Liquid Liquid Extraction Unit

SOLTEQ
EQUIPMENT FOR ENGINEERING EDUCATION & RESEARCH
EXPERIMENTAL MANUAL
EXCESS FEED
MATERIAL
RECOVERY
SYSTEM
MODEL: BP533-CPP
SOLUTION ENGINEERING SDN. BHD.

NO.3, JALAN TPK 2/4, TAMAN PERINDUSTRIAN KINRARA,
47100 PUCHONG, SELANGOR DARUL EHSAN, MALAYSIA.
TEL: 603-80758000 FAX: 603-80755784
E-MAIL: [email protected]
WEBSITE: www.solution.com.my
274-0515-BP(4)
TABLE OF CONTENTS
LIST OF FIGURES...i
1.0
INTRODUCTION.................................................................................................................. 1
2.0
GENERAL DESCRIPTION .................................................................................................. 3

2.1
2.2
2.3
2.4
Description and Assembly....................................................................................... 3

Valves and Instruments List .................................................................................... 5
Experiment Capabilities .......................................................................................... 6
General Requirements6
3.0
SUMMARY OF THEORY ..................................................................................................... 7
4.0
OPERATING PROCEDURES............................................................................................ 10
4.1
4.2
4.3
General Start-Up Procedure ................................................................................. 10

General Shut-Down Procedure..............................................................................11
Cleaning Procedure .11
5.0
OPERATING PROCEDURES
5.1
Experiment 1: Extraction of Acetone From Water Using Toluene..............12
5.2
Experiment 2: Recovery of Solvent...14
6.0
REFERENCES................................................................................................................... 15
APPENDIX A SAMPLE TABLE FOR EXPERIMENT

APPENDIX B STEP BY STEP CALCULATION GUIDE
APPENDIX C CALIBRATION PROCEDURES FOR LIQUID-LIQUID
EXPERIMENT
APPENDIX D SAMPLE TABLES FOR APPENDIX C.1
APPENDIX E SAMPLE TABLE FOR APPENDIX C.2
APPENDIX F TRIANGULAR PLOT FOR TERNARY DIAGRAM
APPENDIX G PHYSICAL PROPERTIES OF COMPONENTS
APPENDIX H TYPICAL CALIBRATION DATA
APPENDIX I SAMPLE EXPERIMENT RESULTS
EXTRACTION
SOLTEQ CHEMICAL PROCESS PILOT PLANT (EXCESS FEED MATERIAL RECOVERY SYSTEM) (Model: BP533-CPP)
List of Figures
Page
Figure 1
Process Flow Diagram for the Liquid-Liquid Extraction Unit
Figure 2
Flow of Streams and Components in a Liquid-Liquid Extraction System
Figure 3
A Typical 3-Component System Representation on an Equilateral

Triangular Diagram
Figure 4
Operating Lines and Tie Lines Constructions for Determination of

Extraction Efficiency
1.0
INTRODUCTION
The Excess Feed Material Recovery System of the SOLTEQ Chemical Process Pilot
Plant (Model: BP533-CPP) can be used to demonstrate the efficiency of separation and
recovery of recyclable materials. The apparatus requires a cold water, hot liquid from heat
exchanger system, and a triple phase electrical outlet to enable a series of simple
measurements to be made by students needing an introduction to excess feed material
recovery design and operation. This experiment allows the student to understand some
important things in this system which are:
Mass and energy balances
Concept in separation process mainly in liquid-liquid extraction
Liquid sampling on the bottom of extraction column to determine the practical
separation behavior of the particular mixture.
This experiment consists of two important equipments which are extraction column and
solvent recovery column. Two flowrate transmitter are installed in both inlet of extraction
column (top and bottom column) and valves are incorporated in both inlet to regulate the
flow. On the other hand, one temperature measuring device are installed in the outlet of
solvent recovery column.
The process flow diagram for the excess feed material recovery system is given in Figure
1.
EXCESS FEED MATERIAL RECOVERY SYSTEM

V-113
Solvent Tank
Stainless Steel 304

0.290 m (D) x 0.400 m (H)
Approx. 25-L
V-114
Feed Tank
Stainless Steel 304

0.290 m (D) x 0.400 m (H)
Approx. 25-L
V-115
Settling Tank
Stainless Steel 304

0.400 m (D) x 0.560 m (H)
Approx. 70-L
V-116
Raffinate Tank
Stainless Steel 304

0.290 m (D) x 0.400 m (H)
Approx. 25-L
V-117
Intermediate Storage Tank
Stainless Steel 304
0.290 m (D) x 0.400 m (H)
Approx. 25-L
P-113
Solvent Pump
SS316 Metering Pump

Power: 0.12 kW
Capacity: 42LPH @ 40m head
P-114
Feed Pump
P-115
Product Pump
SS316 Metering Pump

Power: 0.12kW
Capacity: 42LPH @ 40m head
SS304 Vertical Centrifugal Pump

Power: 0.37kW
Capacity: 10LPM @ 35m head
P-117
Transfer Pump
SS304 Vertical Centrifugal Pump

Power: 0.37kW
Capacity: 10LPM @ 35m head
E-407
Reboiler 2
E-408
Condenser 3
20-L vessel, horizontal

Material: SS304
Electrical heater: 2 x 2 kW
Coil Heat Exchanger

Material: SS304
Area: approx. 0.5 m2
T-501
Extraction Column
Packed column; SS304

Packing: Random packing
(Pall ring, Raschig ring)
0.080 m (D) x 2.500 m (H)
T-502
Solvent Recovery Column
Packed column; SS304
Packing: Random packing
(Pall ring, Raschig ring)
0.080 m (D) x 1.600 m (H)
Vent
HV 620
HV 623
E-408
HV 616
TT
FI
305
114
SG
HEAT EXCHANGER
SYSTEM
TI
114
V-114
V-115
HV 619
LSL
TIC
TT
112 112
HV 612
S
T-502
FT
SV 05
312
Drain/
Sampling
TIC
HV 608
112
HV 604
HV 624
Drain
N8
DN32
114
HV 614
HV 611
FS
Drain/
Sampling
302
HV 606
HV 605
P-114
Drain/
Sampling
Drain/ HV 609
Sampling
HV 622
P-115
HV 610
TIC
113
TT
113
Vent
LS
116
PWR
1
HV 621
E-407
HV 613
T-501
SG
Drain/
Sampling
V-113
LSL
V-116
113
FT
SG
SG
V-117
311
Drain/
Sampling
LSL
HV 601
HV 602
P-113
117
HV 603
HV 607
Drain/
Sampling
Drain/
Sampling
HV 615
Drain/
Sampling
Figure 1: Process flow diagram for the excess feed material recovery system.
C.W. Supply
Drain
HV 617
HV 618
P-117
HV 619
2.0
GENERAL DESCRIPTION
2.1
Description and Assembly

Before operating the excess feed material recovery system, users must familiarize
themselves with all the components of the unit. Please refer to Figure 1 to understand the
process.
Solvent Tank (V-113)
Material : SS 304
Capacity: approx. 25-L
Dimensions: 0.290m (D) x 0.400m (H)
Feed Tank (V-114)
Material: SS 304
Settling Tank (V-115)
Material: SS 304
Raffinate Tank (V-116)
Material: SS 304
Intermediate Storage Tank (V-117)
Material: SS 304
Solvent Pump (P-113)
Material: SS 316
Type: Metering pump
Capacity: 42 LPH @ 40m head
Rating: 0.12 kW
Feed Pump (P-114)
Material: SS 316
Type: Metering pump
Rating: 0.12 kW
Product Pump (P-115)

Material: SS 304
Type: Vertical Centrifugal pump
Rating: 0.37 kW
Transfer Pump (P-117)
Material: SS 304
Type: Vertical Centrifugal pump
Capacity: 10 LPM @ 35m head
Rating: 0.37 kW
Reboiler 2 (E-407)
Material: SS 304
Capacity: 20 L
Electrical Heater: 2 x 2 kW
Condenser 3 (E-408)
Type: Coil Heat Exchanger
Material: SS 304
Area: approx 0.5 m2
Extraction Column (T-501)
Material: SS 304
Type: Packed Column
Packing: Raschig ring
Dimension: 0.080 m (D) x 2.500 m (H)
Solvent Recovery Column (T-502)
Material: SS 304
Type: Packed Column
Packing: Raschig ring
Dimension: 0.080 m (D) x 2.500 m (H)
Instrumentations
Temperature measurement and control (TT-112-TT-114 and TI-114)
Flow measurement (FI-305, FT-311 and FT-312)
Level switch (LSL-113 - LSL-117)
Please refer to the manufacturers manual for further details on the component
specifications, installation and operation, safety requirements and servicing.
2.2
Valves and Instruments List

Valves list:
Tag
HV 601
HV 602
HV 603
HV 604
HV 605
HV 606
HV 607
HV 608
HV 609
HV 610
HV 611
HV 612
HV 613
HV 614
HV 615
HV 616
HV 617
HV 618
HV 619
HV 620
Location
V-113 drain valve
V-113 outlet valve to pump, P-113
T-501 (bottom) inlet valve
V-114 drain valve
V-114 outlet valve to pump, P-114
T-501 (top) inlet valve
T-501 (bottom) drain valve
T-501 (top) drain valve
V-115 drain valve
E-407 inlet valve
V-115 inlet valve from HEX
V-115 cooling water drain valve
E-407 drain valve
E-408 sampling/drain valve
V-116 drain valve
E-408 cooling water outlet valve
V-117 outlet valve
V-117 outlet valve to P-117
P-117 outlet valve to V-113
P-117 outlet valve
Instruments list:
Tag
TT-112
TT-113
TT-114
TI-114
FI-305
FT-311
FT-312
LSL-113
LSL-114
LSL-115
LSL-116
LSL-117
Description
V-112 hot water temperature
E-407 temperature
T-502 top column temperature
V-115 cooling water drain
temperature
E-408 cooling water temperature
Solvent flowrate
Feed flowrate
V-113 low level switch
E-407 low level switch
Units
oC
oC
oC
Range
0 150
0 150
0 - 150
oC
0 - 100
LPM
LPM
LPM
N/A
N/A
N/A
N/A
N/A
0 20
03
03
N/A
N/A
N/A
N/A
N/A
Accuracy
N/A
N/A
N/A
N/A
N/A
Additional Note:
All piping are 3/4" stainless steel 304 tubing unless stated otherwise.
2.3
Experimental Capabilities
a) Determination of the mass and energy balance of excess feed material recovery
system.
b) Demonstration of the effect of feed flow rates on the flowrate efficiency.
c) Study concept of thermodynamics of liquid-liquid system.
d) Study the operation of liquid-liquid extraction and solvent recovery system.
e) Demonstration of the effect of solvent to feed ratio on the extraction efficiency.
f) Demonstration of the effect on of organic and aqueous phase as continuous phase.
g) Determination the number of theoretical plates for the extraction column.
2.4
General Requirements
Electrical
: 415 VAC/ 50Hz (3-phase)
Cooling water : Laboratory tap water
3.0
SUMMARY OF THEORY
When separation by distillation is ineffective or very difficult, liquid-liquid extraction is one of
the main alternatives to consider. Close boiling mixtures or substances that cannot
withstand the temperature of distillation, even under a vacuum, may often be separated
from impurities by extraction, which utilizes chemical differences instead of vapor pressure
differences.
Separation by liquid-liquid extraction can be defined as the selective removal of one or
more components either from a homogeneous liquid mixture or from a solution, using a
second liquid or solvent, which is partially or wholly immiscible with the first.
The following terms are widely used to describe the different streams in a liquid-liquid
extraction system:
F
S
R
E
:
:
:
:
Feed
Solvent
Raffinate
Extract
EXTRACTION PROCESS
solvent,
S
extract, E
solute
raffinate, R
feed, F
Figure 2: Flow of Streams and Components in a Liquid-Liquid Extraction System
In an extraction process, a quantity of feed liquid, F is mixed with a quantity of solvent, S in

an agitated vessel, after which the layers are settled and separated. The extract may be
lighter or heavier than the raffinate, and so it may be shown coming from the top of the
equipment in some cases and from the bottom in others.
Since the feed is a two component system, by convention, the material to be extracted is
commonly referred to as the solute while the other component is generally referred to as
the diluent.
The raffinate stream has the same components as the feed, though the proportions are
different, with the raffinate having a much lower solute concentration (leaner). An ideal unit
with perfect extraction will yield a raffinate which has only one component, that being pure
diluent.
The liquid used to strip the solute from the feed is referred to as the solvent. However,
solvent is a general term and should not be confused with the feed solvent or diluent. The
solvent after becoming enriched in solute leaves the system as the extract.
It is also important to define the composition of the four streams and this may be done in
several ways:
a) Molar concentration
b) Molal concentration
=
=
c) Mole fraction, xA
d) Mole ratio, xA/B
e) Mass fraction, xA
f) Mass ratio, xA/B
mol/dm3 (note numerically this is the same as kmol/m3)

mol/kg
No. of moles A
Total no. of moles
No. of moles A
No. of moles B
Mass of A
Total mass
Mass of A
Mass of B
Note: Fractions and ratios are dimensionless and may also be expressed in percent (%).
The common basis used in most literatures are either mole or mass fraction.
Since liquid-liquid extraction involves a 3-component system, a graphical representation of
the liquid mixtures is usually employed. There are two graphical systems, namely:
a) Rectangular coordinates
b) Triangular coordinates
The rectangular coordinates are easier to plot, but the triangular coordinates offer a more
representative view of the component compositions. However, it is important to fix the
basis for the representation before doing any calculations.
This manual will assume a composition basis of mole fraction and plots all component
compositions in triangular coordinates.
A
P
E
B
8
Figure 3: A Typical 3-Component System Representation on an Equilateral Triangular Diagram
The individual components of the chosen ternary system are usually represented by
symbols as follows:
A = Solute
B = Diluent
C = Solvent
The assignment of symbols are arbitrary. Confusion shall not arise as long as the apex for
the solute is at the top while the bottom apexes are for the solvent and diluent.
Referring to Figure 3, the curve on the triangular diagram is called the binodal or solubility
curve of the ternary system. The curve, which is essentially a combination of diluent-rich
and solvent-rich curves, separates the upper region of stable single phase mixture from the
lower region of unstable mixture, which tends to separate into two phases.
The compositions of extract, E and raffinate, R are connected by tie-lines having different
slopes (i.e. not parallel). The tie lines get shorter as they get away from the x-axis, and
eventually they converge at a point P (plait point). The point P is not normally the highest
part of the curve.
The number of theoretical stages can be determined graphically by constructing operating
lines and tie-lines on the binodal/solubility curves, as outlined in Figure 4. Consequently,
the effects of different stirrer speeds and feed flow rates on the extraction efficiency can
then be evaluated.
P
E
R
R
Figure 4: Operating Lines and Tie Lines Constructions for Determination of Extraction Efficiency
4.0
The following chemicals will be used in the experiment:
a) Acetone (solute)
b) Water (diluent)
c) Toluene (solvent)
4.1
General Start-Up Procedure
1. Prepare the following chemicals:

a) Feed (heavy phase): mixture of acetone-water solution at the desired
composition
b) Solvent (light phase): pure toluene
2. Ensure that all valves are closed.
3. Turn on the power of the control panel and SOLDAS Software.
4. Open valves HV620 and HV621.
5. Fill solvent V-113 with pure toluene solvent and feed tank V-114 with acetonewater solution.
6. Close all valves except outlet vessel valves (HV 602 and HV 605).
7. Open valve HV606. Switch on pump P-114. Allow the acetone-water solution
(heavy phase) to enter the column and fill to a level of about 5--10 cm above
the solvent inlet. Switch off pump P-114.
8. Open HV 603 and switch on solvent pump P-113.
9. Once the liquid starts to overflow at the top of the column, switch off pump P113.
Recommendation: Set the desired flowrate of FT-311 and FT-312 (refer to
experiment 1) before overflow at the top of column.
10. The unit is now ready for experiment.
10
4.2 General Shut-Down Procedure

1. Make sure turn off all pumps (P-113, P-114, P-115 and P-117) and the heater
of reboiler 2 E-407.
2. Open valves HV 615, HV 617, HV 613 and HV 609 to drain all chemicals from
the tanks.
Note: Make sure temperature TIC-113 in the reboiler, E-407 is drop to room
temperature before drain the chemicals.
3. If the equipment will not use for a long period, follow procedure 4.3 to clean
the equipment.
4. Turn off the power for the control panel.
4.3 Cleaning Procedure
1. Drain all chemicals in tanks, columns and reboiler 2.
2. Fill feed tanks (V-113 and V-114) with filtered water.
3. Open HV 602, HV 603, HV605 and HV 606.
4. Switch on pump P-113 and P114 to pump all water to the extraction column,
T-501.
5. Switch off P-113 and P-114.
6. Repeat steps 1 to 5 using alcohol (methanol) if necessary.
11
5.0
12
5.1
EXPERIMENT 1: Extraction of Acetone from Water Using Toluene

In this experiment, there are two feeds and two outlet flows from the column.
Feed flows:
Solvent: Toluene (light phase)
Feed: Acetone-water mixture (heavy phase)
Outlet flows:
Extract : Toluene rich phase
Raffinate: Water rich phase
OBJECTIVE:
1. To study mass balance of the system
2. To study the effect of feed flow rates on the extraction efficiency
PROCEDURES:
1. Ensure that all equilibrium and calibration data are obtained (Appendix H).
2. Perform the general start-up procedures (Section 4.1).
3. Start both pumps P-113 and P-114 and set the desired feed and solvent flow
rates by adjusting the pump speed controller or/and HV 603 and HV 606
respectively.
4. Allow both liquids to flow into the collection tanks V-115 and V-116
respectively by adjusting overflow tube. The bottom product contains the water
rich phase (raffinate) while the top product contains the toluene rich phase
(extract).
5. Let the experiment run for a while to attain steady state.
6. Open valve HV 607 to collect 5 mL sample of raffinate and open valve HV 608
to collect a 5 mL sample of extract.
Note: Take samples at suitable intervals and measure their refractive indices.
When the readings are consistent over time, steady state has been
reached. Suggestion: every 10 minutes.
7. Record the refractive index of both samples at steady state and use the
calibration curves (Appendix H) to determine the acetone (solute) composition
in each phase.
8. Record all data in the sample table in Appendix A.
9. Repeat the experiment (steps 4 to 10) by using different ratio of solvent to feed
flow rates.
13
ANALYSIS AND DISCUSSION:

1. Determine the required theoretical extraction stage from the liquid-liquid
extraction experiment results. Refer to Appendix B for a step-by-step
calculation guide.
2. Calculate the height equivalent theoretical plates (HETP) of the extraction
column for different rotating disc speed.
HETP =
Effective column height

No. of theoretica l plates
3. Calculate the separation efficiency for different solvent to feed ratios and
rotating speed.
Efficiency =
=
Amount of extracted solute

Amount of solute in feed
Extract flowrate Extract compositio n

Feed flowrate Feed compositio n
4. Compare the HETP values or separation efficiency for different solvent to feed
ratio.
14
5.2
EXPERIMENT 2: RECOVERY OF SOLVENT
Objective:
1.
To study the thermodynamics of liquid-liquid systems
2.
To study the operation of liquid-liquid extraction and solvent recovery

system
Procedure
1.
Open HV 610 and HV 622.
2.
Switch on pump, P-115 to transfer extracted solution to reboiler 2 E-407.
3.
Observe the level of extracted solution. Turn off pump, P-115 immediately
when the level of extracted solution is volume of total volume of the
reboiler, E-407.
4.
Close HV 610 after transfer extracted solution to the reboiler 2 E-407.
5.
Open HV 623 and HV 624 to supply cooling water to condenser, E-408 by

controlling the flowrate of water using HV 616 to 15 L/min.
6.
Switch on the heater in the reboiler, E-407 and adjust the power of heater
to 1000W slowly.
7.
Wait until toluene in the reboiler evaporate.
8.
Collect sample from HV 614 and record refractive index of sample.
9.
Repeat steps 1 to 9 using 2000W of heater power.
15
6.0
REFERENCES
1. McCabe, Smith & Harriott, Unit Operations of Chemical Engineering, McGraw Hill,
(Singapore), 2001.
2. Robert E. Treybal, Mass Transfer Operations, Third Edition, McGraw Hill Book Co.
(Singapore), 1980.
3. Robert E. Treybal, Liquid Extraction, Second Edition, McGraw Hill Series, 1963.
4. Institution of Chemical Engineers, Standard Test Systems for Liquid Extraction,
Second Edition, 1985.
16
7.0
MAINTENANCE AND SAFETY PRECAUTIONS

1. The unit must be operated under the supervision of trained personnel.
2. All operating instructions supplied with the unit must be carefully read and understood
before attempting to operate the unit.
3. Always check and rectify any leak.
4. Always make sure that the heater is fully submerged in the water.
5. Do not touch the hot components of the unit.
6. Be extremely careful when handling liquid at high temperature.
7. Always switch off the heater and allow the liquid to cool down before draining.
8. Restore the system to operating conditions after any repair job.
9. Only properly trained personnel shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
10. Before servicing, shut down the whole operation and let the system to cool down.
17
APPENDICES
APPENDIX A
SAMPLE TABLE FOR EXPERIMENT EXPERIMENT 1
Run No.
Feed
flow rate
(L/min)
Solvent
flow rate
(L/min)
Solvent
to feed
ratio
Rotating
Disc
Speed
(RPM)
Raffinate
Time
(min)
Refractive
index
Solute
composition
(wt%)
Extract
Refractive
index
Solute
composition
(wt%)
HETP
(mm)
Separation
efficiency

Time (min)
Refractive Index (RI)
Purity of Solvent (%)
APPENDIX B
STEP BY STEP CALCULATION GUIDE
1. Obtain the equilibrium data from Appendix D or from literature. Plot the binodal/solubility curve
and the corresponding tie lines on a triangular plot (Appendix G).
2. Locate the points for:

Feed, F
Solvent, S
Raffinate, R
Extract, E
Feed and solvent mixture, M
acetone
F
M
toluene
R
water
3. Locate the point R, where all operating lines should meet.

acetone
M
R
toluene
water
4. Draw a tie line from point E to its equilibrium point on the binodal plot. Connect an operating
line from that equilibrium end of the tie line to point R. Extend that operating line so that it
intersects with the binodal plot at the other end. Draw another tie line from that new intersection
and continue until a tie line has passed the operating line connecting R and S.
acetone
R
R
toluene
water
5. Count the number of tie lines contained inside the E-F-R-S quadrilateral (it may not be a round
number). That will be the number of required theoretical stage to achieve the final raffinate and
extract compositions.
APPENDIX C
CALIBRATION PROCEDURES FOR LIQUID-LIQUID EXTRACTION EXPERIMENT
C.1
Determination Of The Binodal/Solubility Curve

OBJECTIVE:
To obtain the binodal/solubility curve for both toluene and water rich phases.
APPARATUS:
1. Conical flasks, measuring cylinders, titration apparatus.
2. Refractometer for calibration.
PROCEDURES:
1. Record the average ambient temperature throughout the experiment and obtain the
pure component densities for acetone, water and toluene at the experiment
temperature.
Toluene rich phase
2. Prepare 6 homogenous mixtures of acetone and toluene in 6 different conical flasks
according to the recommended composition listed in the first table in Appendix D.
3. Prepare the apparatus for titration and fill the burette with water.
4. Put a magnetic stirrer bar into the solution in a flask and place the flask on the stirrer
plate. Switch on the stirrer on average speed.
5. Slowly titrate the solution in the flask with water and continue titrating until cloudiness
appears and persists in the mixture. When this occurs, record the exact amount of
water that has been added. This is known as the cloud point where all three
components are in equilibrium and this represents a point on the ternary
binodal/solubility curve.
6. Take about 10 mL sample of the ternary mixture and measure the refractive index
using a refractometer. Take 3 series of readings for the same sample and record the
average.
7. Repeat the experiment (steps 3 to 6) for all 6 mixtures. Calculate the mass fraction of
each component during equilibrium and record the results in the first table in Appendix
D.
Water rich phase
1. Prepare 6 homogenous mixtures of acetone and water in 6 different conical flasks
according to the recommended composition listed in the second table in Appendix D.
2. Prepare the apparatus for titration and fill the burette with toluene.
3. Put a magnetic stirrer into the solution in a flask and place the flask on the stirrer plate.
Switch on the stirrer on average speed.
4. Slowly titrate the solution in the flask with toluene and continue titrating until
cloudiness appears and persists in the mixture. When this occurs, record the exact
amount of toluene that has been added. This is known as the cloud point where all
three components are in equilibrium and this represents a point on the ternary
binodal/solubility curve.
5. Take about 10 mL sample of the ternary mixture and measure the refractive index
using a refractometer. Take 3 series of readings for the same sample and record the
average.
6. Repeat the experiment (steps 9 to 12) for all 6 mixtures. Calculate the mass fraction of
each component during equilibrium and record the results in the second table in
Appendix D.
1. Use the sample tables in Appendix D for data collection.
a) For the toluene rich phase, after titration with water, enter the volume of water
required for ternary equilibrium. From the knowledge of pure densities for each
component, calculate their mass fraction in the mixture. Enter the refractive index
for each mixture in the appropriate column.
b) For the water rich phase, after titration with toluene, enter the volume of toluene
required for ternary equilibrium. Again, from the knowledge of pure densities for
each component, calculate their mass fraction in the mixture. Enter the refractive
index for each mixture in the appropriate column.
2. Plot the refractive index of each mixture as a function of acetone (solute) composition.
Do a separate plot for the toluene rich phase and water rich phase. This will serve as
the calibration curves for the toluene-water-acetone system, which will be used in
further experiments.
3. Plot the binodal/solubility curve for the toluene-water-acetone system. Use the ternary
diagram (triangular plot) with toluene and water at the bottom axis and acetone (solute)
at the top peak as shown in Appendix F.
C.2
Determination of Equilibrium Solute Distribution (Tie Lines)

OBJECTIVE:
To determine the tie lines connecting the binodal curves in the toluene-water-acetone
system.
APPARATUS:
1. Separating funnels for settling and separating the mixtures.
2. Conical flasks, measuring cylinders, and standard laboratory apparatus.
3. Refractometer.
PROCEDURES:
1. Obtain the calibration curve from Appendix C.1.
2. Record the average ambient temperature throughout the experiment and obtain the
pure component densities for acetone, water and toluene at the experiment
temperature.
3. Prepare 6 heterogeneous mixtures of acetone, toluene and water in 6 different conical
flasks according to the compositions recommended in the table in Appendix E.
4. Agitate the mixtures for about 60 minutes.
Note: To prevent emulsification, do not agitate the mixtures too vigorously.
5. Pour each of the mixture into a separating funnel. Let the mixture settle into two distinct
clear layers with a sharp interface.
6. Identify the top layer as the toluene rich phase (light) and the bottom layer as the water
rich phase (heavy). Withdraw a sample of each phase and measure their refractive
indices. Take the average result out of 3 readings for each sample.
7. Repeat the experiment (steps 4 to 5) for all mixtures. Using the calibration curves
prepared in Appendix C.1, determine the composition of acetone in each phase.
Record the results in the table in Appendix E.
1. Use the sample table in Appendix E for data collection. After measuring the refractive
index for each phase, fill in the corresponding columns in the table.
2. Calculate the mass fraction of each component in a mixture and mark it as the total
mixture point on the same ternary diagram as the binodal/solubility curve.
3. Using the acetone composition in each phase, locate the points of the light and heavy
phase on the binodal/solubility curve. Then, draw a tie line for each mixture by
connecting those two points. The tie lines must pass through their respective total
mixture points as a result of material balance.
4. Plot the tie line compositions (acetone composition in the toluene rich phase against
acetone composition in the water rich phase).
APPENDIX D
SAMPLE TABLES FOR APPENDIX C.1
Toluene Rich Phase
Amount in mixture (mL)
No
Acetone
Toluene
160 mL
40 mL
140 mL
60 mL
120 mL
80 mL
100 mL
100 mL
80 mL
120 mL
60 mL
140 mL
Water
added
(mL)
Composition (wt%)
Acetone
Water
Toluene
Refractive
index
Water Rich Phase

No
Acetone
Water
160 mL
40 mL
140 mL
60 mL
120 mL
80 mL
100 mL
100 mL
80 mL
120 mL
60 mL
140 mL
Toluene
added
(mL)
Composition (wt%)
Acetone
Water
Toluene
Refractive
index
APPENDIX E
SAMPLE TABLE FOR APPENDIX C.2

No.
Water rich phase
Toluene rich phase
Acetone
Acetone
Refractive
Refractive
Toluene
composition
composition
index
index
(wt%)
(wt%)
Acetone
Water
20 mL
90 mL
90 mL
40 mL
80 mL
80 mL
60 mL
70 mL
70 mL
80 mL
60 mL
60 mL
100 mL
50 mL
50 mL
120 mL
40 mL
40 mL
APPENDIX F
TRIANGULAR PLOT FOR TERNARY DIAGRAM
acetone
toluene
water
APPENDIX G
PHYSICAL PROPERTIES OF COMPONENTS
G.1
Physical Properties of Pure Components in the Ternary System
Component
Water
Toluene
Acetone
Temp
(oC)
Density
(kg/m3)
Viscosity
(10-3 Pa.s)
Surface
Tension
(10-3 Nm-1)
Refractive Index
20
25
20
25
20
25
998.2
997.02
866.7
862.3
790.5
784.4
1.003
0.8903
0.586
0.552
0.322
0.304
72.75
72.58
28.4
27.6
23.4
23.2
1.333
1.332
1.497
1.494
1.359
1.356
Acetone (CH3COCH3) :
A colourless, volatile, extremely flammable liquid, miscible with water,

used as a solvent and reagent. Also known as 2-propanone.
Toluene (C6H5CH3)
A colourless, aromatic liquid derived from coal tar or from the catalytic
reforming of petroleum naphthas; insoluble in water, soluble in alcohol
and ether, used as a chemical intermediate, for explosives, and in
high-octane gasolines. Also known as methylbenzene;
phenylmethane; toluol.
G.2
Fire and Safety Properties

Property
Acetone
Toluene
Boiling Point (oC)
56.5
110.4
Melting Point (oC)
-94.6
-95
-19
lower (% vol.)
2.6
1.2
upper (% vol.)
12.8
7.0
Ignition Temperature (oC)
538
508
Vapour Pressure @ 20 oC (mmHg)
185
22
ppm in air
1000
200
mg/m3 of air
2400
750
200-450
50
Flash Point (oC) closed cup

Explosive Limits in Air
Thresshold Limit Value
Odour Thresshold (ppm)
G.3
Binodal Compositions for Acetone-Toluene-Water System
Acetone
(wt%)
Toluene
(wt%)
Water
(wt%)
Acetone
(wt%)
Toluene
(wt%)
Water
(wt%)
0.5
0
1
1.5
2.499
4.997
10
19.97
29.91
18.9
34.5
35.71
39.56
42
42.68
42.7
46.4
49.7
49.14
48.97
53.2
54.59
55.5
57.4
59
58.81
59.19
61.5
62.2
62.84
62.85
63.5
65.1
64.23
65.62
0.026
0.029
0.03
0.043
0.05
0.054
0.06
0.16
0.3
0.4
0.5
0.62
0.92
1
1.03
1.12
1.5
2
2.05
2.06
3
3.66
4
5
6
6.12
6.54
8.5
10.04
10.23
10.38
11.5
14.9
16.22
17.63
99.474
99.971
98.97
98.457
97.451
94.949
89.94
79.87
69.79
80.7
65
63.67
59.52
57
56.29
56.18
52.1
48.3
48.81
48.97
43.8
41.75
40.5
37.6
35
35.07
34.27
30
27.76
26.93
26.77
25
20
19.55
16.75
66
66
65.9
65.01
65
64.07
62.4
62.18
59.49
58.4
55.4
54.88
54.6
51.1
48.76
48.1
46.57
44.4
42.6
42.51
40
36.08
30.1
29.57
29.4
23.5
19.85
9.98
4.995
3.996
2.997
1.999
1
0
19
19.8
20.63
24.9
25
26.94
30.6
31.53
34.43
36.6
40.6
41.47
41.58
45.9
48.76
49.4
51.19
53.6
55.69
55.8
58.5
62.63
68.9
68.97
69.78
76
79.37
89.82
94.917
95.918
96.937
97.939
98.942
99.943
15
14.2
13.47
10.09
10
8.99
7
6.29
6.08
5
4
3.65
3.82
3
2.48
2.5
2.24
2
1.71
1.69
1.5
1.29
1
1.46
0.82
0.5
0.78
0.2
0.088
0.086
0.066
0.062
0.058
0.057
G.4
Tie Line Compositions for Acetone-Toluene-Water System
Acetone Composition (wt%)

Water Rich
Phase
Toluene Rich
Phase
Water Rich
Phase
Toluene Rich
Phase
0.27
0.59
0.95
1.08
1.54
1.72
2.32
2.41
2.43
2.7
3.13
3.42
4.2
4.5
5.1
5.24
6.12
6.27
7.15
7.25
7.67
8.11
9.2
9.4
10.58
11.2
0.21
0.36
0.59
0.78
1.13
1.11
1.52
1.69
1.74
1.85
2.38
2.45
3.15
2.8
3.84
4.09
5.03
5.33
5.86
5.98
6.13
6.78
6.8
8.11
9.2
9
12.42
13.05
14.1
14.41
17.32
19.3
20
20.5
21.44
25.7
25.8
31.51
32
32.3
32.82
35.4
36.7
36.8
39.84
44.9
49.7
51.5
57.6
58.2
62.8
11.3
11.91
13.1
13.52
16.98
18.8
20.2
21.35
22.62
27.4
29.05
38.12
37.5
39.6
41.06
43.7
44.9
46.15
55.32
56
60.9
62.4
65.8
65.71
62.8
APPENDIX H
TYPICAL CALIBRATION DATA
Determination Of The Binodal/Solubility Curve
Refractive index for pure acetone = 1.3581
Refractive index for pure water = 1.3332
Refractive index for pure toluene = 1.4954
Toluene Rich Phase
Composition (wt%)
Acetone
Toluene
Water
added
(mL)
12.7
104.1
2.5
9.79
2.42
87.78
1.4753
25.2
91.8
3.0
19.48
2.92
77.60
1.4649
54.0
64.6
4.1
41.61
3.97
54.42
1.4304
67.4
50.0
5.4
52.30
5.27
42.43
1.4147
77.4
37.5
7.3
60.67
7.20
32.14
1.4006
81.6
16.3
23.0
63.58
22.54
13.89
1.3687
No
Acetone
Water
Toluene
Refractive
index
Water Rich Phase

Composition (wt%)
Acetone
Water
Toluene
added
(mL)
81.6
22.0
16.8
63.93
21.68
14.39
1.3681
80.1
25.1
13.9
63.14
24.88
11.98
1.3682
74.7
34.6
8.0
58.84
34.27
6.89
1.3661
65.0
46.1
3.6
51.22
45.68
3.10
1.3618
50.4
59.6
1.6
39.65
58.97
1.38
1.3556
25.5
80.2
1.4
19.94
78.86
1.20
1.3449
No
Acetone
Water
Toluene
Refractive
index
Calibration Curve for Toluene Rich Phase
1.5100
1.5000
1.4900
1.4800
1.4700
1.4600
RI
1.4500
1.4400
1.4300
1.4200
1.4100
1.4000
1.3900
1.3800
0
10
15
20
25
30
35
Acetone composition (wt%)
40
45
50
55
60
65
Calibration Curve for Water Rich Phase
1.3700
1.3650
1.3600
RI
1.3550
1.3500
1.3450
1.3400
1.3350
1.3300
0
10
15
20
25
30
35
40
Acetone composition (wt%)
45
50
55
60
65
70
Binodal/Solubility Curve on the Triangular Diagram
acetone
toluene
water
Determination of Equilibrium Solute Distribution (Tie Lines)

No.
Water rich phase
Toluene rich phase
Acetone
Acetone
Refractive
Refractive
Toluene
composition
composition
index
index
(wt%)
(wt%)
Acetone
Water
76.5
20.0
23.2
1.3621
51.7
1.3735
69.8
68.8
20.0
30.2
1.3574
40.8
1.3979
55.5
63.7
20.0
34.8
1.3544
32.7
1.3943
50.4
56.1
20.0
41.7
1.3531
30.1
1.4213
42.2
45.9
20.0
51.0
1.3494
21.4
1.4084
39.4
30.6
20.0
64.9
1.3443
9.6
1.4183
32.5
Tie Line Compositions
80
Acetone composition in toluene rich phase (wt%)
70
60
50
40
30
20
10
10
15
20
25
30
35
Acetone composition in water rich phase (wt%)
40
45
50
55
60
APPENDIX I: RESULTS
EXPERIMENT 1
Raffinate
Run
No.
Feed flow
rate
(L/min)
Solvent
flow
rate
(L/min)
Solvent to
feed ratio
Time
(min)
0.12
0.12
1:1
10
20
30
40
50
60
70
1.3341
1.3342
1.3354
1.3358
1.3363
1.3371
1.3363
0
10
20
30
1.3369
1.3373
1.3374
1.3371
10
20
30
40
1.4098
1.4121
1.3422
1.3413
0.12
0.12
0.12
0.24
1:1
1:2
Refractive
index
Extract
Solute
composition
(wt%)
HETP
(mm)
Separation
efficiency
(%)
5.0
1.4511
1.4508
1.4411
1.4435
1.4461
1.4461
1.4464
32.1
760
64.0
7.0
1.4431
1.4445
1.4444
1.4463
32.6
797
65.2
Solute
composition
(wt%)
Refractive
index
1.3395
1.3425
1.4162
1.4211
50
60
70
1.3422
1.3402
1.3390
9.5
1.4631
1.4655
1.4651
19.5
889
39.0
Composition Diagram for Run 1 Data
For Run 1 data:

=
2000
2.63
= 760
=
=
=

32.1%
50%
= 0.640
For Run 2 data:
2000
2.51
= 797
=
=
=

32.6%
50%
= 0.652
For Run 3 data:
2000
2.25
= 889
=
=
=

19.5%
50%
= 0.390
POWER OF HEATER
REFRACTIVE INDEX
PURITY OF TOLUENE (%)
1000 W
1.4850
90
2000 W
1.4901
93

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SOLTEQ

EQUIPMENT FOR ENGINEERING EDUCATION & RESEARCH

SOLUTION ENGINEERING SDN. BHD.

GENERAL DESCRIPTION .................................................................................................. 3

Description and Assembly....................................................................................... 3

SUMMARY OF THEORY ..................................................................................................... 7

General Start-Up Procedure ................................................................................. 10

APPENDIX A SAMPLE TABLE FOR EXPERIMENT

Process Flow Diagram for the Liquid-Liquid Extraction Unit

Flow of Streams and Components in a Liquid-Liquid Extraction System

A Typical 3-Component System Representation on an Equilateral

Operating Lines and Tie Lines Constructions for Determination of

EXCESS FEED MATERIAL RECOVERY SYSTEM

Stainless Steel 304

Stainless Steel 304

Stainless Steel 304

Stainless Steel 304

SS316 Metering Pump

SS316 Metering Pump

SS304 Vertical Centrifugal Pump

SS304 Vertical Centrifugal Pump

20-L vessel, horizontal

Coil Heat Exchanger

Packed column; SS304

Description and Assembly

Product Pump (P-115)

Valves and Instruments List

Figure 2: Flow of Streams and Components in a Liquid-Liquid Extraction System

In an extraction process, a quantity of feed liquid, F is mixed with a quantity of solvent, S in

d) Mole ratio, xA/B

f) Mass ratio, xA/B

mol/dm3 (note numerically this is the same as kmol/m3)

Figure 3: A Typical 3-Component System Representation on an Equilateral Triangular Diagram

General Start-Up Procedure

1. Prepare the following chemicals:

4.2 General Shut-Down Procedure

EXPERIMENT 1: Extraction of Acetone from Water Using Toluene

ANALYSIS AND DISCUSSION:

Effective column height

Amount of extracted solute

Extract flowrate Extract compositio n

EXPERIMENT 2: RECOVERY OF SOLVENT

To study the thermodynamics of liquid-liquid systems

To study the operation of liquid-liquid extraction and solvent recovery

Open HV 610 and HV 622.

Switch on pump, P-115 to transfer extracted solution to reboiler 2 E-407.

Close HV 610 after transfer extracted solution to the reboiler 2 E-407.

Open HV 623 and HV 624 to supply cooling water to condenser, E-408 by

Wait until toluene in the reboiler evaporate.

Collect sample from HV 614 and record refractive index of sample.

Repeat steps 1 to 9 using 2000W of heater power.

MAINTENANCE AND SAFETY PRECAUTIONS

EXPERIMENT 2: RECOVERY OF SOLVENT

Refractive Index (RI)

Purity of Solvent (%)

2. Locate the points for:

3. Locate the point R, where all operating lines should meet.

Determination Of The Binodal/Solubility Curve

Determination of Equilibrium Solute Distribution (Tie Lines)

Water Rich Phase