Fresnoza, Anthea Bettina A.

Date Performed: September 26, 2017

5ChE-B Date Submitted: October 18, 2017
Group No. 5

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

I. Introduction

Distillation is a process in which a liquid or vapor mixture of two or more substances is

separated into its component fractions of desired purity, by the application and removal of heat
[1]. It can be performed by either two methods: flash and differential distillation.

Flash distillation as shown in figure 1 is done by partially vaporizing a multicomponent liquid

feed such that the vapour is in equilibrium with the residual liquid. The vapour and liquid mixture
is separated through a vapour separator tank at a specified pressure and temperature [2]. It is
based on the production of a vapour without allowing any liquid to return to the still [2]. It is
mostly used for components with extremely different boiling temperatures.

Figure 1. Plant for flash distillation

On the other hand, differential distillation also known as rectification or fractional distillation is
carried out using distillating column, condenser, reboiler and a reflux drum as shown in figure 2.
The feed enters the column at the feed plate. The feed plate divides the distillating column into
two sections. The upper part of the feed plate is called the rectifying section while the bottom
part is the striping section. The feed flows down the reboiler where heat is supplied to generate
vapor. The liquid removed from the reboiler is called the bottoms. The vapour generated from
the reboiler moves up the column, liquefied in the condenser and enters a reflux drum. The
condensed liquid can either be collected as distillate or some can be recycled back to the top of
the column known as reflux [1].

Figure 2. Basic components of distillation

Either of these methods may be conducted as batch or continuous process. In a batch process,
the feed is introduced to the column then the distillation process is conducted. When the desired
separation is achieved, a next batch of feed is introduced. While continuous process operates
by continuous input of feed. In this experiment, it focuses on batch differential distillation.

In determining the efficiency of the column, the McCabeThiele method is considered to be the
simplest method for the analysis of binary distillation [8].It was a graphical solution method
based on Lewis method and the observation that the operating equations plot as straight lines
on equilibrium curve diagram [10] to determine the number of theoretical stages required for a
certain degree of separation [7].
For an ideal system, the equilibrium components can be obtain using Raoults and Daltons
Law.

yi=Kixi Equation 1
where Ki is the vaporization equilibrium equal to . For more than two components, Ki is in

terms of fugacity, and activity coefficients, shown in equation 2.

Ki = Equation 2

For batch distillation of binary mixture shown in figure 3, the overall differential mass balance is

Equation 3

While the differential mass balance of the volatile component is

Equation 4

Integrating equation ___, Rayleighs Equation was obtained [3].

( ) Equation 5

where B = bottoms product

F = Feed

xB = mole fraction of the bottoms product

xD = mole fraction of the distillate product

 Figure 3. Schematic diagram of distillation column operating in batch process

II. Scenario
Industries such as beverages production, petrochemical and natural gases industry uses
distillation as their process in obtaining their desired products . In this experiment, an alcohol
industry wants to produce the strongest alcohol to beat the existing strongest alcohol in the
world. To reach their goal, the company owner asked his engineers to distill a raw material
composed of 20 % ethanol by weight. The company owner also wants to attain the best
combination so he challenged his peers to find the best combination of temperature and reflux
that will produce the highest concentration in 30 mins.

III. Objectives
Main:
To find the best combination of temperature and reflux ratio under constant time
which will give the highest efficiency of the distillate.

Specific:

To validate the relationship between reflux vs. temperature, concentration vs.

temperature and concentration vs. reflux.
 To get the efficiency of the column by using the Mc-Cabe thiele method in
obtaining the theoretical value.

IV. Procedure

Figure 1 shows the set-up for the Distillation experiment (See Appendix A for the schematic
diagram of the Distillation set-up).

Figure 4. Distillation Set-up

A 5L ethanol-water mixture was prepared by mixing 20% ethanol by weight and 80% water by
weight. The specific gravity of the mixture was then computed using a pycnometer. Afterwards,
the ethanol-water mixture was poured into the evaporator. All valves was opened to ensure that
all vapour was eliminated prior to the experimentation. The distillate drain valve was closed to
avoid spillage then the reflux ratio was set to 0. The water inlet was connected to the faucet and
maintained a flow rate of 150L/hr. The assigned temperature was maintained for 10 minutes
and reflux ratio was adjusted based on the assigned data of 75%. The distillate was collected
every 5 minutes and the density of every distillate was measured at 15 to obtain the specific
gravity using figure 9 (See Appendix C). The process was repeated for 50% reflux ratio. After
collecting all the necessary data, the master switch and water supply was turned off. Lastly, the
system was cooled down before draining the evaporator.

V. Data and Discussions

Table 1.1 Initial Mixture

Mass of empty pycnometer: 43.9430 g

Mass of the feed + Density of the feed Specific Gravity of the

pycnometer (g) (g/mL) Distillate

Feed 92.4258 0.9683 0.9712528173

The data obtained for the feed was shown in Table 1.1. The composition of the feed (xF) was
obtained from the table according to Windisch using the density. By interpolation, the weight
percent composition of the feed is 22.6018% while the volume percent composition is
27.5464%.

Table 1.2 Percent Composition and Percent Recovery for 75% and 50% Reflux Ratios

Reflux Ratio 75 % 50 %

%
% Composition
Composition
Time (min) *% Recovery by Mass of *% Recovery
by Mass of
Distillate (xD)
Distillate (xD)

5 85.9823 28.81757 79.16153047 6.768616

10 88.642306 1.205299 79.1330818 6.459157

15 97.6119849 2.002024 83.3389948 2.495668

20 86.211608 8.530937 81.51773906 0.410056

25 54.93630291 0.750227 70.84640251 0.275393

Total 82.4068 40.98948 75.98628 16.02681

Table 1.2 summarizes the composition of distillate and percent recovery for reflux ratio of 75%
and 50% at distilling temperature of 80 The composition by mass of distillate was obtained
from the table according to Windisch, given in the laboratory. Theoretically, the recovery of most
volatile component decreases over time. However, the data for 75% reflux ratio is inaccurate.
The highest percentage recovery was obtained from 75% reflux ratio at the time of 5 minutes for
the reason that the distillate started to build up in the phase separation tank as the temperature
reached 79 . Initially, the assigned distilling temperature was 85 , however, the temperature
became constant at 80 and at this temperature, the distillate started to overflow which made
the students decide to conduct the experimentation at 80 . The distillate in the phase
separation tank was brought back to the reboiler and waited for the temperature to reach 80

Using the equilibrium curve for ethanol (See Appendix E), the theoretical composition of
distillate at 80 was 75% by volume. Through experimentation, the acquired composition of the
distillate was 87.41144% and 82.1115% by volume for reflux ratio of 75% and 50%. It signifies
that all the ethanol was distilled.

xD vs Time
1.2
y = -0.0129x + 1.0203
Composition of distillate

1 R = 0.3959

0.8
75%
0.6 y = -0.0028x + 0.8307
R = 0.2218 50%
0.4
Linear (75%)
0.2 Linear (50%)
0
0 5 10 15 20 25 30
Time, min

Figure 5. Distillate composition vs time with linear trend line

 xD vs Time
1.2
y = -0.0025x2 + 0.0627x + 0.5791
Composition of distillate
1 R = 0.9248

0.8
75%
0.6 y = -0.0008x2 + 0.0206x + 0.6942
50%
R = 0.8042
0.4
Poly. (75%)
0.2 Poly. (50%)
0
0 5 10 15 20 25 30
Time, min

Figure 6. Distillate composition vs time with polynomial trend line

As seen in figure 5 and 6, it depicts the graph for the composition of distillate vs time with linear
and polynomial trendline respectively. Theoretically, the composition of distillate decreases
over time. As distillation continues, there is a rise in temperature that results in increase in other
component, water, in vapour [5]. However, the data acquired has different trend. It increases in
the beginning however, it started to decrease at 15 minutes mainly because of the difficulties
encountered.

A linear trend line shown in figure 5 presented a linearity of 0.3959 and 0.2218 for reflux ratio of
75% and 50% respectively thus making it inaccurate to use. On the other hand, figure 6
presented an R2 of 0.9248 and 0.8042 for reflux ratio of 75% and 50% using polynomial trend
line making it more accurate. Equation 6 and 7 represents the equation to obtain the component
of the distillate at any time for reflux ratio of 75% and 50% respectively.

y = -0.0025x2 + 0.0627x + 0.5791 Equation 6

y = -0.0008x2 + 0.0206x + 0.6942 Equation 7

 Rd vs xD
80
70
Reflux ratio, Rd 60
50
40
75%
30
50%
20
10
0
0 0.2 0.4 0.6 0.8 1 1.2
Composition, xD

Figure 7. Reflux ratio vs distillate composition

Figure 7 shows the graph for reflux ratio vs the composition of ethanol in the distillate. It is
observed that increasing the reflux ratio of the column increases the degree of separation
between the feed composition and the distillate composition thus obtaining a distillate of higher
purity. According to McCabe-Thiele method, increasing the reflux ratio will result to lesser
number of theoretical plates needed thus results to higher distillate composition [6]. Higher
reflux ratio signifies further vapour and liquid contact can occur in in the distillation column [9].

The ethanol concentration of the feed and distillate is not efficient for McCabe-Thiel method
(See Appendix F). The rectifying line does not meet the feed line resulting to unachievable
calculation for the efficiency of the column.

VI. Conclusion and Recommendation

After performing the experiment, it was seen that in order to achieve higher purity of the
distillate and degree of separation between the feed and distillate composition, it would
mean higher reflux ratio needed for the system. The temperature of the column also
affects the purity of the distillate.

The experimentation shows that the composition of the distillate decreases over time
and the relationship to compute for the concentration as a function of time for different
reflux ratios was successfully obtained as shown in equation 6 and 7. The degree of
separation between the feed and distillate composition was successfully achieve since
the distillate composition acquired through experimentation, 87.41144% and 82.1115%
by volume for reflux ratio of 75% and 50% respectively, was evidently higher than the
theoretical value of 75% at 80

However, the experimentation failed to calculate for the efficiency of the column using
McCabe-Thiele method to obtain the theoretical number of plates of the column. Some
factors that may have affected the distillate concentration were that the students did not
wait for the temperature to stabilize for 10 minutes before performing the experiment
due to time constraint. Also, the distillates build up in the phase separation tank before
the desired temperature was reached. Make sure to turn on the reflux switch. Lastly, the
volume of the distillate in the pycnometer decreased as the temperature reached 15
which had affect the density and distillate composition acquired.

VII. References

[1] Basic Distillation Theory. Retrieved October 15, 2017 from https://chemeng-
processing.blogspot.com/2009/02/basic-theory-distillation.html
[2] McCabe,W.L.,Smith,J.C.,& Harriot,P. (1993). Unit Operations of Chemical Engineering 5th
Ed. pp.521-550.
[3] Distillation. Retrieved October 15, 2017 from http://www.che.ufl.edu/unit-ops-
lab/experiments/Distillation/Distillation-theory.pdf
[4] Distillation Theory. (2010, March 11). Retrieved October 15, 2017 from
http://stupidityshouldhurt.com/reference/org/theory.htm
[5] Distillation. (2014,October). Retrieved October 15, 2017 from
https://en.wikipedia.org/wiki/Distillation
[6] Reflux Ratio. Retrieved October 15, 2017 from
http://www.separationprocesses.com/Distillation/DT_Chp04n.htm
[7] The McCabe-Thiele Method. Retrieved October 15, 2017 from
http://www.separationprocesses.com/Distillation/DT_Chp04f.htm
[8] McCabe-Thiel Method. Retrieved October 15, 2017 from
https://en.wikipedia.org/wiki/McCabeThiele_method
[9] Reflux Ratio. Retrieved October 15, 2017 from http://www.solvent--
recycling.com/reflux%20ratio.html.
[10] Wankat, P.C. (2011). Separation Process Engineering : includes mass transfer analysis 3rd
Ed. United States: Pearson Education
[11] Couper, J.R., Penney, W.R., Fair, J.R., & Stanley, M.W. (2012). Chemical Process
Equipment: Selection and Design. p.400.

VIII. APPENDICES

Appendix A: Schematic Diagram

Figure 8. Schematic Diagram

I Packed Column V Top Product Tank

II Evaporator IX Cooling Water Flow Meter

III Top Product Condenser LSL Level Switch Evaporator

IV Phase Separation Tank P1 Column Pressure Loss

T1 Evaporator Temperature P2 System Pressure, Relative

 T2-T9 Column Temperature

T10 Top Product Temperature

T13 Column Top Temperature

T11 Cooling Water Inlet Temperature

Appendix B: Raw Data

Table 1.3 At T=80oC, Reflux ratio=75%

Volume of the
Time Mass of the Distillate Volume of Distillate Density of the
Distillate collected
(min) + pycnometer (g) in pycnometer (mL) Distillate (g/mL)
(mL)

5 440 85.2025 49.5 0.833525

10 18 58.4088 17.5 0.826617

20 28 65.1841 26.5 0.8015509

25 130 85.5897 50 0.832934

30 30 58.3885 29 0.498121

Total 646 85.6496 49.5 0.842558

Table 1.4 At T=80oC, Reflux ratio=50%

Volume of the
Time Mass of the Distillate Volume of Distillate *Density of the
Distillate collected
(min) + pycnometer (g) in pycnometer (mL) Distillate (g/mL)
(mL)

5 110 85.6215 49 0.850581633

10 105 85.6249 49 0.85065102

15 39 75.7036 37.8 0.840227513

20 8 48.7594 7 0.688057143

25 6.9 47.6418 6 0.6164666667

Total 268.9 86.8585 50 0.85831

Appendix C: Table for density and content of aqueous ethanol solutions relative to water
15 degrees = 1.00 (according to Windsch)

Figure 9. Table for density and content of aqueous ethanol

Appendix D: Sample Calculation

Density of the Distillate/Feed:

weight of pyc ometer a d disti ate weight of pyc ometer
distillate/feed
vo ume

92 4258g 43 9430g
distillate/feed
50 068mL

Specific Gravity of the Feed:

g
distillate/feed 0 96833
mL
de sity of disti ate
s g distillate
de sity of water @ 25C

g
0 96833 mL
s g distillate g
0 997 mL

s g distillate 0 9712528173

Percent Recovery:

% recovery x100

% recovery x100

440 0 8335 0 85982

%recovery x100
5000 0 9683 0 22602

% recovery 28 82%
Appendix E: Equilibrium curve for Ethanol

Figure 10. Equilibrium Curve for Ethanol

Appendix F: McCabe-Thiele Graphical Method for Different Reflux ratio

Figure 11. McCabe-Thiel graph for 75% refflux ratio

Figure 12. McCabe-Thiel graph for 50% refflux ratio