Unit Operation II Lab Extraction

1. Introduction

For thousands of years, for the treatment of illnesses, many a medicine was used
throughout human history. That said, the effectiveness of such medicines was lower than
it is now, mainly because the bioactive natural product amount was quite low compared
to that of now. To create medicines and drugs with high efficacy, isolating a product
needed and utilizing methods of extraction is quite crucial. To separate substances from
each other, a method called extraction is utilized. There are quite a few methods of
extraction, such as the distillation method, solvent extraction, sublimation, and pressing.
The most widely utilized method is solvent extraction, which is also the method used in
our case. Though it might sound somewhat complicated in theory, it is quite easy to
calculate the necessary values from the aforementioned extraction method. The method is
one of the most preferred as it is fairly easy, and 4 versatile to use. Even in our everyday
life, solid – liquid extraction method is used by us. That is, boiling tea leaves in hot water
results in the extraction of products such as theobromine, caffeine, and tannins into the
water out of the leaves. Other applications of the extraction method are extraction of
acetic acid, extraction of phenol from wastewater, neutralization of acids and bases, and
in fields such as biotechnology, hydrometallurgy, and phytoprocesses.

2. Theory

From this point onwards, mainly liquid – liquid extraction is going to be discussed.
Liquid – liquid extraction, alternatively known as partitioning and solvent extraction, is a
process that involves two liquids immiscible in each other. Generally, one liquid is of
organic nature, whereas the other is aqueous, which is chosen so that separate compounds
are created. Via contacting and mixing of two liquids, the solute is transferred from one
solvent to the other one. Following this is a phase separation, which involves two liquids
becoming separate. The process involves two solutions, one feed contains the solute, and
another is solvent. Some considerations must be taken into account when selecting the
appropriate solvent. Some factors are solubility, safety, selectivity, and cost. It is known
that if the solvent and solute’s polarity values are similar, the process will happen
optimally. Temperature influences the solubility, and in turn, the extraction process.

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Higher temperature values mean a rise in diffusion and solubility. However, caution must
be exercised so that the temperature is not too high, as it might result in impurities and
decomposition. Another thing to consider is the scale of the operation. A separatory
funnel is utilized for the batch single –stage extraction in smaller scale labs, whereas in
larger scale labs, multistage 5 countercurrent continuous processes are utilized to achieve
desired purity and extraction level. The procedure used in our experiment is the simplest
form of bath single – stage extraction. The solvent and the feed solutions are in direct
contact, and the solute, ethanol, is transferred to water due to the difference in solubility
of sunflower oil and water.

3. Objectives of the experiment

• Liquid/liquid extraction
• Efficiency of extraction; mass balance; solid/liquid extraction
• Three-component system exercises (extraction of oil from soybean laminate using
hexane, for example).

4. Reasons for using extraction:

1. Distillation is impractical for separation.

2. Zeotropes must be broken.

3. Distillation requires prohibitively high energy costs.
4. A sophisticated distillation procedure is necessary.
5. The substance is susceptible to heat.

6. The substance is not volatile.

5. Experimental Technique
Apparatus The unit utilized to conduct the experiment was unit CE 620. The unit
comprised five tanks, two pumps, an extraction column, valves, round – bottomed flask,
and the switch panel. The tanks were utilized to hold raffinate, extract, feed, distillate,
and solvent supplies. The pumps were utilized to supply the feed and solvent streams.
Some pictures regarding the equipment, and their names are as follows:

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Figure (1.1):liquid-liquid extraction

Figure (1.2):solid-liquid extraction

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6. Health and Safety Precautions

It goes without saying that all experiment participants must abide by the laboratory rules
throughout the process. Some must – follow rules are as follows:

 As the blending of the feed is done via a hand agitator, it should be treated
meticulously as the shaft can cause harm.
 As the material of the flash and extraction column is glass, great care must be
exercised while interacting with the aforementioned tools.
 Contact with ethanol is best avoided, and in case of failing to do so, the contact
zone is to be cleaned via distilled water.
 As the device has an electric cabinet, pouring any liquid substances on it as well
as high humidity levels must be avoided.
 As ethanol is easily flammable and can spread quite fast, no potential ignition
source should be allowed inside the room, and it should be made sure that the
ventilation system works properly.

6. Procedure:

1) As the first step, a water supply of 5 liters is supplied to the solvent stream. Then,
ethanol of 0.5 kg mass is supplied to the feed stream. Afterward, the third component –
sunflower oil is fed to the feed stream. An agitator is utilized to achieve the mixing of
sunflower oil and ethanol.

2) The lids are covered to avert the possibility of ethanol vaporization.

3) The modification of three – way valves is done to allow the system to operate in batch
mode. The valves V30 and V4 are unlocked to allow the feed to leave its tank, whereas the
drainage and V3 valves remain locked beforehand.

4) The unit’s electric plug is then joined to the electricity, and the main switch is turned
on. Pump 1 is switched on to supply water to the column.

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5) The equilibrium point is denoted in the middle part of the column. If the water supply
is to reach that level, pump 1 is switched off.

6) Simultaneously, pump 2 is switched on to supply oil feed to the column. When the
sunflower oil is at around the top, valve V30 is deactivated.

7) To control the phase boundary, and achieve its stability at the middle point, valves V1
and V2 are used. Once more, pump 1 is switched on to supply water to the column.

8) The equilibrium point is achieved after around 20 minutes. The 1st sample is also
procured at this point. The thermometer is utilized to note the temperature value, and a
scale is used to learn the mass value. The density value will be found by using the learned
mass value, and the volume value denoted on the flask.

9) At time intervals, another sample is obtained. The supplys repeated until there are little
to no changes to be observed in density and temperature values.

10) After the acquisition of the final – 8 th sample, valve V30 is switched on, whereas V1
and V4 are deactivated. In order to achieve the supplying of water to the solvent tank, V3
is activated. As soon as the pumping of water is completed, V3 is deactivated. 11

11) Finally, the pumps are switched off, and the main switch is turned off. The unit then
is unplugged from the electricity source.