Solid-Liquid extraction unit (Model: BP 40)

The SOLTEQ solid-liquid extraction unit (Model: BP 40) 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 wither 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 returned to the reboiler where the solvent is regenerated for
further extraction.

General Operating Procedures

The procedures outlined below will serve as a general guideline for operating the equipment and
running the experiment.

1.1. Calibration of Solute Composition

Chemicals needed: Peanut oil (solute)
n-Hexane (solvent)
1. Prepare mixtures of peanut oil and n-hexane in different compositions, vary from 0.0 to 1.0 g
oil / g solvent.

2. Use the recommended calibration volumes in the sample table in Appendix D. Use a basis of
100 g solvent.

3. For example (0.1 g oil / g solvent):

a) Weigh 100 g of n-hexane solvent in a beaker.

b) Then, weigh 10 g of peanut oil (PO) in another beaker.

c) Add the oil into the solvent to form a homogenous solution.

 Note: Do this step quickly to avoid solvent evaporation since n-hexane is volatile.
4. Measure the density of the calibrated solution.

5. Plot a calibration curve of density vs. solute composition.

6. Use that calibration curve for further experiments.

1.2. Sampling Procedures

All samples should be collected in sampling vials with caps to avoid excessive evaporation of the
solvent. The samples will be used for density measurements later.

1. Effluent sampling

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.
2. Reboiler sampling
Note: Sample taken from the reboiler will be at the boiling point of the solvent and must be
handled with extra care.
a) Place a sampling vial below valve V1.
b) Open valve V1 and collect approximately 50 ml of reboiler content in the sampling vial.
Quickly close valve V1.
c) Cool the sample by immersing the vial in cold water.

3. Distillate sampling
a) Place a sampling vial below valve V11.
b) Open valve V11 and collect approximately 50 ml of distillate in the sampling vial.
c) Close valve V11.

1.3. Charging of Fresh Solid

Fill the extraction vessel B2 with fresh solid whenever it is required in the experiment.
 1. Screen some crushed peanuts to obtain solids of sizes between 2 mm and 4 mm. Weigh
approx. 1000 g of the peanuts.

2. Charge the extraction vessel B2:

a) Ensure that the extraction vessel is drained of solvent.

b) Carefully remove the vessel cover and the solids container.

c) Discard any used solid in the container.

d) Fill the container with the screened peanuts.

e) Carefully place the container back into the extraction vessel.

f) Replace the extraction vessel cover.

3. Check that the solvent feed line is properly connected to the extraction vessel.

1.4. Solvent Refill in the Reboiler

When the solvent level in the reboiler is low, refill as necessary.
1. Switch off the heater W1 power.

2. Allow the solvent temperature in the reboiler to drop below boiling point and observe until the
boiling has stopped.

3. Open reboiler cap quickly refill the reboiler to minimize escape of solvent vapor. Immediately
close valve reboiler cap.

4. Switch on the heater W1 power.

Cautions: DO NOT open reboiler cap while the temperature in the reboiler is still boiling.

1.5. General Shut-Down Procedures

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 solids container thoroughly, especially the porous support, to prevent
molds from growing among the pores.
Experiment 1: Continuous Downward Extraction of Peanut Oil (PO) From Peanuts Using
n-Hexane

OBJECTIVE:
To investigate the effect of solvent flow rate on the extraction of Peanut oil (PO) from crushed
Peanuts by continuous downward extraction through a fixed solid bed.

PROCEDURES:
1. Perform the general start-up procedures (section 1.1). Check that all valves are initially closed
except the 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,
record the value.

5. Close valve V12 to prevent any more solvent from entering the extraction vessel B2. Close
valves V2 and V5.

6. Charge fresh solid in the extraction vessel (section 1.3). Record the solids weight.

7. Record the initial reboiler temperature. Then take a sample from the reboiler and measure its
density.

8. To start the extraction, open valves V2 & V5 and open valve V12. Observe the flow of solvent
through the solids in the extraction vessel B2.

9. Once the effluent has started flowing into the reboiler B1 through valve V2, start the timer and
collect the first sample of the effluent at time t = 0. Determine the density.

10. Continue sampling the reboiler contents and effluent every 5 minutes. Determine each
samples density. Also record the reboiler temperature at the specified time intervals.
11. Stop the experiment when the effluent density determined in step 11 shows no significant
solute composition (nearly pure solvent).

12. Switch off the heater W1 power and drain the reboiler. Refill the reboiler with fresh solvent
(section 1.4).

ANALYSIS AND DISCUSSIONS:

1. Data collection. For different solvent flow rates, use a new table.

a) Enter the mass of solids and solvent flow rate for every set of experiment.

b) At the specific time intervals, record the reboiler temperature and each samples density.

c) Obtain the solute composition from the calibration curve (section 1.1).

2. For every set of experiment (different solvent flow rate):

a) Plot a graph of reboiler content composition vs. time.

b) Plot a graph of effluent composition vs. time.

c) Estimate the total amount of extracted solute.

Note: To find the total amount of extracted solute, calculate the area below the graph of effluent
composition vs. time, then multiply the area with the solvent flow rate.