BATCH DISTILLATION AT CONSTANT REFLUX
EXPERIMENT 2: BATCH DISTILLATION AT CONSTANT REFLUX OBJECTIVE:
To operate a batch distillation unit at constant reflux.
To examine the change in top and bottom composition over time in a batch distillation.
PROCEDURES:
1. Perform the general start-up procedures (Section 4). Refer appendix 1.
2. Record initial volume and refractive index of the liquid mixture in the reboiler.
3. Set the heater power to 1.5kW.
4. Set reflux timer to 10 second for set 1 and 30 second for set 2.
( Note: Set 1: Product liquid to tank B4 (distillate) ; Set 2: Product liquid return to column (reflux)). Set the reflux control to position 3. (Timer controlled reflux).
5. As the top column temperature sensor, TT 112 reach steady state, record the temperature.
6. Open sampling valve V9 and collect 10ml of distillate sample using conical flask. Close valve V9.
7. Adjust bottom overflow level. Open valve V2 and V3 and collect 10 ml of sample bottom product using conical flask.Close valve V2 and V3.
8. Measure the refractive index of the samples and record the value into data table.
(Note: Do not discard the sample as to perform material balance at the end of the experiment.)
9. Repeat steps 6 to 9 until the bottom sample RI values constant.
10. Switch off heater power and allow the system to cool down to ambient temperature.
Optional Mass Balance Calculation:
11. Open drain valve V12 and collect all the liquid from the reboiler. Measure the volume and refractive index of the liquid. Record all the values.
12. Open valve V7 and collect all the distillate from product tank. Measure the volume and refractive index of the distillate. Record all the values.
(Note: Remember to include all previous samples.)
ANALYSIS & DISCUSSION:
1. Use the sample table in Appendix 1b for data collection.
2. Compare the quality of distillate among the sieve tray column and the packed column.
3. Using the X-Y equilibrium diagram for ethanol-water system, mark the top and bottom compositions for each
To operate a batch distillation unit at constant reflux.
To examine the change in top and bottom composition over time in a batch distillation.
PROCEDURES:
1. Perform the general start-up procedures (Section 4). Refer appendix 1.
2. Record initial volume and refractive index of the liquid mixture in the reboiler.
3. Set the heater power to 1.5kW.
4. Set reflux timer to 10 second for set 1 and 30 second for set 2.
( Note: Set 1: Product liquid to tank B4 (distillate) ; Set 2: Product liquid return to column (reflux)). Set the reflux control to position 3. (Timer controlled reflux).
5. As the top column temperature sensor, TT 112 reach steady state, record the temperature.
6. Open sampling valve V9 and collect 10ml of distillate sample using conical flask. Close valve V9.
7. Adjust bottom overflow level. Open valve V2 and V3 and collect 10 ml of sample bottom product using conical flask.Close valve V2 and V3.
8. Measure the refractive index of the samples and record the value into data table.
(Note: Do not discard the sample as to perform material balance at the end of the experiment.)
9. Repeat steps 6 to 9 until the bottom sample RI values constant.
10. Switch off heater power and allow the system to cool down to ambient temperature.
Optional Mass Balance Calculation:
11. Open drain valve V12 and collect all the liquid from the reboiler. Measure the volume and refractive index of the liquid. Record all the values.
12. Open valve V7 and collect all the distillate from product tank. Measure the volume and refractive index of the distillate. Record all the values.
(Note: Remember to include all previous samples.)
ANALYSIS & DISCUSSION:
1. Use the sample table in Appendix 1b for data collection.
2. Compare the quality of distillate among the sieve tray column and the packed column.
3. Using the X-Y equilibrium diagram for ethanol-water system, mark the top and bottom compositions for each