ChE 302 Chemical engineering laboratory - II

Experiment No. 1 Name of the experiment: Group No. 03 (A2)

EXTRACTION OF OIL FROM OIL CAKE BY SOXHLET EXTRACTOR

Submitted by: Md. Hasib Al Mahbub

Student Id: 0902045 Level: 3; Term: 1 Section: A2

Date of performance: 21/05/2013 Date of submission: 30/05/2013

Partners Student Id. 0902041 0902042 0902043 0902044

Department of Chemical Engineering. Bangladesh University of engineering and technology, Dhaka.

Summery
The main objective of this experiment was to have a basic idea about the solid-liquid extraction process which is industrially known as leaching process which was performed here by using a Soxhlet extractor apparatus. The percentage amount of extracted oil that was present in the oil cake and also the percentage recovery of the solvent used for the extraction process were to be determined. n-hexane was the solvent that was used in the Soxhlet extractor to carry out the extraction process. A usual distillation method was used for the recovery of the solvent. The calculated amount of the percent extraction of oil was found to be nearly about 3% and the percent recovery of the solvent was found to be equal to nearly about 70%.Through this experiment, the solid-liquid extraction process and also the siphoning phenomena were studied and our objectives were completed.

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Name of Apparatus and Solvent Used

Round bottom flask Electric heater Thimble Siphoning tube Soxhlet holder Condenser Conical flask Thermometer Solvent: n-hexane

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Experimental Setup a) Soxhlet Extraction

Hot water out Condenser

Cold water in Thimble with oil-cake

Vapor line Siphon n-Hexane in contact of oil-cake n-Hexane and oil Heater

Figure 2: Experimental Setup of Soxhlet Extraction Process.

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b) Recovery of n-Hexane

Hot water out n-Hexane and oil Heater Cold water in Recovered n-Hexane

Figure 3: Recovery of n-Hexane by Distillation.

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Observed data
For Soxhlet Extraction Process Weight of the empty round bottom flask Weight of the round bottom flux with n-hexane Weight of the empty thimble Weight of the thimble with oil cake For Distillation Process Weight of the empty conical flask Weight of the conical flask with recovered n-hexane Final weight of the round bottom flask with oil = 111.325 g = 176.391 g = 63.87g = 125.616 g = 219.158 g = 3.853 g = 31.526 g

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Calculated data
The initial weight of n-hexane taken Weight of the oil cake Weight of the extracted oil Weight of n-hexane recovered Percentage of extraction of oil Percentage of recovery of solvent = 93.542 g = 27.673 g = 2.639 g = 47.52g = 9.5 % = 69.55 %

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Sample Calculation
Initial Weight of n-Hexane Weight of empty round bottom flask = 125.616 g Weight of the round bottom flask with n-hexane = 219.158g Weight of n-hexane = (219.616 125.616) g = 93.542 g Weight of Recovered n-Hexane Weight of the empty conical flask = 111.325 g Weight of the conical flask with recovered n-hexane = 176.391 g Weight of the recovered n-hexane = (176.391 111.325) g = 65.066 g Weight of Oil Cake Weight of the empty thimble = 3.853 g Weight of the thimble with oil cake = 31.526 g Weight of the oil cake used for extraction = (31.526 3.853) g = 27.673 g Weight of the Extracted Oil Weight of the empty round bottom flask = 125.616 g Final weight of the round bottom flask with oil = 128.255 g Weight of the extracted oil = (128.255 125.616) g = 2.693 g

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Percentage of Extraction of Oil Percentage extraction of oil

Weight of the oil extracted from the oil cake 100% Weight of total oil present in the oilcake
2.693 100% 27.673

= 9.5 %

Percentage of Recovery of Solvent Percentage recovery of the solvent

Weight of n - hexane recovered 100% Weight of n - hexane taken initially

65.066 100% 93.542

= 69.55%

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Results & Discussions

In this experiment the following results were found: The percent of n-Hexane recovery = 69.55 % The percent of oil extracted = 9.5 %

In the experiment the amount of oil found in oil cake and the recovery of hexane was low. A large amount of hexane was lost during the experiment. The causes of this kind of results are given bellow:

A precondition for efficient extraction is proper preparation of raw material. It is experimentally proved that an efficient extraction cannot be achieved, unless the solvent is able to move freely through the material under examination. The oil cake sample should have particle size small enough to permit the solvent to reach right up to the core, but, not so small as to constitute fines; should have fairly uniform size so as to pack well in the extractor and should allow solvent to pass through freely. So the oil cake might not be grinded properly to reach high extraction. The experiment was completed after only 5 full cycles which took 1 hour. The extraction time has a fundamental importance for oil recovered from oil cake. The higher the extraction time the higher the amount of oil extracted. The number of cycles we applied was not sufficient to have better results. Slow and uniform heating at boiling point is necessary to get a steady evaporation rate. So slow heating rate increase the contact time of solvent and oilcake. Sufficient time is required to let the solute and solvent in contact which reach the equilibrium. Thus proper heating increases the extraction. It might be a cause of deviation of the result. The oilcake we used in the laboratory was collected many days ago and the oil content was also determined then. The oilcake was not preserved in air tied place. So the residual oil content decreased day by day for air contact. So it may remain a few amount of oil in the oilcake than the initial one.

The percentage of recovery of n-Hexane was also in a very low percentage. There might be some limitations which caused this result. The solvent lost during the process is mostly Page | 9

occurred when the extracted oil was collected from the system. A large amount of n-hexane was vaporized, some was attached on the inside wall of the apparatus, some was wet the cotton of the top of the condenser and a huge might be remained in the oil cake residue. These might be the prime reasons of low recovery. Of all solvents available hexane was chosen even though it is highly volatile as well as it is inherently combustible material & the installation comes under the explosives directorate. It is therefore, necessary to observe good management practices in the operation of solvent extraction plant. All those described above are possible causes for getting less percentage of solvent extraction. Though the percent of oil extracted & recovery of solvent is not so high, the objectives of the experiment are fulfilled.

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