Experiment 4

Solid-Liquid Extraction (Leaching)

1. Objective(s)

The students should be able to:

 Operate solid-liquid extraction experiment using Solid-Liquid Extraction Unit.

 Analyze the sample by using density measurement to obtain gram of oil extracted from the solid
per gram of solvent.
 Obtain the time when the solid-liquid extraction is nearly finish.

2. Introduction

Extraction is an important unit operation in many chemical industries. Extraction essentially is a

separation process where the raw materials undergo purification and isolation of a final useful product.
Without an efficient separation technology, raw materials would be in short supply, more expensive and
of a lower quality. In solid-liquid extraction process, one or more components from a solid phase (or
mixtures of phases) can be removed by using a liquid (solvent) to selectively dissolve the required
solute fraction.

Solid-liquid extraction can be defined as the removal of one or more components from a solid
phase (or a mixture of phases) by using a liquid to selectively dissolve the required solute fraction. A
complete extraction generally includes the following three steps:

 Contact of solid with liquid and selective dissolution of one or more components of the solid
phases.
 Separation of the resulting solution from the residual solid.
 Separation of the solute from the solvent in the extracted solution.

Solid-liquid extraction can be used either when the extracted component is required or to
recover the solid residue. The former is generally described as Leaching while the latter is more often
associated with purification such as washing of filter cakes.

The solvent feed (solvent stream, extractant etc.) is allowed to come into intimate contact with
the solids feed (solid stream, charge etc.). The resulting solution (solute and solvent) which leaves the
plant, is described as the Overflow (effluent stream etc.) whilst the residual solid (inerts etc.) together
with entrained solution make up the Underflow.

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 Although the Overflow is generally less dense than the Underflow and so might separate
naturally in that order, this is not a pre-requisite of this description and the terms are always applied in
the sense given here, irrespective of practical aspects of the separation.

The Solid-Liquid Extraction unit (Model BP 04) is designed to operate as a fixed-bed extractor
either in a batch or continuous mode of operation. Pure solvent vapour generated in the reboiler (B1)
rises through a packed column (K1) and is condensed in a vertical water-cooled condenser (W2) before
being cooled down in a product cooler (W4). The liquid solvent is then directed either to the collecting
vessel (B3) or through the extraction vessel (B2). A pre-heater (W3) is provided to allow for extraction
processes at different solvent temperature.

Solid to be extracted is contained inside a glass container with porous bed support. The
container is then placed in the extraction vessel (B2). The solvent and extracted solute (now in solution)
from the extraction vessel may be turned to the reboiler where the solvent is regenerated for further
extraction.

The components of solid-liquid extraction unit are as shown below:

 Reboiler (B1)
 Column (K1)
 Condenser (W2)
 Product cooler (W4)
 Receiver vessel (B3)
 Extraction vessel (B2)
 Pre-heater (W3)
6 L spherical evaporator vessel made of borosilicate glass.
Electrically Safety Handling Mantel (W1), 1700W with temperature
control.
DN 50x1000 mm column made of borosilicate glass.
Packings: Glass Raschig rings (8 mm x 8mm).
Vertical coil heat exchanger DN50 made of borosilicate glass.
Heat transfer area: 0.3 m2
Vertical coil heat exchanger made of borosilicate glass.
Heat transfer area: 0.03 m2
6 L spherical vessel made of borosilicate glass.
4 L cylindrical container made of borosilicate glass with porous
support for solid samples and quick closure unit.
250 W cartridge heater with temperature control.

A process flow diagram for the Solid-Liquid Extraction unit is as shown in the next page.

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Figure 1: The Solid-Liquid Extraction Unit (Model BP 04)

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3. Chemicals and Ancillary Equipment

a) Chemicals required:
Industrial grade Ethanol (5 – 6 L)
Crushed raw soybean (500 g)

b) Ancillary equipment/apparatus required:

Density meter
Measuring cylinder (100 mL)
Beaker (50 mL)
Test Tube (11 test tube per group)
Dropper
Glass rod

4. Operating Instruction

4.1 Safety Consideration

1. Inspect the equipment for chemical leakages or glass breakages. Refer to manufacturer for
replacement of any defective parts.
2. The plant should be kept well ventilated while in operation in order to avoid organic vapours
and fumes.
3. Check whether the solvent in tank is appropriately filled before commencement of a trial.
4. Sampling measurements ethanol need to be carried out quickly in order to avoid solvent
evaporation as ethanol is volatile.
5. Since flammable liquids are used, standard precautions to be taken in case of fire should be
studied before the experiment.
6. In case of any emergency, stop the ethanol flow pump and al the electrical switches.

4.2 General Start-up Procedure

1. Materials needed: Ethanol (solvent) and Crushed raw soybean (solids that containing soybean
oil as solute).
2. Ensure that all valves are initially closed. Open all vent valves V6, V7 and V9.
3. Charge the Reboiler B1 with ethanol as follows:
a) Measure and record the required amount of solvent in the reboiler.
b) Unscrew the charge port cap.
c) Carefully pour the solvent into the reboiler through the charge port.
d) Ensure the liquid level is above the vessel equator.
e) Screw back the charge port cap.
4. Ensure that all tubing are properly connected.

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5. Run the cooling water through the Product Cooler W4 and Condenser W2.
Note : Open the Cooling Water valve V13 and keep it open throughout the experiment. Open the
valve slowly to prevent a pressure surge to the cooling system.
6. Switch on the heating system for the reboiler as follows:
a) Initially close valve V12 to allow for total reflux.
b) Switch on the main power supply on the control panel.
c) Adjust the Temperature Controller TIC-101 setpoint to a few degrees above the boiling
point of the solvent. In case of ethanol, adjust to 80oC.
d) Switch on the power to Heater W1.
e) Observe the temperature rise in the reboiler.
f) Allow the system to reach steady state at total reflux.
Note : If the column starts to flood and liquid begins to accumulate above the Reflux Separator,
temporarily switch off the Heater W1 until column conditions are back to normal.
7. The equipment is now ready for experiment.

4.21 Charging of Fresh Solid

1. Weigh approximately 500g of the raw soybeans.

2. Charge the Extraction Vessel B2:
a) Ensure that the extraction vessel is drained of solvent.
b) Carefully remove the vessel cover and the solid container.
c) Discard any used solid in the container.
d) Fill in the container with the raw soybeans
e) Carefully place the container back into the extraction vessel.
f) Replace the extraction cover.
3. Check that the solvent feed line is properly connected to the extraction vessel.

4.22 Sampling Procedures

1. All samples should be collected in Sampling Vials with caps to avoid excessive evaporation of
solvent. The samples will be used for density measurement later.
2. Conduct effluent sampling as per following:
a) Place a sampling vial below valve V3.
b) Open valve V3 and collect approximately 50 mL of effluent in the sampling vial.
c) Close valve V3.

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4.23 Solvent Refill in the Reboiler

1. When the solvent level in the reboiler is low, refill as necessary:

a) Switch off the Heater W1 power.
b) Allow the solvent temperature in the reboiler to drop below boiling point and observe
until the boiling has stopped.
c) Open the charge port cap and quickly refill the reboiler to minimize escape of solvent
vapour. Immediately screw back the cap.
d) Switch on the Heater W1 power.

4.3 Experiment: Batch Extraction of Soybean Oil from Raw Soybean using Ethanol

1. Check that all valves are initially closed except vent valves V6, V7 and V9. Ensure that the
extraction vessel B2 is empty of solids.
2. Open valves V2, V5 and V12. Make sure valve V12 is fully open to obtain the maximum solvent
flow rate.
3. Allow the solvent to pass through the Product Cooler W4, Flow Indicator FI-301, Pre-heater
W3, Extraction Vessel B2 and back into Reboiler B1.
4. Monitor the solvent flow rate at the Flow Indicator FI-301. Once it is relatively constant, close
valve V12 to prevent any more solvent from entering the Extraction Vessel B2.
5. Charge fresh solid in the extraction vessel (see Section 4.2.1). Record the solid’s weight.
6. Close valve V2, V5 and open valve V12. When the solvent starts to enter the extraction vessel,
immediately start the timer.
7. Allow the solvent to fill the vessel until all solids are fully immersed in the solvent. Keep on
monitoring in the solvent flow rate FI-301. Record the average flow rate value.
8. Close valve V12 to prevent more solvent from entering the extraction vessel B2. Stop the timer
and record the filling time to determine the volume of solvent in the vessel B2.
9. Reset the timer. Let the extraction process to take place for 30 minutes. In the meantime, make
sure that vessel B3 is empty by opening valve V10 and draining all liquid. Close back valve
V10.
10. Temporarily switch off the Heater W1 power to avoid flooding in the column.
11. Refill the reboiler with solvent if necessary (see Section 4.2.3).
12. After 30 minutes, open valves V4 and V5. Let all the effluent flow into vessel B3. Leave for a
few minutes to allow for the effluent to completely drain from the solids.
13. Measure the volume of effluent collected in the vessel B3 by using a measuring cylinder.
14. Collect a 50 mL sample of the effluent for density measurement.
15. Record your data in the provided table.

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4.31 Calibration Curve: Density of Solution vs Gram Soybean Oil/Gram Ethanol

1. Obtain 11 test tubes; label the test tubes with A1 until A11. Total volume in each test tube is 10
ml.
2. Prepare the mixture of pure soybean oil and ethanol to each test tube according to volume
indicated by Table 1 (see Results)
3. Stir the mixture of solution (A1 until A11) with glass rod.
4. Obtain density reading for solution in each tube using density meter.
5. Record the density reading for each tube tests at Table 1 (see Results).
6. Calculate weight/weight (w/w) soybean oil/ethanol and record at each of density reading at
Table 1 (see Results).
Note : Density of soybean oil @25 oC is 0.917g/mL; density of ethanol @25oC is 0.789 g/mL.
7. By using a graph paper, plot the graph of Density of solution vs g soybean oil/g ethanol.

4.4 General Shut-Down Procedure

1. Open all vent valves V6, V7 and V9.

2. Place a container under valve V10. Open valves V4, V5, V8 and V10 to drain all liquid from the
equipment.
3. Shut-down the reboiler as follows:
a) Let the cooling water run. Switch off the Heater W1.
b) Close valve V12 for total reflux.
c) Allow the solvent in the reboiler to cool down to room temperature.
d) Empty the reboiler B1 by draining all liquid through valve V1.
4. Shut-down the cooling water flows as follows:
a) Let the cooling water run until the solvent in the reboiler has cooled down to room
temperature.
b) Close valve V13.
5. Clean the extraction vessel B2 as follows:
a) Ensure that the vessel is drained of solvent.
b) Carefully remove the vessel cover and the solids container.
c) Discard the used solid and clean the container.
d) Carefully place the container back into the extraction vessel.
e) Replace the extraction vessel cover.
Note : Always clean the solid container thoroughly especially the porous support, to prevent
molds from growing among the pores.

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5. Results (Please attach this part in your report)

 Discuss all your results. Your discussion should covers, but not limited to, on the factors that
affected efficiency of leaching process, the choice of solvent or others solvent available and
function and performance of contact time factors in this experiment.
 By using provided formula, please complete the following table and construct a calibration curve.

𝒈 𝒔𝒐𝒚𝒃𝒆𝒂𝒏 𝒐𝒊𝒍 𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑷𝒖𝒓𝒆 𝑺𝒐𝒚𝒃𝒆𝒂𝒏 𝑶𝒊𝒍 𝑫𝒆𝒏𝒔𝒊𝒕𝒚 𝒐𝒇 𝑺𝒐𝒚𝒃𝒆𝒂𝒏 𝑶𝒊𝒍

𝑹𝒂𝒕𝒊𝒐 = ×
𝒈 𝒆𝒕𝒉𝒂𝒏𝒐𝒍 𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑬𝒕𝒉𝒂𝒏𝒐𝒍 𝑫𝒆𝒏𝒔𝒊𝒕𝒚 𝒐𝒇 𝑬𝒉𝒂𝒏𝒐𝒍

Table 1
Test Volume of Pure Volume of Ethanol Density g soybean oil/
tube Soybean Oil (mL) (mL) (g/mL) g ethanol
A1 0 10
A2 1 9
A3 2 8
A4 3 7
A5 4 6
A6 5 5
A7 6 4
A8 7 3
A9 8 2
A10 9 1
A11 10 0

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 By referring to a calibration curve, determine solute composition and amount of solute (Table 2).
Table 2

Mass of soybean : ___________kg

Solvent Flow Rate : 60 mL/min
Solvent Feed Temperature : _________ oC

Solvent Effluent
Contact

Solute Amount of
Time

solute
Filling

Density composition
(min)
Time

Volume
Volume (L) (g/mL) (g soybean oil/g (g)
(L)
ethanol)
30
min

Useful formula:

𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑺𝒐𝒍𝒗𝒆𝒏𝒕 = 𝑺𝒐𝒍𝒗𝒆𝒏𝒕 𝑭𝒍𝒐𝒘 𝒓𝒂𝒕𝒆 × 𝑺𝒐𝒍𝒗𝒆𝒏𝒕 𝑭𝒊𝒍𝒍𝒊𝒏𝒈 𝑻𝒊𝒎𝒆

𝑨𝒎𝒐𝒖𝒏𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆 = 𝑺𝒐𝒍𝒖𝒕𝒆 𝒄𝒐𝒎𝒑𝒐𝒔𝒊𝒕𝒊𝒐𝒏 × 𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕 × 𝑫𝒆𝒏𝒔𝒊𝒕𝒚 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕