SINGLE STAGE MIXER SETTLER

EXPERIMENT 5: SINGLE PHASE MIXER SETTLER

1.

INTRODUCTION The Single Stage Mixer Settler (Model: BP 13) has been designed to demonstrate the basic principles of a liquid-liquid extraction process. The normal mode of operation is that the light phase and heavy phase are pumped into the mixing chamber where the extraction takes place before flowing into the settling chamber. Finally, the light phase and heavy phase are separated in the separating chamber. Sample points are provided at key positions around the plant to allow samples of both light and heavy phase liquids to be collected for analysis. In this way the effects of changing the stirrer speed or feed flow rate can be evaluated. A schematic diagram of the plant is shown in Figure 1. 2. THEORETICAL BACKGROUND

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. A widely used terminology describes the system in terms of: F: S: R1 : E1: Feed Solvent Raffinate Extract

Each stream consists of two components. The feed stream consists of the required component (solute) and solvent (diluent or feed solvent or raffinate solvent). The raffinate stream has the same components as the feed, though the proportions are different. On the other hand, the extract stream consists of the required component (solute or extracted component) and solvent (extracting solvent or extractant). The difference between the extracted component (solute) and the extracting solvent or extractant should be made clear at all times. 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 has the same components as the feed, though hopefully it is much less concentrated in solute, i.e., it is said to be leaner. An ideal unit with perfect extraction gives a raffinate which has one component only, that being pure diluent.

V7 V8
SINGLE STAGE MIXER SETTLER

SINGLE STAGE MIXER SETTLER

V9
sampling sampling

V10

V11

V12

V5

V6

V4

V3

B3
(EXTRACT)

B4

B2
(SOLVENT)

(RAFFINATE)

P2

P1

B1
(FEED)

V2

V1

V15

V16

V14

V13

Figure 1. Single Stage Mixer Settler Process Diagram.

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The liquid used to strip the solute from the feed is referred to as the solvent. However, solvent is a general term and can sometimes be confusing as for example by describing the diluent as the feed solvent. The term feed solvent should then be avoided. 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: i) Molar concentration mol.dm-3 (note numerically this is the same as kmol.m-3) mol.kg-1 = (no. of moles A)/(total no. of moles) = (no. of mole A)/(no. of moles B) = (mass of A)/(total mass) = (mass of A)/(mass of B)

ii) iii) iv) v) vi)

Molal concentration Mole fraction, xA Mole ratio, xA Mass fraction, xA Mass ratio, xA

Note: a) fractions and ratios are dimensionless b) fractions and ratios may also be expressed as % Since liquid-liquid extraction generally involves a 3-component system, a graphical representation of the liquid mixtures is usually employed. There are two graphical systems, namely: a) Rectangular coordinate b) Triangular coordinate The choice of which system to use is a matter of preference and convenience. However, it is important to fix the basis for the representation. A common basis is mass fraction. The individual components of the chosen ternary system are usually represented by symbols as follows: A = Solvent B = Diluent C = Solute However, one might come across with literature assigning the symbols differently. Confusion shall not arise as long as the apex for the solute is at the top while the bottom apexes are for either solvent or diluent. The curve on the diagram is called binodal (solubility) curve of the ternary system. The curve, which is essentially a combination of diluent-rich and solvent-rich curves,

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separates the upper region of stable single phase mixture from the lower region of unstable mixture which tend to separate to give extract and raffinate.
c

P F M

E1

Rn S B A

Figure 2. A typical 3-component system representation on equilateral triangular diagram.

P F R1 R R2 R3 Rn R4 B M

E1 E2 E3

E4 S A

Figure 3. Tie lines constructions for determination of HETS (height of equivalent to one theoretical stage).

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 to a point P (plait point). The point P is not normally the highest part of the curve.

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The number of theoretical stages can then be determined graphically by constructing tie-lines E1-R1, E2-R2, and so forth, as outlined in Figure 3. The effect of changing the stirrer speed or the feed flow rate shall then be evaluated. 4. LIQUID-LIQUID EXTRACTION EXPERIMENT (MIXER SETTLER UNIT) In all of the experiments outlined below, the following chemicals used are: A = toluene (solvent) B = water (diluent) C = acetone (solute). 4.1 General Start-up Procedure Before running Experiment 3, it is necessary to perform the following start-up procedures. i) Perform a pre-start-up check on the valves. a) All valves closed (screwed in). ii) Charge the feed vessels and set the interface level. a) Prepare the chemicals (heavy phase and light phase) prior to lab session. b) Charge vessel B1 with feed (heavy phase). c) Charge vessel B2 with solvent (light phase). d) Set the interface level by adjusting valve V7. (Please refer to manufacturers manual on setting the interface level) iii) Start-up the plant. a) Open inlet valves V1 and V2. Open vent valve V3, V4, V5 and V6. b) Switch on main power for the feed pumps. Set the stroke for pumps P1 and P2 to middle. c) Allow the heavy phase and light phase to enter the mixing chamber and overflow into settling chamber to form two layers. d) Watch the interface level which forms between the light and heavy phase. Carefully adjust the interface level as necessary. Allow the heavy phase and light phase to overflow into respective collection vessels B3 and B4. e) Stop the pumps. Close inlet valves V1 and V2. f) The plant is now ready for experiment.

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4.2

Experiment A: Determination of Binodal/Solubility Curve OBJECTIVE: To obtain the binodal/solubility curve for both water-rich and toluene-rich phases. APPARATUS: 1. Beakers, measuring cylinders, titration apparatus. 2. Refractometer for calibration. PROCEDURE: Toluene rich phase: 1. Prepare at least six different homogenous mixtures of acetone and toluene in separate flasks (usually used in titration) properly labeled. 2. Place one of the mixtures on a magnetic stirrer. Switch the stirrer on average speed. 3. Slowly titrate the above solution 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 one point on the ternary binodal/solubility curve. Keep at least 10 ml of the resulting mixture for calibration purposes. 4. Repeat steps 2 and 3 above for the other homogenous mixture of acetone and toluene prepared earlier. 5. Measure the refraction indices using a refractometer for each of the resulting solution that you kept for calibration in step 3. Be sure to take an average of three readings. Water rich phase: 6. Prepare at least six different homogenous mixtures of water and acetone in separate flasks (usually used in titration) properly labeled. 7. Place one of the mixtures on a magnetic stirrer. Switch the stirrer on average speed. 8. Slowly titrate the above solution 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 one point on the ternary binodal/solubility curve. Keep at least 10 ml of the resulting mixture for calibration purposes. 9. Repeat steps 7 and 8 above for the other homogenous mixture of water and acetone prepared earlier. 10. Measure the refraction indices using a refractometer for each of the resulting solution that you kept for calibration in step 8. Be sure to take an average of three readings.

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11. Measure the average temperature during your experiments. CALCULATIONS AND EXERCISES: 1. You may use the sample tables in Appendix A for data collection. 2. For the toluene rich phase use the first table. Fix the volume of toluene and acetone and enter the values in the table. After titration with water, enter the volume of water required for ternary equilibrium in the table. From the knowledge of pure densities for each component the rest of the columns in the table can then be calculated. Measure the refraction indices and enter the values in the last column of the table. 3. For the water rich phase use the second table. Fix the volume of water and acetone and enter the values in the table. After titration with toluene, enter the volume of toluene required for ternary equilibrium in the table. Again, from the knowledge of pure densities for each component the rest of the columns in the table can then be calculated. Measure the refraction indices and enter the values in the last column of the table. 4. Plot the refractive indices vs. solute (acetone) composition. This will be the calibration curve for the Toluene-Water-Acetone system. This curve will then be used in the Experiments B and C. 5. Plot the binodal/solubility curve for this system. You may use the triangular graph supplied in Appendix B. 4.3 Experiment B: Determination of Equilibrium Solute Distribution (Tie Lines) Note: Before starting Experiment B, you must plot the calibration curve from the steps 5 and 10 in Experiment A. You may plot both curves on one graph (refraction index vs. weight fraction of acetone). OBJECTIVE: To determine the tie lines connecting the binodal curves obtained in Experiment A. APPARATUS: 1. Conical flasks and separating funnels for settling separating the solution. 2. Beakers, measuring cylinders, standard laboratory apparatus. 3. Refractometer PROCEDURE: 1. Fill the conical flasks with heterogeneous mixture of water, acetone and toluene. Prepare at least 6 different compositions. 2. Agitate the mixtures prepared in step 1 simultaneously for at least 90 minutes. 3. Stop the agitator. Let the mixtures to settle (for about an hour) in a separating funnel into two distinct clear layers with a sharp interface.

SINGLE STAGE MIXER SETTLER

4. Withdraw a sample of each phase and measure the refractive index of each phase. Again, take an average of three readings for each phase. The water rich phase (raffinate) would be the heavy phase and toluene rich phase would be the light phase (extract). 5. Repeat step 4 for all of the heterogeneous mixtures. 6. The calibration curve prepared in Experiment A can be used to determine the composition of acetone in each phase determined in steps 4 and 5. 7. Draw the tie lines connecting the extract and raffinate using the composition determined in steps 4 and 5. These tie lines must pass through the total mixture point (M) based on the amount added in step 1. 8. Measure the average temperature during your experiments. CALCULATIONS AND EXERCISES: 1. Student may use the sample tables in Appendix C for data collection. 2. After taking the refractive index on each phase, enter these values in the corresponding columns in the table prepared in Appendix C. 3. The percent weight of each phase can then be determined by using the calibration curve prepared in Experiment A. 4. Plot the two points (for each phase) on the binodal/solubility curve prepared in Experiment A and connect them by straight lines. These straight lines represent the tie lines in the binodal/solubility curve. 4.4 Experiment C: Liquid-liquid Extraction Using a Single-Stage Mixer Settler Unit. In this experiment, there are two feeds to the mixer i.e. light phase and heavy phase. There are also two outlets i.e. extract and raffinate. For this experiment: Feed Flows: Light Phase: Pure Toluene Heavy Phase: Fixed composition of acetone-water mixture (say 50% weight) Outlet Flows: Extract: Toluene rich phase Raffinate: Water rich phase OBJECTIVE: To study the effect of stirrer speed on the extraction efficiency. PROCEDURE: 1. Perform the start-up procedure as outlined in section 4.1. 2. Switch on the pumps. Open inlet valves V1 and V2. Set the desired feed ratio by adjusting the pumps stroke. 3. Switch on the stirrer and set the speed to 150 rpm.

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4. Allow the plant to run until steady state has been reached. Collect a sample (about 10 ml) of each phase from the respective outlet streams (extract: toluene rich phase, and raffinate: water rich phase). Use sampling valves V11 and V12 for heavy phase and light phase, respectively. Note: Take samples at suitable intervals and each time take refractive index readings for each phase. When readings are consistent with the previous set, steady state has been reached. This may take about 40 to 60 minutes. 5. Measure the refractive index of the sample taken in step 4 for each phase using a refractometer. The calibration curve prepared in Experiment A can be used to determine the composition of acetone in each phase. 6. Repeat steps 3 to 5 for different stirrer speeds of 200, 250, 300, 350 rpm (while maintaining the feed composition and flow rates). 7. Summarize your results in a table (Appendix D) and comment on the effect of stirrer speed on extraction efficiency. CALCULATIONS AND EXERCISES: 1. Determine the experimental extraction efficiency for each stirrer speed. 2. Plot the Extraction Efficiency vs. Stirrer Speed.