Unit Operation Laboratory BSK3472

EXPERIMENT 8

BATCH DISTILLATION AT TOTAL REFLUX

USING SIEVE TRAY DISTILLATION

OBJECTIVE
To determine the height equivalent theoretical plates (HETP) at total reflux.
To determine the effect of liquid and vapor loading on the HETP at total reflux.

EXPERIMENTAL PROCEDURES I
Preparation of a Refractive Index (RI) vs. Composition Plot
1. Prepare a set of mixtures containing ethanol and water within a specified range of
composition between pure water and pure ethanol as following :

Table 1: Composition Data Based on Refractive Index

Volume of Volume of Mole fraction Ethanol Refractive
ethanol water (ml) ethanol wt% index (RI)
(ml)
0.0 10.0
1.0 9.0
2.0 8.0
3.0 7.0
4.0 6.0
5.0 5.0
6.0 4.0
7.0 3.0
8.0 2.0
9.0 1.0
9.5 0.5
1 10.0 0.0

2. For each mixture, obtain their refractive index (RI) readings using refractometer.

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 Unit Operation Laboratory BSK3472

3. Prepare a plot of refractive index (RI) vs. ethanol mole fraction for the whole range of
mixtures. This will serve as the calibration curve for further experiments

EXPERIMENTAL PROCEDURES II
1. Prepare a set of mixtures containing ethanol and distilled water at desired composition (for
instance 5L mixture containing 2L of ethanol and 3L of distilled water).

2. Collect 10ml of ethanol and distilled water mixture to determine ethanol concentration in
aqueous solution using a refractometer.

3. Ensure all valves of Sieve Tray Binary Fractional Distillation unit are closed.

4. Open the charge port cap and charge the reboiler B1 with the ethanol-distilled water mixture.
Close the charge port cap.

5. Prepare another mixture of ethanol and water (4L of pure ethanol and 6L of filtered water)
and pour into feed tanks B2 and B3 separately.

6. Make sure all the valve are properly close except V1.

7. Turn on the main power on the control panel.

8. Open the main cooling water valve V1. Let the cooling water flow into the condenser (W2).

9. Switch on the cartridge heaters W1a & W1b and set the heater power controller to 1.0 kW
and allow the reboiler temperature reach approximate 85oC.

10. Ensure the reflux control is 1 position. (total reflux)

11. As the top column temperature sensor TT 112, reach steady state, record the temperature.
2

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 Unit Operation Laboratory BSK3472

12. Measure the distillate flow rate as follows:

a) Set the reflux control to position 1 (Total reflux)
b) When the distillate start flowing into the phase separator, start the timer.
c) As distillate reach 200 ml on the measure tank, stop the timer.
d) Determine the flow rate of the distillate.

13. Set the reflux control to position 2 (Total distillate offtake). Open valve V9 and collect 10 ml
sample distillate using conical flask. Close valve V9 and set the reflux control to position 1.
(Total reflux).

14. To collect bottom product sample, open valve V8 and collect 10 ml of sample bottom
product using conical flask. Close valve V8.

15. Find the concentration of ethanol for distillate sample and bottom products sample by using a
refractometer.

16. Wait approximately 15 to 30 minutes and allow the distillation unit to achieve new steady
state.

17. Repeat steps 9 to 15 for different ethanol-distilled water mixture loading, adjust the heater
power settings according table below:
Heater Power
(kw)
1.00
1.50
2.00

18. Switch off heater power and allow the system to cool down to ambient temperature.

Faculty of Industrial Sciences & Technology, UMP

 Unit Operation Laboratory BSK3472

RESULT & DISCUSSION

1. Using the X-Y equilibrium diagram for ethanol-water system, mark the top and bottom
compositions on the diagram and determine the theoretical number of plates in the
distillation unit using the McCabe-Thiele method.

2. Calculate the height equivalent theoretical plates (HETP) by dividing the effective column
height with the number of theoretical plates.

3. Plot a graph of HETP vs. Heating Power and observe the relationship.

Faculty of Industrial Sciences & Technology, UMP

 Unit Operation Laboratory BSK3472

EXPERIMENTAL DATA SHEET

Table 1: Composition Data Based on Refractive Index

Volume of Volume of Mole fraction Ethanol Refractive
ethanol water (ml) ethanol wt% index (RI)
(ml)
0.0 10.0
1.0 9.0
2.0 8.0
3.0 7.0
4.0 6.0
5.0 5.0
6.0 4.0
7.0 3.0
8.0 2.0
9.0 1.0
9.5 0.5
10.0 0.0

Table 2: Data Collection for Distillate and Bottom Product

Heater Distillation Bottom Product HETP
W1, W2 Temp Refractive Mole Temp Refractive Mole (mm)
Power (oC) Index Fraction (oC) Index Fraction
(kW)
1.00
1.50
2.00

Faculty of Industrial Sciences & Technology, UMP