BKF3751-Chemical Engineering Laboratory II

1.0

Introduction

1.1

Introduction (Literature review and theory)

Short path distillation is a distillation technique that involves the distillate travelling a

short distance, often only a few centimeters, and is normally done at reduced pressure. The vapor
stream travels a "short path" directly to the condenser which is located within the evaporator
chamber. Since the vapor stream is immediated condensed, the short path distillation process
precludes the vapor from forming vapor pressure. This allows ultimate pressures of 0.001 mbar
to be attained. Short residence time and low evaporation temperature will cause a minimum
thermal stress to the distilled product. This also allows heat sensitive materials to undergo
purification at much lower temperatures preventing degradation. A short path ensures that little
compound is lost on the sides of the apparatus. Typical applications are high molecular organic
compounds particularly from the fields of chemistry, pharmaceutical and food industry.
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 vaporization 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 vapors 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 condense.
Separation processes can essentially be termed as mass transfer processes. The
classification can be based on the means of separation, mechanical or chemical. The choice of
separation depends on the pros and cons of each. Mechanical separations are usually favored if
possible due to the lower cost of the operations as compared to chemical separations. Systems
that cannot be separated by purely mechanical means (e.g. crude oil), chemical separation is the
remaining solution. The mixture at hand could exist as a combination of any two or more states:
solid-solid, solid-liquid, solid-gas, liquid-liquid, liquid-gas, gas-gas, solid-liquid-gas mixture.
Separation of components from a liquid mixture via distillation depends on the
differences in boiling points of the individual components. Also, depending on the
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BKF3751-Chemical Engineering Laboratory II

concentrations of the components present, the liquid mixture will have different boiling point
characteristics. Therefore, distillation processes depends on the vapor pressure characteristics of
liquid mixtures. The vapor pressure of a liquid at a particular temperature is the equilibrium
pressure exerted by molecules leaving and entering the liquid surface. Here are some important
points regarding vapor pressure: energy input raises vapor pressure, vapor pressure is related to
boiling, a liquid is said to boil when its vapor pressure equals the surrounding pressure, the ease
with which a liquid boils depends on its volatility liquids with high vapor pressures (volatile
liquids) will boil at lower temperatures, the vapor pressure and hence the boiling point of a liquid
mixture depends on the relative amounts of the components in the mixture, distillation occurs
because of the differences in the volatility of the components in the liquid mixture. The
Separation efficiency denotes by:
Separation efficiency =

X 100

Mechanical stirring a determining factors for the distillation efficiency, mechanical

stirring ensures a complete mixing and a better heat transfer rate between the hot oil jackets and
the feed. The higher degree of stirring increasing the heat transfer rate subsequently bringing the
higher distillation effect.
Temperature of the evaporator is another important variable in optimizing the distillation
efficiency where the optimum temperature should have to be selected to supply enough heat for
the water to be condensed. The distillation efficiency will be increased by increasing of
temperature. However, excessive of heat can result in degradation of product.
Feed rate control is crucial in distillation process, as the residence time in the evaporator
determine the efficiency of heat transfer. If the feeding rate is high then the residence time of
feed in evaporator decrease may causing the feed to be not well heated. Hence the feed will be
passing through without any separation happen.

BKF3751-Chemical Engineering Laboratory II

1.2

Objectives
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.

BKF3751-Chemical Engineering Laboratory II

2.0

Methodology

2.1

Equipment/Apparatus/Material
1. Short Path Distillation Unit
2. Ethylene glycol water mixture

2.2
1.

Procedures
The ethylene glycol is mixed with water in a ratio of 7:3 at total of 1 litre in a beaker. Then
the mixture is stirred homogeneously.

2.

All valves are initially checked closed except the valves HV02, HV04, HV05, HV11 and
HV12. The cold trap is ensured to be filled with dry ice.

3.

Valve HV-01 is removed and the feeding funnel V-100 is filled with the homogeneous
mixture.

4.

The main power supply at the control panel is switched ON.

5.

The computer and the software program are turned ON.

6.

The thermostat is set at 70C, Chiller at 12C and vacuum pump pressure at 100mbar. The
pressure throughout the experiment is manually mantained. [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.

Valve HV-13 is opened 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
experiment is started.

9.

Every set of experiment is run for 10 minutes. After 10 mins, the volume of distillate is
recorded down from V-104 and volume of concentrate from V-105-107.

10. The experiment is repeated with different operating parameters as shown in the table in
result and discussion.

BKF3751-Chemical Engineering Laboratory II

SAMPLING PROCEDURE
1.

For every batch of experiment, HV03 is kept opened at each sampling to ensure the flowrate
is constant throughout experiment. To do this, the vacuum pump is switched off, while
HV07, HV08 and HV09 are opened 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, HV07, HV08 and HV09 are closed. The next
experiment is continued by switching on the vacuum pump again.

3.

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

4.

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

BKF3751-Chemical Engineering Laboratory II

3.0

Result and Discussion

3.1

Result

3.1.1 Effect of stirrer speed

Vacuum Pressure, PT-200

100mbar

Evaporator Temperature, TT-100

70oC

Feed Flow Rate

13ml/min

Contact Time

10min

EG-Water Ratio

7:3

Time Start

Stirrer Speed
(rpm)
50
100
200
220

0920
0930
0940
0950

Distillate
Volume (ml)
23
19
16
15

Concentrate
Volume (ml)
87
90
97
100

Separation
Efficiency (%)
66.92
69.23
74.62
76.92

Concentrate
Volume (ml)
100
50
42
40
38

Separation
Efficiency (%)
76.92
38.46
32.31
30.77
29.23

3.1.2 Effect of evaporator temperature

Feed Flow Rate

13ml/min

Stirrer Speed, M-500

220rpm

Vacuum Pressure

100mbar

Contact Time

10min

EG-Water Ratio

7:3

Time Start

Temperature (oC)

0950
1000
1010
1020
1030

70
72
74
76
80

Distillate
Volume (ml)
15
15
13
12
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BKF3751-Chemical Engineering Laboratory II

3.2

Discussion

The graph of stirrer speed against separation efficiency and evaporator temperature against
separation efficiency are as below:

Graph of Stirrer Speed against Separation

Efficiency
78

Separation Efficiency (%)

76
74
72
70
68
66
0

50

100

150

200

250

Stirrer Speed (rpm)

Graph 1: Graph of Stirrer Speed against Separation Efficiency

Graph of Evaporator Temperature against

Separation Efficiency
90

Separation Efficiency (%)

80
70
60
50
40
30
20
10
0
68

70

72

74

76

78

80

82

Evaporator Temperature (oC)

Graph 2: Graph of Evaporator Temperature against Separation Efficiency

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BKF3751-Chemical Engineering Laboratory II

Under same temperature, when stirrer speed increase, distillate volume decrease and
concentrate volume increase and thus separation efficiencies increase. However, distillate
volume and concentrate volume are both decrease when evaporator temperature increase and
stirrer speed is constant. Thus, the separation efficiencies decrease.
The separation efficiency at different operating conditions is calculated using the
following formula:
Efficiency

ConcentrateVolume
x100 %
Feed Volume

Short path distillation also called molecular distillation. It offers the advantage of
distillation at considerably reduced pressure and thus reduced evaporation temperature with
economical distillation rates. As the distance for the vapors between evaporator and condenser is
extremely short and thus it is no pressure drop. So the obtainable vacuum is not limited. Short
path distillation can be applied whenever all other distillation methods lead to thermal product
damage, or rough vacuum require extremely high temperature.
As mentioned, short path distillation is applied whenever heat-sensitive substance have to
be distilled for purification, typical applications are particularly from the field of chemistry,
pharmaceuticals, plastic industry, cosmetics industry and food industry. Typical examples of
such heat-sensitive products are synthetic vitamins, paraffin waxes, derivatives of alkaloid, e.g.
Quinine and THC, acrylates, plasticizer, fragrance, and essential oils such as ginger oil, pepper
oil, fish oil and others.

BKF3751-Chemical Engineering Laboratory II

4.0

Conclusion and Recommendations

From the experiment, it can be concluded that as the stirrers speed increases, the volume of pure
ethylene glycol increases, while the volume distillate of pure water decreases. On the other hand,
as the temperature increases, the distillation of pure water increases, while the condensate of
ethylene glycol decreases. Therefore, an increase of stirrer speed in short path distillation,
improves the separation efficiency of the homogenous mixture. The maximum separation
efficiency achieved is 76.92% at stirrer speed of 220rpm.
To ensure constant feed flow rate, HV03 should not be closed at each sampling. Instead, switch
off the vacuum pump, open HV07, HV08 and HV09 to let the condensate and distillate to flow
into V104 to V107 respectively.

BKF3751-Chemical Engineering Laboratory II

5.0

Reference

Retrieved 29 July, 2010 from http://www.bayertechnology.com/en/products/reaction-and-polymertechnology/stirring-technology/our-service.html

Retrieved 29 July, 2010 from http://lorien.ncl.ac.uk/ming/distil/distildes.htm

Retrieved 29 July, 2010 from http://www.avta-us.com/basics.html
Retrieved 29 July, 2010 from http://www.chemtechservicesinc.com/short-path-distillation.html

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BKF3751-Chemical Engineering Laboratory II

6.0

Appendix

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