CCB 3062 Unit Operation Laboratory 2 January 2014

Experiment Group Group Members

: : :

Single Phase Mixer Settler 2 Muhammad Hafiz bin Mokhtar Kamil NurAlia Syairah binti Osman Mohd Ikmal Hisham bin Azahari Nur Amirah binti Mohamed Rashidi Nur Farhana Ajua binti Mustafa Nurul Alia bt Mohamad 15641 15669 15640 15570 15583 15607

Lab Instructor

Mr. Ahmed Ali 28 January 2014

Date of Experiment :

1.0 INTRODUCTION Mixer-settlers are widely used in industry because of their reliability, operating flexibility, and high capacity. They can handle difficult-to-disperse systems, such as those having high interfacial tension and/or large phase density difference. They can also cope with highly viscous liquids and solid-liquid slurries Single stage mixer settler has been designed to demonstrate the basic principles of liquid-liquid extraction process. It mainly consists of a glass mixer settler, feed vessels, feed pumps and receiver vessels. The mixer settler has 3 zone which are mixing, settling and separation zones. The normal mode of operation is that the light phase and heavy phase are continuously 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. Sampling 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.

2.0 OBJECTIVE

1. To run the process of liquid-liquid extraction using a single stage mixer settler. 2. To run extraction process using any tertiary system (e.g. acetone water-toluene). 3. To determine the extraction efficiency of the mixer settler and study the effect of solvent to feed ratio on the extraction efficiency. 4. To study the effect of stirrer speed on the separation performance. 5. To obtain the bimodal/solubility curve for both water-rich and toluene-rich phases. 6. To determine the tie lines connecting the bimodal curves obtained in Experiment A.

3.0 THEORY 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: Feed S: Solvent R: Raffinate E1: Extract Each stream consists of two components. The feed stream consists of the required omponent (solute) and solvent (dilute 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 orextractant should be made clear at all times. Since the feed is a two-component system, by convention, the material to be extractedis 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 withperfect extraction gives a raffinate which has one component only, that being purediluent. 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.

4.0 RESULT
Experiment A : Determination of binodal/solubility curve

Refractive index of pure water : 1.3340

No Amount in mixture, mL Acetone 1 2 3 4 5 6 55 50 40 30 20 10 Toluene 5 10 20 30 40 50 9.5 6.6 3 2 1 0.5 Water added, mL Composition, wt% Acetone 75.79 72.07 60.79 45.79 30.65 15.24 Water 16.64 12.09 5.79 3.88 1.96 0.97 Toluene 7.57 15.85 33.42 50.34 67.39 83.79 1st 1.37162 1.39277 1.40763 1.43061 1.45591 1.46618 Refractive index(RI) 2nd 1.38213 1.39317 1.40786 1.43030 1.45590 1.46542 3rd 1.37106 1.36932 1.40785 1.42829 1.45590 1.46596 average 1.37494 1.38509 1.40778 1.42973 1.45590 1.46585

Table 1 : Toluene Rich Phase

No

Amount in mixture, mL Acetone Water 5 10 20 30 40 50

Touleneadde d, mL Acetone 24.8 11.6 3 1.5 1.3 0.5 62.06 66.26 58.21 43.15 27.81 7.83

Composition, wt%

Refractive index(RI)

Water 7.17 16.85 36.99 54.49 70.23 49.42

Toluene 30.76 16.89 4.79 1.97 1.97 42.75

1st 1.39925 1.38775 1.36969 1.36031 1.35120 1.34604

2nd 1.36545 1.37231 1.36951 1.36000 1.35064 1.34689

3rd 1.36569 1.37203 1.36869 1.36016 1.35087 1.34649

average 1.37679 1.37736 1.36929 1.36016 1.35090 1.34667

1 2 3 4 5 6

55 50 40 30 20 10

Table 2 : Water Rich Phase The calibration curve is shown in the appendix.

Experiment 2 : Determination of Equilibrium Solute Distribution-Tie Line

N o. Amount in Mixture Acetone Water Toluene 1st 1 2 3 4 5 6 10 20 30 40 50 60 40 35 30 25 20 15 40 35 30 25 20 15 1.34494 1.34505 1.34921 1.35216 1.35847 1.36383 Water Rich Phase Refractive Index(RI) 2nd 1.34499 1.34501 1.34982 1.35427 1.35931 1.36351 3rd 1.34489 1.34505 1.34969 1.35413 1.35914 1.36251 Average 1.34494 1.345046 1.34957 1.35352 1.35897 1.36328 Acetone Composit ion (wt%) 7.0816 7.1898 11.8061 15.8367 21.3980 25.7959 Toluene Rich Phase Refractive Index (RI) 1st 1.47727 1.46672 1.44717 1.42540 1.40331 1.36572 2nd 1.48116 1.47009 1.44793 1.42955 1.40330 1.36630 3rd 1.47766 1.46624 1.45180 1.43028 1.40331 1.36617 Average 1.47870 1.46768 1.44897 1.41925 1.40331 1.36606 Acetone Composit ion (wt%) 17.30 28.32 47.03 76.75 92.69 129.94

Graph for Experiment B are plotted in the appendix

Experiment C: Liquid-liquid Extraction Using a Single-Stage Mixer Settler Unit

Stirrer Speed (RPM)

Feed Composition (wt %) Heavy Light Phase Phase (Water(Toluene) Acetone)

Pump Stroke Setting (mm) Heavy Phase (P1) Light Phase (P2) Time (min)

Outlet Composition (RI) Heavy Phase (WaterAcetone) 1.349 1.346 1.349 1.363 1.349 1.349 1.349 1.349 1.349 1.348 1.346 1.348 1.349 1.349 1.349 Light Phase (Toluene) 1.451 1.467 1.429 1.379 1.468 1.457 1.467 1.467 1.466 1.467 1.467 1.468 1.465 1.466 1.467

150

200

50

Pure Toluene

Middle

Middle

250

10 20 30 40 50 10 20 30 40 50 10 20 30 40 50

Outlet Composition (wt %) Heavy Light Phase Phase (Water(Toluene) Acetone) 13.750 30.330 10.000 19.670 13.750 45.000 31.250 78.300 13.750 19.000 13.750 26.330 13.750 19.670 13.750 19.670 13.750 20.330 12.500 19.670 10.000 19.670 12.500 19.000 13.750 21.000 13.750 20.330 13.750 19.670

Extraction Efficiency (Average)

0.48

0.52

0.59

Graph for Experiment C is plotted in the appendix

Sample Calculation Experiment A : Determination of binodal/solubility curve 1) Composition (wt%) Mass = Density*Volume Mass of Acetone : Mass of Toluene : Mass of Water : 0.7844 x 55 0.8623 x 5 = = 43.142 g 4.3115 g 9.47169 g

0.99702 x 9.5 =

wt% of acetone = wt% of acetone : x 100 = 75.79%

x 100

Experiment B: Determination of Equilibrium Solute Distribution (Tie lines) 2) Tie Line Graph. The composition is taken by using the calibration of the graph. As you can see in the graph, the water rich phase formula is y = 0.0008x + 1.338 and the toluene rich phase is y = - 0.001x +1.496. Just substitutes the number of refractive index will get the composition.

Experiment C: Liquid-liquid Extraction Using a Single-Stage Mixer Settler Unit 3) Extraction Efficiency Extraction Efficiency =

5.0 DISCUSSION In the Experiment A: Determination of binodal/solubility curve, calibration curve for waterrich phase was prepared by using six homogenous mixtures with different compositions at the same volume, fixed at 60 ml. The amount of acetone and toluene is as shown in table below. The homogenous mixtures of acetone and water were prepared in a beaker where a magnetic stirrer was used and make sure it stir well then titrated it with toluene until it reach equilibrium point that is when the mixture turn to cloudy. For toluene-rich phase, six different mixtures were prepared and titrated until it reaches the equilibrium point that is when the mixture turn cloudy. The homogenous mixtures of acetone and toluene were titrated the same way with water as water-rich mixtures with toluene. The end point is when the 3 components, water acetone and toluene reach equilibrium and the solution become cloudy. The refractive index is measured three for each mixture and the average reading is calculated. A graph of refractive index against acetone composition is plotted to obtain the calibration curves for toluene-rich phase, it shown that the refractive index of the sample mixture decreased as the composition of acetone increased. This shows us that as we increase the volume of toluene the refractive index of the mixture sample decrease. For water rich phase, based on the calibration curve, the refractive index is increasing as the acetone composition decrease. The composition of toluene is also decreasing when the composition of acetone decreases. This means that the lower the volume of toluene added, the less the refractive index. In experiment B, six heterogeneous mixtures of different compositions of water, acetone and toluene were prepared. The solutions were mixed for 40 minutes and then left to settle in the settling tank about 45 minute to let it settle into 2 distinct layers. After it had separated into a heavy (water rich phase) and light (toluene rich phase) in the settling tank, the refractive index of the light phase and heavy phase were measured. The result shown that in water rich phase, the average refractive index is 1.34 to 1.36 significantly. The refractive index for toluene rich phase is a bit higher than water rich phase. From the refractive index measured, referring to the calibration curve prepared in part A, the acetone composition of each heavy phase and light phase could be determined. Based on the calibration curve, acetone composition for both heavy and light phase is increased. Then, by using the acetone compositions in each phase, the points of the light and heavy phase could be located on the bimodal/solubility curve. A tie line was then drawn by connecting the two points. The equation of tie line composition is y = 5.5144x 16.558.

6.0 CONCLUSION For the first experiment, the end point is when the 3 components, water acetone and toluene reach equilibrium and the solution seems cloudy. For the toluene-rich phase, the refractive indexes are increasing as the amount of toluene in the mixture increases which is close to the value of refractive index of the toluene. For water-rich phase, the refractive index is decreasing as the amount of the water increases which is close to the value of refractive index of the water. For the second experiment, six homogenous mixtures of different compositions of water, acetone and toluene were prepared. From the refractive index measured, referring to the calibration curve prepared in part A, the acetone composition of each heavy phase and light phase could be determined. Then, by using the acetone compositions in each phase, the points of the light and heavy phase could be located on the bimodal/solubility curve. The refractive index for toluene rich phase is a bit higher than water rich phase. For the third experiment, a Single-Stage Mixer settler unit was used, having four tanks for the feed, Solvent, extract and raffinate. Three different stirrer speeds were used, 150rpm, 200rpm, and 250rpm to determine the refractive index and the compositions of the heavy phase and light phase. The composition for the heavy and the light phase was determined from the calibration curve of part A. Water-rich phase curve was used to determine the compositions of acetone in heavy phase, and toluene-rich phase curve was used to determine the compositions of acetone in light phase. We have proven that when we increase the rotation of the disc, the separation efficiency increases. This is due to the increase of the surface area of the fluid. This makes more molecules of acetone extracted from the water phase.

7.0 APPENDIX
Experiment A : Determination of binodal/solubility curve

Refractive Index of Water Rich Phase

1.4 1.39 1.38 Refractive Index (RI) 1.37 1.36 1.35 1.34 1.33 1.32 1.31 1.3 0 20 40 60 Acetone Composition (%) Refractive Index of water Rich Phase Linear (Refractive Index of water Rich Phase) y = 0.0008x + 1.338

Refractive Index of toluene Rich Phase

1.48

1.46

1.44 Refractive Index of toluene Rich Phase Linear (Refractive Index of toluene Rich Phase) y = -0.0015x + 1.4965 1.38

1.42

1.4

1.36 0 20 40 60 80

Experiment B: Determination of Equilibrium Solute Distribution (Tie lines)

Tie Line Composition

140 Acetone Composition of Toluene Rich Phase(%) y = 5.5144x - 16.558 120 100 80 Tie Line Composition 60 40 20 0 0 5 10 15 20 25 30 Acetone Composition of Water Rich Phase (%) Linear (Tie Line Composition)

Experiment C: Liquid-Liquid Extraction Using a Single-Stage Mixer Settler Unit

Stirrer Speed VS Extraction Efficiency

0.7 Extraction Efficciency 0.6 0.5 0.4 0.3 0.2 0.1 0 0 50 100 150 200 250 300 Stirrer Speed (RPM) y = 0.0011x + 0.31