2010 2nd International Conference on Chemical, Biological and Environmental Engineering (ICBEE 2010)

Effect of variable reflux ratio on binary distillation in a laboratory scale distillation

column

Amir Shafeeq, Syed Sheraz Daood, Ayyaz Muhammad and Aamir Ijaz
Institute of Chemical Engg. & Tech. University of the Punjab, Lahore, Pakistan

Abstract- This paper investigates the effect of variable reflux The distillation column operation may also be affected
ratio on final product composition in a laboratory scale by vapour flow conditions such as foaming which could be
distillation column. The findings of this study include a due to the expansion of liquid within the vapor flow. Though
minimum reflux ratio at which the highest purity of the it provides high interfacial liquid-vapour contact, excessive
product could be achieved. The experimental setup is a foaming would lead to liquid holdup on trays. Entrainment
Technovate Distillation Column with five sieve plates, a feed is another important factor and refers to the liquid carried
tank, a reboiler, and a condenser. The feed and reflux ratio along with vapor stream. This could be due to high vapor
was varied with the help of flow meters associated with two flow rates. This could reduce the tray efficiency because low
centrifugal pumps. The feed composition was set to 45 percent
ethanol-water mixture. The final composition obtained was
!
volat l� material could be to a plate holding liquid of higher
volatlitty. It could also result in contaminating the high
95% ethanol in the distillate. The minimum reflux ratio was
purity distillate and would also lead to flooding [4-6].
found to be 60 percent of maximum flow.
Weeping is another term in distillation which could be
Keywords: Binary distillation, Reflux ratio due to low vapor flow. The pressure exerted by the vapour
could not be sufficient for liquid hold up above the tray.
I. INTRODUCTION Hence, liquid starts to perforate through the tray holes.
Excessive weeping could lead to dumping. Dumping is a
Distillation is a process in which a liquid or vapour
. term to show the case when the liquid from all the trays
mIxture of two or more substances is separated into its
would crash (dump) to the base of the column and that could
component fractions using the difference in their boiling
result in the shut down of the distillation column operation.
points. The basis of distillation is that the vapors of a boiling
Weeping could be indicated by a sharp pressure drop in the
mixture would be rich with the components having lower
column. Flooding could be due to excessive vapor flow thus
boiling points. Hence, on cooling, the condensate would be
causing liquid to be entrained in the vapour up the column.
having more volatile components. On contrary, the original
The increased pressure from excessive vapour could also
mixture would be rich in less volatile substance [1,2].
cause an increase in the liquid holdup on the
Amongst the various factors effecting distillation is feed
plate. Depending on the degree of flooding, the maximum
composition that would have an impact on the number of
capacity of the column could be severely reduced. Flooding
stages required for effective separation as well as location of
could be detected by a sharp increase in column differential
the feed tray. To overcome the problems associated with the
pressure and significant decrease in separation efficiency [7-
feed composition, distillation column could be designed to
8].
have more than one feed points. The other most important
The present study has been conducted keeping in view of
factor is reflux ratio. With the increase in reflux ratio, the
all the above factors for a case of binary distillation of a
amount of liquid being rich in the more volatile components
system of ethanol-water mixture. A laboratory scale
would be recycled into the column. This result in good
distillation column shown in Fig. 1 is used for this purpose.
separation and also less number of trays is needed to achieve
The column is operated at different reflux ratios to find the
the same degree of separation. The required number of trays
one that gives optimum performance.
is minimum in case a distillation column would be operated
under total reflux conditions [3].

978-1-4244-8749-3/10/ $ 26.00 © 2010 IEEE 35

 2010 2nd International Conference on Chemical, Biological and Environmental Engineering (ICBEE 2010)

0 Thermocouple

� Sample Port

>- Feed Port

em Turbine Aow-f eter

Otstllate
Recei'ler

Alternate
Feed Tank

Fig.1 Technovate Distillation Column at I.C.E.T P.U LHR PAK

A. Experimental Setup o Power input indication with Volt meter

The pilot scale distillation column consists of: and Ammeter.
• Feed tank: Stainless steel tank. Capacity= o Pump control switches for feed and
approximately 8.0 gal. reboiler pumps.
• Reboiler: Stainless steel tank. Capacity= o Thermal overload indicator for reboiler.
approximately 4.0 gal. o Feed and reflux preheater continuously
• Condenser: Coil and Tube heat exchanger. Pyrex variable controls.
outer tube. Stainless steel inner coil. Counter-current o Feed pump indicator light.
flow configuration with chilled water as the cooling o Reflux, product and bottoms pump
fluid. Heat transfer area is about 1.5 ff. controls.
• Distillate Receiver: Pyrex cylinder capped top and • Rotometers for flow measurement:
bottom with stainless steel. Diameter= 3 in. Height= o feed
12 in.
o reflux
• Immersion Preheaters: Two cartridge heaters; Feed:
750 watts, Reflux: 500 watts.
B. Materials and Methods
• Control Panel:
The following chemicals were used in the present study.

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 2010 2nd International Conference on Chemical, Biological and Environmental Engineering (ICBEE 2010)

1. Ethyl Alcohol (Analytical Grade)

2. Water

A mixture of 45% ethanol in water was taken in the feed

tank and then fed to the reboiler with the help of feed pump.
The amperage of reboiler was set at 14. Cooling water
supply to the condenser was energized. The feed pump was
switched on such that feed was introduced in the reboiler
during the operation of distillation column keeping the liquid
level and composition in the reboiler constant with the help
of auto drain switch. The experimental study was performed
at different reflux ratios with the help of reflux pump. The
Fig. 3. Impact of Percent Reflux on Distillate
temperature and composition of distillate was noted at
various reflux ratios. The experimental data is being
II. DISCUSSION ON RESULTS
tabulated in Table 1 and 2. The curves thus obtained have
been shown in Fig. 2 and 3. It is observed that variation in temperature is not much
pronounced at higher reflux ratios. This shows that
increasing reflux ratio beyond the minimum value i.e. 60
TABLE 1: EFFECT OF % REFLUX ON PLATE TEMPERATURE percent does not have any significant impact on temperature
variation on plates and percentage purity of the product but
% Reflux Plate Tern erature °c
causes an increase in reboiler duty and thus increasing load
1 2 3 4 5 on condenser. It is also observed that increasing the reflux
20 81 80.5 79.5 79 78.1 ratio of the column increases the degree of separation
40 79 78.1 78 77.9 76.9
between the still composition and the distillate composition
thus allowing a distillate of higher purity to be obtained.
60 78.5 78.1 78 77.8 76.8
However beyond the minimum reflux ratio i.e. 60 percent,
80 78.5 78 78 77.9 76.8
the concentration of light key i.e ethanol in the distillate
100 78.5 78 78 77.7 76.6 almost remains constant i.e. 95 percent.

III. CONCLUSION
Impact of Percent Reflux on Plate Temperature
Water and Ethanol mixture is difficult to separate due to
85 ,-
---, their close boiling points. This could be achieved by making
an azeotrope to change the boiling point of mixture. This
results in the increase of degree of separation. A number of
chemicals could be used for this purpose. Modem
techniques could also be employed which make use of
molecular sieves that would enhance the separation
efficiency.
79

ACKNOWLEDGEMENT

77
The authors acknowledge the support provided by
Institute of Chemical Engg. & Tech., University of the
Punjab, Lahore, Pakistan to carry out this study.
75 .1------__------__----__------------__---------1

P1ateNo.

1__ 20 -'-40 __ 60 ___ 80 ....... 1001

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• Fig. 2. Impact of percent Reflux on Plate Temperature [I] Coulson & Richardson's Chemical Engineering, 5th ed., Vol.2,
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 2010 2nd International Conference on Chemical, Biological and Environmental Engineering (ICBEE 2010)

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