Chemical Engineering Laboratory II

BKF3751
EXPERIMENT 7: SHORT PATH DISTILLATION

OBJECTIVE
1. To introduce the short path distillation principles using continuous system.
2. To observe the effects of stirrer speed and temperature on the efficiency of separation, e.g
ethylene glycol-water.

INTRODUCTION
This Short Path Distillation is a thermal separation process for thermal sensitive products.
Short residence time and low evaporation temperature will cause a minimum thermal stress to the
distilled product. Typical applications are high molecular organic compounds particularly from the
field of chemistry, pharmaceutical and food industry. Distillation is one of the most important
thermal separation methods.
Short path distillation is a continuous separation process working under vacuum conditions.
Evaporation takes place from a heated wiped film. Caused by the pressure drop between the place
of evaporation and the vacuum system the operating pressure in typical wiped film evaporators with
external condenser is limited to some millibars.
The considerably lower pressure in the short path evaporator is obtained by the short
distance for the vapours on their way from the evaporator surface to the condenser. In addition,
the cross section area of flow is equal to the evaporator surface, so that there is only a minor
pressure drop between evaporator and condenser

EQUIPMENT/APPARATUS/MATERIAL

1. Short Path Distillation Unit

2. Ethylene glycol – water
mixture
Chemical Engineering Laboratory II
BKF3751

EXPERIMENTAL PROCEDURES

1. Mix the ethylene glycol and water with a ratio of 7:3 at total of 1 litre in a beaker. Then stir
the mixture homogeneously.

2. Check that all valves are initially closed except the valves HV02, HV04, HV05, HV11 and
HV12. Ensure that the cold trap is filled with dry ice.

3. Remove valve HV-01 and fill the feeding funnel V-100 with the homogeneous mixture.

4. Switch ON the main power supply at the control panel.

5. ON computer or the software program.

6. Set the thermostat at 70°C, Chiller at 12°C and vacuum pump pressure at 100mbar.
Manually maintain the pressure throughout the experiment. [To adjust vacuum pump
pressure, manually adjust valve, V14. To adjust the desired flow rate, adjust the opening
valve HV03. To adjust the desired stirrer speed, adjust it from the software].

7. Open valve HV-13 to allow for some of the hot bath to circulate through the heating jacket
of the feeding funnel to pre-heat the feed in the funnel.

NOTE: Valve HV13 must be close before switching off the thermostat, B-400.
8. Once the chiller temperature and thermostat temperature have reach the set points, the
equipment is ready for experiment
9. For every set of experiment, run for 10 minutes. After 10 mins, records down the volume of
distillate from V-104 and volume of concentrate from V-105-107.

10. Repeat the experiment with different operating parameters as shown in the table in result and
discussion.

11. Follow the operating procedure to shut down the equipment. DO NOT let the wiper roller to
run without the flow of feed.
Chemical Engineering Laboratory II
BKF3751

SAMPLING PROCEDURE

1. For every batch of experiment, to ensure the feed flowrates are the same, HV03 should not
be close at each sampling. To do this, switch off the vacuum pump, open HV07, HV08 and
HV09 to let the condensate and distillate to flow into V-104 to V-107 respectively.

2. After all the liquid are flows into each vessel. Close back HV07, HV08 and HV09. Continue
to run the next experiment by switching on the vacuum pump again.

3. The collected distillate and condensate can then be used for further testing.

4. The feed flowrate is calculated by dividing the total volume of sample collected to the total
time taken.

GENERAL SHUT-DOWN PROCEDURES

1. Switch off vacuum pump.
2. Close valve HV03 to stop feeding.
3. Switch off stirrer motor.
4. Turn off thermostat. Close HV13.
5. Open valve HV 01, HV 06 and HV 07.
6. After 15 minutes, switch off chiller and turn off the main power.
NOTE: DO NOT attempt to remove any vessel while the vacuum pump is running.

RESULT
1. Effect of stirrer speed

Vacuum pressure, PT-200 100mbar

Evaporator Temperature, TT-100 70°C
Feed Flow rate ml/min
Contact time 10 min
EG-water ratio 7:3

Distillate Concentrate Separation

Time Start Stirrer Speed(rpm)
Volume (ml) Volume (ml) Efficiency (%)
Chemical Engineering Laboratory II
BKF3751

50
100
200
220

2. Effect of evaporator temperature

Feed flow rate ml/min

Stirrer speed, M-500 220rpm
Vacuum pressure 100mbar
Contact time 10min
EG-water ratio 7:3

Distillate Concentrate Separation

Time Start Temp (°C)
Volume (ml) Volume (ml) Efficiency (%)
70
72
74
76
80
Chemical Engineering Laboratory II
BKF3751

V-100 V-101 V-102, V-103 V-104 to V-107 V-108 T-200

Feeding Funnel Cold Trap Graduated Cylinders Product Vessels Vessels Short Path Evaporator
Material: Boro. glass Material: Boro. glass Material: Boro. glass Material: Boro. glass Material: Boro. glass Material: Boro. glass
Capacity: approx. 2000 ml For dry ice usage Capacity: 250 ml Capacity: 250 ml Capacity: 20 ml c/w roller wiper cage (Rulon rolls); magnetic
c/w tempering jacket; pressure c/w drain valve DN6 c/w/ DN3 valves for inlet Round bottom Round Bottom stirrer sealing, heating jacket (0.03 m2);
equalizing tube, needle valve Vacuum: 2x KF15/3 outlet & venting cooling coil (0.05 m2); Feed: NS29/32;
Inlet: GL45; Outlet: NS29/32 Outlet: NS29/32 Inlet: NS29/32; Outlet: NS29/32 Outlet: NS29/32; Vacuum: NS29/32

E-300 E-301 B-400 B-401 M-500 P-100

Heating Jacket Cooling Coil Thermal Oil Bath Chiller Stirrer Drive Vacuum Pump
Material: Boro. glass Material: Boro. glass Range: 28 to 280 °C (±0.01 K) Range: 5 to 25 °C (±2 °C) Power: 100 W 2-stage Rotary Vane Type
Surface: 0.03 m2 Surface: 0.05 m2 Heater: 3000 watt Cooling capacity: 18,000 BTU/hr Torque: 250 Ncm Ultimate Vacuum: 6 x 10-3 mbar
Bath capacity: approx. 12-L Bath capacity: 50-L Speed: 8 to 2000 rpm Pumping Speed: 2.9 m3/hr
Pump: max. 24 LPM Pump: 50 LPM Output: 0 – 10V

HV 01

V-100 HV 02
HV 13

SIC
TIC TT 500
100 100 ST
500

M
M-500 HV 03

El. B-400 TT
102

T-200

PT (E-300, E-301)
200

Vent
V 14

P-100 TT
V-101 HV 04 103 HV 05

HV 06 HV 07

HV 10
V-102 V-103

V-108

HV 12
TIC TT
101 101 HV 11
HV 08 HV 09

El. B-401

V-104 V-105 V-106 V-107

Short Path Distillation Unit

Chemical Engineering Laboratory II
BKF3751

ANALYSIS AND DISCUSSIONS:

1. Plot a graph of stirrer speed vs. separation efficiency and evaporator temperature
vs. separation efficiency.
2. Discuss the effects of the parameters on the thermal separation efficiency.
3. Briefly explain the importance and application of short path distillation system in
industry.