American University of Beirut

Department of Chemical and Petroleum Engineering

CHEN 410 Unit Operations Lab

Experiment:
Distillation

S2G4
Section 2
Group 4

Moustafa Houmani Mmh112@mail.aub.edu

Shant Mher Deyirmenjian Sgd08@mail.aub.edu
Valarie Aoun Vra00@mail.aub.edu
Malik Aboul Naja Msa102@mail.aub.edu

March 8, 2017
CHEN 410: Unit Operations Lab Experiment: Distillation

Abstract

The objective of this experiment is to study the variation of the pressure drop in a distillation
column when the boil-up rate is increased. The reboiler produces necessary vapor to fulfill the
separation process so it is important to pick the adequate boil-up rate to maximize the efficiency
of the column.

A liquid mixture is fed to an 8-trays distillation column with total reboiler. The boil-up rate is
directly correlated to the velocity of the vapor in the column which in turn dictates the degree of
foaming on the trays. Increasing the heat duty of the reboiler, will cause an increase in the vapor
flow rate which could eventually lead to flooding. While decreasing the reboiler heat duty, will
decrease the vapor flow and could cause weeping.

The power to the reboiler was varied from 0.4 kW to 1.15 kW with 0.15 kW increments and for
every reading, the boil-up rate was measured, the pressure drop between the top and the bottom
of the column was calculated, the temperature at each tray was recorded and the degree of
foaming was observed.

The results of this experiment show that the pressure drop increases with increasing boil-up rates
and a spike was noted in pressure drop when the power was increased from 0.85 kW to 1.00 kW
where as the foaming changed from violent localized to flooding. This indicated that the optimal
operation condition of the column occurs when the power input to the reboiler is 0.85kW.

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CHEN 410: Unit Operations Lab Experiment: Distillation

Table of Contents
1. Introduction............................................................................................................................3
A. Objectives and deliverables..........................................................................................................4
2. Theoretical Background........................................................................................................4
3. Experimental Methods..........................................................................................................6
A. Setup..............................................................................................................................................6
B. Procedure......................................................................................................................................6
4. Results and Discussion..........................................................................................................8
A. Degree of Foaming and Boil-up Rate..........................................................................................8
B. Pressure Drop Across Column.....................................................................................................9
C. Temperature Profile Across Trays.............................................................................................11
D. Error Analysis.............................................................................................................................14
5. Conclusion............................................................................................................................15
References.....................................................................................................................................16
Appendix.......................................................................................................................................17

Table of Figures and Table

Figure 1: Experimental Setup.......................................................................................................6
Figure 2: Column pressure drop vs. boil-up rate........................................................................9
Figure 3: Log of pressure drop vs. log of boil-up ratio.............................................................10
Figure 3:The temperatures (C) at different trays for different boil-up rates (L/hr)............11
Figure 5:: Reboiler temperature at different power inputs to the reboiler (kW)..................13

Y
Table 1:Collected experimental data at each reboiler power input..........................................8
Table 2: Qualitative degree of foaming on trays at Index..........................................................8
Table 3:Measurements and statistics for error analysis...........................................................14
Table 4: Temperatures of the eight trays and the reboiler (T9) at..........................................17

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CHEN 410: Unit Operations Lab Experiment: Distillation

1. Introduction

Distillation is the most widely used method of separating fluid mixtures on a commercial scale, it
is an important part of many processes in the oil and chemical industries1. It is used to separate
different components based on their different volatilities and boiling points, into an overhead and
bottom products2.

Industrial application of distillation columns include production of many chemical products such
as naptha, phenols, toluene and phytosterols, etc. In the oil industry, it is used to separate
hydrocarbons. Liquor, beer and wine are produced after undergoing several stages of distillation
which eliminates the additive and produce a final distilled form of the spirits. Distillation plants
can also convert ocean water into drinking water and supply it to areas having scarcity of water3.

On entering the column, because of the effect of temperature, the feed separates into a liquid
phase and a vapor phase. As the latter rises, it cools and while part of it continues up as vapor,
some of it (enriched in the less volatile components) falls back downward by gravity. A reboiler
at the bottom of the column heats the liquid and vaporizes it. The higher the boil-up rate, the
more vapor/liquid contact can occur in the distillation column. So higher boil-up rate usually
means higher purity of the distillate4.

However, distillation is one of the most energy intensive operations. It is easily the largest
consumer of energy in petroleum and petrochemical processing2. Higher boil-up rate also means
higher energy requirement. A study must be conducted to determine the optimum boil-up rate
that would achieve a high purity separation for which the total cost will be the least. The more
energy supplied to the reboiler, the higher the velocity of the vapor entering the column. This
consequently affects the pressure drop inside the column which determines the temperature level
of the column.

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CHEN 410: Unit Operations Lab Experiment: Distillation

A. Objectives and deliverables

In this experiment, we shall determine the variation of the pressure drop in the distillation
column when the boil-up rate is increased. To do so, the power delivered to the reboiler is
increased in increments of 0.15 kW and the pressure drop between the top and the bottom of the
column is measured. The temperature at each tray is recorded and the degree of foaming is
identified to further describe the effect of increasing pressure drop and boil-up rate. Several
readings at a constant power of 0.85 kW are taken for error analysis purposes.

2. Theoretical Background
The distillation column is filled with liquid condensing from the top of the tower and vapor
rising from the reboiler. Consequently, every sieve tray has vapor emerging from the holes as
well as liquid passing on the surface of the tray. The holes restrict the flow of the emerging vapor
causes a pressure drop across every sieve tray and the pressure drop is augmented if foaming is
present. The equation below sums up the two pressure drops in terms of head loss in meters:
htray =hd +hliq
The dry head loss, or hd , can be calculated using the equation below:
v
hd =
( 0.186
Co 2

)( )
l
v hole
2

Where,
C o is orifice size coefficient, m/s2
v is the density of the vapor, kg/m3
l is the density of the liquid, kg/m3
v hole is the velocity of the emerging vapor, m/s

In turn, the velocity of the vapor can be calculated using the area of the hole and the boil-up
ratio:
Q vap
v hole =
Ahole
Where,
Qvap is the boil-up ratio of the vapor, m3/s

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CHEN 410: Unit Operations Lab Experiment: Distillation

d hole2
A hole is the area of the hole, m2, and can be found by A hole=
4

As seen by the equations above, the pressure drop will be equal to the dry head loss in the
absence of liquid and therefore will be proportional to the square of the vapor velocity. This is
when the sieve trays behave like an orifice. However, sieve trays in distillation columns contain
both vapor and liquid for the most part and therefore the pressure drop is a result of both.
Foaming is the phenomenon where liquid is expanded as a result of the passing vapor. In most
cases, a great increase in the pressure drop as a result of a small change in the boil-up ratio is
achieved when the liquid head is overcome by the high vapor flow rate. The relationship between
pressure drop and velocity in the absence of foaming is further justified by Bernoullis equation:
P 1 v 12 P v2
+ + g z 1= 2 + 2 + g z 2
2 2
This equation, however, assumes an incompressible, one-directional flow with negligible friction
in steady state. The equation can be further simplified by neglecting the potential energy
difference between adjacent trays. The equation is reduced to:
2
P= (v v 12 )
2 2
The velocities, v 1 and v 2 , can be found using the boil-up ratio and the cross sectional area

Q
of the column ( v = .
Ac
In this experiment, the boil-up ratio was found by collecting the condensed vapor at the top of
the tower and measuring the volume that is being condensed in one minute according to the
following equation.
V
Q=
t
With V being the volume collected and t being the sample time which will be taken as 1
minute in this experiment.
Finding the relationship between boil-up ratio and pressure drop is of high importance in
distillation columns. At very high boil-up ratios, the column operates at a pressure that is too
high for separation since the liquid will move up the column with the vapor formed and flooding
will occur. On the other hand, at very low boil-up ratios, the pressure throughout the column is

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CHEN 410: Unit Operations Lab Experiment: Distillation

too low to allow efficient separation. This is why an optimum boil-up ratio needs to be found in
order to operate the distillation column at a pressure that will allows maximum separation.

3. Experimental Methods
A. Setup
The experimental setup can be seen in the figure below which includes all the equipment
involved in the distillation column, condenser and reboiler. In addition, the valves can be
observed as well as all the temperature and pressure sensors that will be used to record the data.

Figure 1: Experimental Setup

Before starting the experiment, the reflux ratio timer on the console should be turned off to
ensure that the reflux ratio is one. Close all the valves except valve V10 on the reflux pipe and
load 10 liters of the liquid feed mixture that will be distilled into the reboiler through the filler
cap.
B. Procedure
The following steps are needed in order to heat the liquid in the reboiler to increase the
temperature of the feed to proceed with the experiment. In the meantime, take the following
steps to make sure the system is running properly:

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CHEN 410: Unit Operations Lab Experiment: Distillation

Open the valve V5 to make the flow rate to the condenser approximately 3 liters/min.
Throughout the experiment, this value will fluctuate, but make sure that the value stays
within 2.5 and 3.5 liters/min.
Set the temperature selector to T9 to observe the temperature of the feed in the reboiler.
Set the reboiler power to 1.75 kW by turning the power controller clockwise.
To make the pressure drop across the column is zero, open valves V6 and V7 and make
sure the manometer reads a pressure difference of zero. Close the valves after reading the
manometer.
Open valve V10 to make sure the condensate flows back and the decanter doesnt get
full.

Measurements should not be taken until the temperatures across sensors T1-T8 become constant.
After steady-state is reached, set the reboiler power to 0.4 kW and proceed with the following
steps:
1. Record temperatures T1-T9 from the control panel.
2. Record the pressure drop across the column from the manometer by opening valves V6
then V7 and quickly close both valves in the same order that they were opened.
3. Drain the condensate from the reflux system by opening V3 until the tube is empty and
then close the valve.
4. Use a stopwatch set for 1 minute and collect a sample to measure the boil-up ratio by
opening V3. Once the one minute is over, close the valve.
5. Change the reboiler power by increments of 0.15 kW and repeat steps 1-4. Wait 10
minutes for the system to reach steady state.
6. For a specific reboiler power, measure the temperature T1-T9, the pressure drop and boil-
up ratio three times to later perform an error analysis.

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CHEN 410: Unit Operations Lab Experiment: Distillation

4. Results and Discussion

A. Degree of Foaming and Boil-up Rate

Foaming is observed in distillation and absorption towers in industry. It can cause severe
operations problems, as well as reduced tower capacity & separation efficiency. Therefore, it is
necessary to examine the onset and degree of foaming experienced at different tower
configurations in order to avoid the onset of foaming. Table 1 below contains qualitative and
quantitative data collected for this experiment. It displays the set reboiler power input and
measurements of the resulting liquid boil-up rate & column pressure drop, along with the degree
of foaming experienced along the column trays.

Table 1:Collected experimental data at each reboiler power input.

Power Boil-up Rate Boil-up Pressure Degree of Foaming Degree of

(kW) (ml/min) Rate (L/hr) Drop Upper Half Foaming Lower
mmH2O Half
0.4 3.8 0.228 49 1 2
0.55 18.5 1.11 54 2 3
0.7 30 1.8 56 3 3
0.85 46.1 2.766 58 3 4
1 56 3.36 67 4 5
1.15 66 3.96 82 5 5

Table 2: Qualitative degree of foaming on trays at Index.

Index Qualitative Degree of Foaming on Trays

1 None
2 Gentle localized
3 Foaming gently over whole tray
4 Violent localized
5 Flooding

As evident from literature, increasing the power input to the reboiler will increase the liquid
vaporization from the reboiler. This increased boil-up rate would in turn control the degree of
foaming on the column trays, as apparent from our experimental data. Therefore, from the
available data, it can be deduced that the optimum reboiler power input to prevent foaming
(neglecting other factors like temperature), while maintaining a reasonably high boil-up rate lies

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CHEN 410: Unit Operations Lab Experiment: Distillation

in the region below 850W before foaming is observed.

B. Pressure Drop Across Column

Pressure drop information is important for several reasons, some of which includes column
design as well as vapor-liquid equilibrium. Most importantly, distillation columns used in
industry are made up of non-transparent material, unlike the column in the lab, so operators are
unable to visually monitor the degree of foaming inside the column. Therefore, Pressure drop
measurements across various column sections are the primary tool for flood point determination.
Figure 1 below displays the pressure drop as a function of the boil-up rate.

85
80
75
70
65
Pressure Drop P (mmH2O) 60
55
50
45
40
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5

Boil-up Rate (L/hr)

Figure 2: Column pressure drop vs. boil-up rate.

The pressure drop is affected by the boil up rate, the orifice size of the trays and the degree of
foaming. Theoretically, the pressure drop is expected to remain somewhat constant until the
liquid head on the top portion of the tray is overcome (onset of foaming). In figure 1, the
pressure drop observed remains somewhat constant until a boil-up rate of 2.8 L/hr is reached,
where a sudden spike is noticed. It is important to note that it is at this point that the onset of
foaming in the trays is observed by the naked eye. Therefore, the spike in pressure drop is
directly caused by the onset of foaming. Moreover, in the somewhat constant pressure drop

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CHEN 410: Unit Operations Lab Experiment: Distillation

region happening between power inputs of 0.4 kW and 0.85 kW, the pressure drop increases
from 49 mmH2O to 58 mmH2O, possibly because the system had not stabilized yet.

The optimum region of operation is better determined by observing a log-log plot of the pressure
drop versus the boil-up rate as shown below in figure 2

1.95
1.9
1.85
1.8
1.75
log of Pressure Drop
1.7
1.65
1.6
1.55
-0.8 -0.6 -0.4 -0.2 0 0.2 0.4 0.6 0.8

log of (Boil-up Ratio)

Figure 3: Log of pressure drop vs. log of boil-up ratio.

At a log (boil-up rate) value of 0.44, a sharp increase in the pressure drop is observed. It
indicates the onset of foaming. Foaming refers to the expansion of liquid due to a higher passage
of vapor or gas, caused by a higher boil-up rate. Although it provides high interfacial liquid-
vapor contact, excessive foaming often leads to liquid buildup on trays. In some cases, foaming
may be so extreme that the foam mixes with liquid on the tray above. Foaming thus leads to
lower separation efficiencies.
An extreme level of vapor boil-up would eventually lead to flooding, causing liquid to be
entrained in the vapor up the column. The increased pressure from excessive vapor also backs up
the liquid in the down comer, causing an increase in liquid holdup on the plate above. Flooding
is detected by a sharp increase in the column pressure drop and a significant decrease in
separation efficiency. This is because any distillation column has a fixed diameter, and thus, a
maximum L/V volume that it can tolerate before excessive vapor resistances are generated and

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CHEN 410: Unit Operations Lab Experiment: Distillation

cause a heightened pressure drop. This pressure drop can be very dangerous during a distillation
column operation. Thus, ultimately, the liquids and vapors should be able to distribute
themselves up and down the column with relative ease to avoid such large pressure drops, and
this ease is challenged at higher boil-up rates caused by undue power inputs into the reboiler.
Thus, the reboiler should be operated at boil-up rates less than 3L/hr, which corresponds to a
reboiler power input less than 850 Watts.

C. Temperature Profile Across Trays

The input power to the reboiler was varied six times throughout the experiment; upon each
change, the system was allowed about five minutes to stabilize. After stabilizing, temperature
readings were recorded for each of the eight trays plus the reboiler. The temperature profile of
the trays as a function of boil-up rate is plotted in Figure 3 below, tray 1 being the uppermost
one, and tray 8 being the one nearest to the reboiler.

80

79.5

79

78.5 0.228 L/hr

1.11 L/hr
Temerature C
78 1.8 L/hr
2.766 L/hr
77.5 3.36 L/hr
3.96 L/hr
77

76.5
0 1 2 3 4 5 6 7 8 9

Tray Number

Figure 4:The temperatures (C) at different trays for different boil-up rates (L/hr).

As expected, a similar trend in temperature distribution along the trays exists for the different
boil up rates. Progressing upwards in the tower, the temperature decreases for each succeeding

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CHEN 410: Unit Operations Lab Experiment: Distillation

stage, except for stage 7, which is at a lower temperature than stage 6 for all the readings. This,
being thermodynamically illogical, is most probably due to a malfunction in the temperature
sensor of tray 7 giving a biased error. Still, the general trend matches the temperature, since as
the hot vapor rises from the reboiler, it exchanges heat with the liquid, partially condensing, and
leading to a lower temperature at higher trays.
Moreover, as the power input to the reboiler is increased, the temperature along the whole
column increases due to a higher boil-up rate of hot vapor that is to exchange heat with the
liquid. However, this increase in temperature is small (less than 1 C for any individual tray
across the whole range of power inputs). This is also expected, since the temperature of the vapor
rising from the vapor is that of saturation temperature at the given reboiler pressure. Now given
that the pressure drop across the distillation column increased from 49 mmH2O to 82 mmH2O
over the range of power inputs, and given that the pressure at the top of the column is
atmospheric pressure (constant), it can be fairly deduced that the pressure of the reboiler
increased by (82 mmH2O - 49 mmH2O = 33 mmH2O = 0.32 kPa) over the whole range of
power inputs. Thus, this increase in pressure is not significant enough to cause a large change in
the saturation temperature of the rising vapor, leading to similar temperature profiles at different
power inputs.
This argument can be further validated by examining the temperature profile of the reboiler at
different power inputs. Figure 4 below depicts the reboiler temperature at different power inputs
(kW) to the reboiler.
81.6
81.5
81.4
81.3
81.2
Reboiler Temperature C 81.1
81
80.9
80.8
80.7
0 0.2 0.4 0.6 0.8 1 1.2 1.4

Power Input kW

Figure 5:: Reboiler temperature at different power inputs to the reboiler (kW).

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CHEN 410: Unit Operations Lab Experiment: Distillation

As expected, the temperature of the reboiler did not rise significantly with the increase in the
power input into the reboiler, as most of the energy input was invested in increasing boil-up ratio
and manifesting as a bigger pressure drop across the distillation column. This outcome further
proves that foaming and flooding reduce the distillation columns efficiency as the energy
invested is not spent as thermal energy that can enhance separation.

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CHEN 410: Unit Operations Lab Experiment: Distillation

D. Error Analysis

Measurements at the power input of 0.85 kW were taken at three distinct times to perform an
error analysis. The results are shown in table 3 below

Table 3:Measurements and statistics for error analysis.

Temperature (C)
Boil-up Pressure T1 T2 T3 T4 T5 T6 T7 T8 T9
Rate Drop
(ml/min) mmH2
O
Replicate 1 46.1 58.0 78.2 78.2 78.5 78.5 78.7 79.0 78.9 78.9 81.3
Replicate 2 40.0 58.0 78.4 78.4 78.8 78.9 79.3 79.7 79.5 79.8 81.3
Replicate 3 43.0 55.0 79.2 79.3 79.6 79.7 80.2 80.7 80.7 81.0 81.3

Average temp 43.0 57.0 78.6 78.6 79.0 79.0 79.4 79.8 79.7 79.9 81.3
C
S.D. 3.1 1.7 0.5 0.6 0.6 0.6 0.8 0.9 0.9 1.1 0.0
Error/Average 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
Error/Average 7.1 3.0 0.7 0.7 0.7 0.8 1.0 1.1 1.1 1.3 0.0
%

As seen in the table above, errors in temperature readings are minimal, as they do not exceed
1.5% of average measurements. These errors are mostly random errors that are inherent to any
sensor. For the pressure drop measurements, the error was 3% of average read pressure drop
measured, which is minimal considering the human intervention required for this measurement
(Opening the valves in a timely fashion for enough amount of time, then proceeding to collecting
the pressure values by sight).
Moreover, and as expected, the biggest error was in the measurement of the boil-up rate (7% of
average value), since the procedure followed is very prone to error (error in cylinder, error in
timing, loss of liquid, reading by sight, etc.).
Nevertheless, even other sources of error prevail, most importantly not giving the system enough
time to stabilize, not having good control over the power input to the boiler, and judging the
degree of foaming subjectively.

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CHEN 410: Unit Operations Lab Experiment: Distillation

5. Conclusion

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CHEN 410: Unit Operations Lab Experiment: Distillation

References

1- Thermopedia.com. (2017). DISTILLATION. [online] Available at:

http://www.thermopedia.com/content/703/ [Accessed 8 Mar. 2017]
2- Anon, (2017). [online] Available at: 1-
https://www.slideshare.net/kumarsachin3801/distillation-column [Accessed 8 Mar. 2017].
3- En.wikipedia.org. (2017). Continuous distillation. [online] Available at:
https://en.wikipedia.org/wiki/Continuous_distillation [Accessed 8 Mar. 2017].

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CHEN 410: Unit Operations Lab Experiment: Distillation

Appendix

Table 4: Temperatures of the eight trays and the reboiler (T9) at

Temperatures ( C)
Power (kW) T1 T2 T3 T4 T5 T6 T7 T8 T9

0.11 77.5 77.7 78 78 78.4 78.7 78.5 78.9 81

0.55 78.1 78.1 78.3 78.3 78.7 78.9 78.7 79.1 81.2
0.7 78.2 78.1 78.3 78.4 78.6 78.9 78.7 79.2 81.3
0.85 78.2 78.2 78.5 78.5 78.7 79 78.9 79.3 81.3
1 78.2 78.2 78.5 78.6 78.8 79.1 79 79.4 81.4
1.15 78.2 78.3 78.6 78.7 79 79.2 79 79.4 81.5

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