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EXPERIMENT NO.

BINARY BATCH DISTILLATION IN BUBBLE CAP TRAY COLUMN


Introduction
Distillation is a unit operation [or method] used to separate the components of a liquid solution. This
process depends upon the distribution of the various components of the liquid mixture between the liquid and
vapour phases. The basic requirement is that the equilibrium vapour phase composition be different from the
composition of the liquid phase at its boiling point. A distillation method is said to be in total reflux if all of the
vapour produced during the operation is returned to the still. Thus, the reflux ratio is given as R = . Variable
and constant reflux are based on the return of part of the condensate to the still under such conditions that this
returning liquid is brought into intimate contact with the vapors on their way to the condenser. Assuming
equimolal overflow, the reflux ratio can be calculated from the general material balance around the dashed-line
section shown on Figure 1. The equation is given by Geankoplis (1995) as
+1 = +
; ,
+1 +1 = + ; +1

+1 =
+
; +1 = + ,
=
+1
+1
+1 + 1

+1 =
+

+1 +1
+1
=

+1
where R = Ln/D = reflux ratio =constant, and the yn+1, xn, and xD can be obtained in relation to Figure 1.
Two common methods used to calculate the relationship between the number of trays, liquid/vapor
ratios, and product composition for a binary mixture (A and B) are the Ponchon and Savarit method and the
McCabe and Thiele method. The former requires detailed enthalpy data while the latter does not and is
therefore also less accurate. Often the McCabe-Thiele method is adequate because the enthalpy effects are not
large.
The effect of the varying compositions of the bottoms product and the distillate [through the use of a
refractometer] to the subsequent calculation of the reflux ratio is explored in this experiment. The column is a
four-tray laboratory distillation column made of glass, with one large bubble-cap on each tray. It is operated
essentially at barometric pressure.

V1
y1

1
x1

L1

y2
2

L
xD

D
xD

x2
yn

xn

Ln
n+1

yn+1

Vn+1

F
xF

Figure 1. Material Balance for Enriching Section: Schematic Diagram

1.

Objectives
1.1. To perform distillation of a binary mixture using the bubble-cap tray column
1.2. Compute the initial and final reflux ratios for the process
1.3. Plot the concentration profile for distillation at total reflux, constant reflux, and variable reflux

2.

Materials and Methods


2.1. Equipment/Apparatus
2.1.1. Sampling bottles
2.1.2. Bubble cap distillation column
2.1.3. Refractometer
2.1.4. Thermometer
2.2. Chemicals and other Materials
2.2.1. Ethanol
2.2.2. Distilled Water
2.2.3. Safety gloves
2.2.4. Laboratory goggles
2.2.5. Face Mask
2.3. Equipment Setup
Cold Water

Cold Water

#5
#4
Condenser
#3
Bubble cap
#2
Bottom
#6
Disltillate

Heating mantle

Figure 2. The Sketch of Experimental apparatus


2.4. Procedure
2.4.1. Prepare a 5-L solution containing 40% volume ethanol and 60% volume water.
2.4.2. Introduce solution to still and proceed with batch distillation at total reflux.
2.4.3. When the solution boils, collect sample both the distillate and bottom product composition
analyses at 5 minute interval for 20 minutes and analyze using refractometer. Make sure you are
on your proper PPE to avoid inhaling vapours.
2.4.4. Open the reflux knob and hold constant for 20 minutes. When temperatures stay steady (as
shown by notes in the lab record), samples can be taken and analyzed every 5 minutes. Note the
tray or stream from which each sample was taken. Sampling should be continued until successive
values agree closely.

2.4.5. Lastly, vary reflux by turning the reflux knob.


2.5. Note the following precautions in operating the column:
2.5.1. Cooling water to the condenser must be on at all times during operation, so that there is no
thermal shock in the condenser and no vapours escape to the atmosphere.
3.

Data Tables
3.1. Calibration Plot
3.2. Solution Composition
Table 1. TOTAL REFLUX Data
Time (min)

Tray #

Bottom

Refractive
Index

Temperature,
o
C

Ethanol Concentration,
mol frxn
Liquid, x
Vapor, y

2
3
4
5
Distillate
Table 2. VARIABLE REFLUX Data
No. of
Turns

Time (min)

Tray #

Bottom

Refractive
Index

Temperature,
o
C

Ethanol
Concentration,
mol frxn
Liquid, x
Vapor, y

2
3
4
5
Distillate
4.

Guide Questions for Discussion


4.1. Calculate the reflux ratio, the overall plate efficiency, and the Murphee plate efficiency for each plate
and the reboiler. How could the separation be improved?
4.2. Is the feed entering at the proper plate? Would a change in the flow pattern between the bottom of the
column and the reboiler be (i) beneficial and (ii) practical?
4.3. Why (do you think) is the apparatus set to 100% reflux and why is that reflux returned to the topmost
tray?
4.4. Where in the column is the temperature highest?
4.5. What conclusion can you draw regarding the number of required equilibrium stages as a function of
the reflux ratio?
4.6. Why is a total condenser not considered an equilibrium stage?
4.7. How can the heat losses be minimised? How can the equipment be made more energy efficient?
4.8. In a given setup how does reboiler heating, reflux ratio, feed conditions influence the degree of
separation?

5.

References
5.1. Geankoplis, C. (1995) Transport Processes and Unit Processes, 3rd edition. Singapore: Prentice Hall
International, Inc.