdf

[4] McCabeThiele method. (2017, September 03). Retrieved September 22, 2017,
from https://en.wikipedia.org/wiki/McCabe%E2%80%93Thiele_method

[5] Kim, K., Diwekar, U. (2005, April 27). Chapter 5: Batch Distillation. USA. p.112-114.

[6] Wired Chemist. (n.d.). Retrieved September 25, 2017, from

http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/distillation
[7] Vogelpohl, A. (1974). The Fundamental Equation of Distillation. Germany. Technical
University of Clausthal.

[8] What is the Difference Between Reflux & Distillation? (n.d.). Retrieved September
25, 2017, from http://sciencing.com/difference-between-reflux-distillation-5953384.html

[9] Albarede, F., Hofmann, A. W., & Condomines, M. (n.d.). The Rayleigh distillation
equation.Geochemistry,220-221. doi:10.1017/cbo9781139165006.017
APPENDIX A

Schematic Diagram

I Packed Column V Top Product Tank

II Evaporator IX Cooling Water Flow Meter

III Top Product Condenser

IV Phase Separation Tank

T1 Evaporator Temperature

T2-T9 Column Temperature

T10 Top Product Temperature

T11 Cooling Water Inlet Temperature

T12 Cooling Water Outlet Temperature

T13 Column Top Temperature

LSL Level Switch Evaporator

P1 Column Pressure Loss

P2 System Pressure, Relative

APPENDIX B

Density of the Distillate/Feed:

weight of pycnometer and distillate weight of pycnometer
distillate/feed =
volume
42.6344g 32.4921g
distillate/feed =
50.068mL
g
distillate/feed = 0.2026
mL

Specific Gravity of the Feed:

density of distillate
s. g.distillate =
density of water @ 25C
g
0.2026 mL
s. g.distillate = g
0.997 mL

s. g.distillate = 0.2032

Percent Recovery:

%conversion = x100

26.10
%conversion = x100
39.607
%conversion = 65.90%
APPENDIX C

Fig. 5 Equilibrium Curve for Ethanol

It can be seen that at T=80oC, the distillate would have a value of 75% by volume
(Theoretical). Plotting the theoretical xD