ABSTRACT

The experiment Solid-liquid extraction was carried out in a way, where Peanut oil (PO) was
extracted from crushed peanuts by using the continuous overflow extraction through a fixed
solid bed method. N-hexane was used as the solvent to extract the oil. Calibration was done
in order to determine the solute composition. Density and solute composition of affluent and
reboiler were measured at different time intervals in order to study the effect of time on solute
composition. In the end the total amount of solvent extracted was calculated and the effect of
different components like temperature and solvent flow rate on the overall extraction were
studied

INTRODUCTION
Separation processes by extraction are a fundamental part of almost every chemical process.
Separations start with the extraction of raw materials and continue to the purification and
isolation of the final product. Without an efficient separation technology, raw materials would
be in short supply, more expensive and of a lower quality. Solid-liquid extraction allows
soluble components to be removed from solids using a solvent.
An everyday example is the preparation of coffee. Water (solvent) is used to remove the
coffee flavours (transition component) from the coffee powder (extraction material,
consisting of solid carrier phase and transition component). Ideally, this results in drinkable
coffee (solvent with dissolved flavours), with the completely depleted coffee grounds (solid
carrier phase) remaining in the coffee filter.
To achieve the fastest and most complete solid extraction possible, the solvent must be
provided with large exchange surfaces and short diffusion paths. This can be done by
pulverising the solid to be extracted. The extraction material can also take the form of a fixed
bed with the solvent flowing through it.

Figure 1: Schematic of solid-liquid extraction process

The experiment conducted used the method of continuous overflow extraction through a
fixed solid bed. Firstly the experiment consisted of the peanuts being crushed. The peanuts
were then placed in the affluent cylinder of the operating machine. The solvent used was N2

hexane. N-hexane was used as it has low heat of vaporisation. The n-hexane is filled in the
reboiler. The temperature of the reboiler is set and the rate of the feed flow rate is also set. As
the solvent boils it goes up and passes through the solid bed. After passing through the solid
bed it is condensed again and ready for use for extraction of oil from the crushed peanuts in
the affluent cylinder. After the solvent flows from the affluent cylinder, it has already
extracted the peanut oil. After that the hexane is removed and the oil is collected. This
method is therefore known as chemical solvent extraction and it is very profitable as the oil
yield using this method is maximum. This method enables a high capacity, low power
consumption, low maintenance and high extract efficiency.

APPARATUS:
The SOLTEQ Solid-Liquid Extraction Unit (Model: BP 40) is designed to demonstrate the
extraction process, where it operates as a fixed-bed extractor and components can be
selectively extracted from solids with the use of a suitable solvent. The unit which can
operate in batch mode or continues mode consists of a pre-heater, an extraction vessel, an
evaporator, condenser, cooler, a packed column and a receiver vessel.
Unit specifications:
1. Re-boiler (B1)
7.0L spherical evaporator vessel made of stainless steel
Electrical safety heating mantle (W1), 2 kW with temperature and level switch.
2. Column (K1)
DN50 x 1000 mm column made of borosilicate glass
Packing: glass Raschig rings (8mm x 8mm)
3. Condenser (W2)
Vertical coil heat exchanger DN50 made of stainless steel
Heat transfer area: 0.3 m2
4. Product Cooler (W4)
Vertical coil heat exchanger made of stainless steel
Heat transfer area: 0.03 m2
5. Receiver Vessel (B3)
5-L spherical vessel made of stainless steel
6. Extraction Vessel (B2)
Cylindrical vessel made of borosilicate glass with 4L solid sample container made of
stainless steel with porous support
7. Pre-Heater (W3)
150 W cartridge heater with temperature control
8. Instruments and Controls
3 temperature measurement points (TI-101, TI-102, TI-103)
2 temperature controller (TIC-101, TIC-103)
1 flow rate measuring point (FI-301)
1 pressure indicator (PI-201)

1 level controller (LIC-101)

9. Framework
Stainless steel tube with clamps
10. Operating Conditions
Allowable pressure: -1 to 3 bar in tube -1 to 1 bar in shell
Allowable temperature: 180C in tube 150C in shell
11. General Requirements
Electrical: 230VAC / 1-phase / 50Hz / 10A
Water supply: laboratory water
Analytical instruments: density bottles
Sample solids: e.g. crushed peanuts
Solvent: e.g. n-hexane
12. Overall Dimensions
Height: 1.730 m
Width: 1.216 m
Depth: 0.608 m

Figure 2: Process flow diagram of SOLTEQ Solid-Liquid Extraction Unit (Model: BP40)

EXPERIMENT PROCEDURE:
General Start-Up Procedures:
The following was performed before starting the experiment:
1. All valves were initially closed. All vent valves V6, V7 and V9 were opened.
2. The re-boiler B1was charged with n-hexane solvent.
3. The cooling water was run through the product cooler W4 and condenser W2.
4. The heating system for the re-boiler was switched on as follows:
a) Valve V12 was closed to allow for total reflux.
b) The main power supply was switched on the control panel.
c) The temperature controller TIC-101 set-point was adjusted to a few degrees above the
boiling point of the solvent. In the case of n-hexane, it was adjusted to 70C.
d) The power for heater W1was switched on.
e) The temperature rise in the re-boiler was observed.
f) The system reached steady state at total reflux.
Calibration of Solute Composition
Chemicals needed:
Peanut oil (solute)
N-Hexane (solvent)
1. Mixtures of peanut oil and n-hexane were prepared in different compositions, from 0.0 to
1.0 g oil / g solvent.
2. The recommended calibration volumes in the sample table in Appendix D were used.
With a basis of 100 g solvent.
3. For example (0.1 g oil / g solvent):
a) 100 g of n-hexane solvent was weighed in a beaker.
b) Then, 10 g of peanut oil (PO) was weighed in another beaker.
c) The oil was added into the solvent to form a homogenous solution.
4. The density of the calibrated solution was measured.
5. A calibration curve of density vs. solute composition was plotted.

EXTRACTION PROCEDURE:
Continuous Downward Extraction of Peanut Oil (PO) From Peanuts Using n-Hexane

1. The general start-up procedures were performed. It was ensured that all valves were
initially closed except the vent valves V6, V7 and V9. It was then ensured that the
extraction vessel B2 is empty of solids.
2. Valves V2, V5 and V12 were opened. It was made sure that valve V12 was fully opened
to obtain the maximum solvent flow rate.
3. The solvent was allowed to pass through the product cooler W4, flow indicator FI-301,
pre-heater W3, extraction vessel B2 and back into the reboiler B1.
4. The solvent flow rate was monitored at the flow indicator FI-301. Once it was relatively
constant, the value was recorded.
5. Valve V12 was closed to prevent any more solvent from entering the extraction vessel B2.
Valves V2 and V5 were closed.
6. Fresh solid was charged in the extraction vessel. The solids weight was recorded.
7. The initial reboiler temperature was recorded. A sample was taken from the reboiler and
its density was measured.
8. Valves V2 & V5 were first opened and valve V12 was then opened to start the extraction.
The flow of solvent through the solids was observed in the extraction vessel B2.
9. Once the effluent started flowing into the reboiler B1 through valve V2, the timer was
started and the first sample of the effluent at time t = 0 was collected. The density was
determined.
10. The reboiler contents and effluent were continued to be sampled every 5 minutes. Each
samples density was determined. Also the reboiler temperature at the specified time
intervals were recorded.
11. The experiment was stopped when the effluent density was determined in step 11 and
showed no significant solute composition (nearly pure solvent).
12. The heater W1 power was switched off and the reboiler was drained. The reboiler was
refilled with fresh solvent.

Results:

4.1.1 Continuous downward extraction

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Mass of solids: 1 kg.

Solvent flow rate: 45 mL/min.
Solvent feed temperature: 32C
Total volume of Hexane: 50 mL
Table1: The reboiler and effluent content at specific time
Time
(min)
0
5
10
15
20
25
30
35

Reboiler Contents
Density
Solute
(g/mL)
Composition
0.6926
0.4847
0.5900
0.4747
0.6296
0.4920
0.6130
0.4896
0.6090
0.5080
0.6212
0.5214
0.6214
0.5214
0.6138
0.5154

Effluent
Density
(g/mL)
0.6694
0.6532
0.6502
0.6390
0.5902
0.5722
0.5704
0.5770

Solute
Composition
0.5153
0.5254
0.5080
0.5104
0.4920
0.4786
0.4786
0.4846

4.1.2 Calibration of solute composition

Basis: 50g of n-Hexane

Table 2: Solute composition and density of hexane with different mass

Mass of peanut oil added
(g)
10
20
30
40
50

Solute composition
(g oil/g solvent)
0.167
0.286
0.375
0.444
0.500

Density
(g/mL)
0.632
0.729
0.733
0.750
0.770

4.2 Graph

4.2.1 Graph of reboiler content composition versus time

Graph of reboiler content composition vs time

Reboiler content composition

(g oil/ g solvent)

0.53
0.52
0.51
0.5
0.49
0.48
0.47
0.46
0.45

10 15 20 25 30 35 40

Time (min)

4.2.2 Graph of effluent composition versus time.

Graph of effluent composition vs time

0.53
0.52
0.51
0.5

Effluent composition (g oil/g solvent) 0.49

0.48
0.47
0.46
0.45

5 10 15 20 25 30 35 40

Time (min)

4.2.3 Graph of calibration of solute composition

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Graph of Density against Solute Composition

0.9
0.8
0.7
0.6
0.5
Density (g/mL) 0.4
0.3
0.2
0.1
0
0.15

0.2

0.25

0.3

0.35

0.4

0.45

0.5

0.55

Solute composition (g oil/g solvent)

4.3 Sample of calculations

1) Reboiler content composition
mass of hexane (reboiler)
= mass of hexane (reboiler + effluent)

31.48
31.48+ 33.47 = 0.4847

2) Density
mass of hexane (reboiler)
= volume of hexane (reboiler)

31.48 g
= 50 mL = 0.6296 g/mL

3) Total amount of extracted solute

= Area under a graph (effluent composition vs time) x solvent flowrate
= 17.46475x 45 mL/min
= 785.914

DISCUSSION:
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The method used was a continuous downward extraction. N-Hexane was used as the solvent
to extract the solid. The Peanuts used in the experiment were crushed before being used for
the extraction purpose as crushed peanuts have larger surface area and allow for more contact
with hexane. The flowrate of the solvent was 45mL/min. The temperature recorded was 32
of the solvent feed.

The graph of reboiler composition vs. time shows irregularities for a continuous process. The
graph in theory should be linear or should show an increasing trend till a certain time limit as
the solute is being extracted but there are irregularities at the 5 and 15 min mark. The highest
solute composition is 0.5214 g oil/g solvent. The graph also shows that the reboiler content
starts decreasing after the 30 min. The graph of affluent composition vs. time should
complement the reboiler content vs. time and it does. The solute composition should decrease
with time here and it does but there are irregularities as for a continuous process the graph
should be in a continuous trend. The highest solute composition of the effluent is 0.5254 g
oil/g. The graph for density vs. solute composition shoes that higher the density more the
solute composition.
From the graphs obtained, it generally shows that as the time increases mores oil is extracted.
The initial high rate of extraction might be caused by the fast solubility of the oil that is
present at the solid surface and higher driving force of the mass transfer by the low oil
concentration in the fresh solvent. The irregularities were caused by the fault in the operating
machine as there was leakage in the affluent container. This leaked solvent might have
contained the extracted solute which in turn could prove why the readings did not follow the
general trend. Moreover there was also leakage from the reboiler which in turn explains the
irregularities from the reboiler composition vs. time graph.

These graph also show that time is a very important factor for this experiment as with more
time, higher amount of peanut oil would have been extracted. The temperature used for this
experiment was high in order to lower the solvent and extract viscosities and increasing the
extract solubility in the solvent.
Conclusion:
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The basic aim of the experiment was achieved which was the extraction of solid by a liquid.
Due to the faultiness of the operating machine, there were irregularities in the results which
showed deviation from a continuous process. In order to improve the experiment, the
equipment being used should be ensured to operate properly. The weight of n-hexane should
be measured quickly as n-hexane is volatile and evaporates quickly.

REFERENCES

1. Joe Givens, Robert Jordheim and George Anderson, tests performed at a 750 ton per
day soybean extraction plant in Dawson, Minnesota, March 10, 1977.
2. Engineers S.B.o.C. 1998. SBP Handbook of Oil Seeds, Oils, Fats and Derivatives.
SBP Consultant & Engineers Pvt. Ltd., New Delhi.
3. Williams, M.A. Obtaining oils and fats from source materials. Baileys Industrial Oil
and Fat Products, Fifth Edition, pp. 106-138 (John Wiley & Sons, New York) (1996).

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