CHAPTER

EIGHT
EXTRACTION

8.1 8.3

Liquid-Liquid Extraction Solid-Liquid Extraction by Soxhlet Apparatus

One of the principal objects of theoretical research is to find the point of view from which it can be expressed with greatest simplicity. J.W.GIBBS

Chapter 8: EXTRACTION

8.1 LIQUID-LIQUID EXTRACTION

Keywords : Liquid-liquid extraction, mass transfer, organic removal.

8.1.1 Object

The object of the experiment is to demonstrate how a mass balance performed on the extraction column, and to measure the mass transfer coefficient and its variation with flow rate with the aqueous phase as the continuous medium.

8.1.2 Theory

Many processes in chemical engineering require the separation of one or more of the components of a liquid mixture by treating the mixture with an immiscible solvent in which these components are preferentially soluble. In some cases purification of a liquid may be the function of the process, in others the extraction of a dissolved component for subsequent processes may be the important aspect. An example of the former is the preparation of the pure organic liquids from products of the oil industry. Liquid-liquid extractions may also be used as energy saving processes by, for example, eliminating distillation stages. It is possible, of course that the substance of interest may be heat-sensitive anyway and that distillation is accordingly an unacceptable process.

When separation by distillation is ineffective or very difficult, liquid extraction is one of the main alternatives to consider. Close-boiling mixtures or substances that cannot withstand the temperature of the distillation, even under a vacuum, may often be separated from impurities by extraction, which utilizes chemical differences instead of vapor pressure differences. For example, penicillin is recovered from fermentation broth by extraction with a solvent such as butyl acetate. Another example for liquid extraction is recovering acetic acid from dilute aqueous solutions; distillation would be possible in this case, but the extraction step considerably reduces the amount of water to be distilled.

When either distillation or extraction may be used, the choice is usually distillation, in spite of the fact that heating and cooling are needed. In extraction the solvent must be recovered for reuse (usually by distillation), and the combined operation is more complicated and often more expensive than ordinary distillation without extraction. However, extraction does offer more flexibility in choice of operating conditions, since the type and the amount of solvent can be varied as well as the operating temperature. In many problems, the choice between the methods should be based on a comparative study of both extraction and distillation.

In liquid-liquid extraction, as in gas absorption and distillation, two phases must be brought into contact to permit transfer of material and then be separated. Extraction equipment may be operated batchwise or continuous. The extract is the layer of solvent plus extracted solute and the raffinate is the layer from which solute has been removed. The extract may be lighter or heavier than the raffinate, and so the extract may be shown coming from top of the equipment in some cases and from the bottom in others. The operation may of course be repeated if more than one contact is required, but when the quantities involved are large and several contacts are needed, continuous flow becomes economical.

The rate at which a soluble component is transferred from one solvent to another will be dependent, among other things, on the area of the interface between the two immiscible liquids. Therefore it is very advantageous for this interface to be formed by droplets and films, the situation being analogous to that existing in packed distillation columns.

The theory for the system Trichloroethylene-Propionic acid-Water is as follows:

Let

Vw : Water flow rate, lt/s Vo : Trichloroethylene flow rate, lt/s X : Propionic acid concentration in the organic phase, kg/lt Y : Propionic acid concentration in the aqueous phase, kg/lt

Subscripts:

1 : Top of column 2 : Bottom of column

Chapter 8: EXTRACTION

Mass Balance :

Propionic acid extracted from the organic phase (rafinate).

= Vo ( X1 − X 2 ) Propionic acid extracted by the aqueous phase (extract) = Vw ( Y1 − 0) Therefore theoretically,

(8.1.1)

(8.1.2)

Vo ( X 1 − X 2 ) = Vw ( Y1 − 0)
Mass transfer coefficient:

(8.1.3)

MTC =

Rateof acid transfer Volumeof packing × Meandriving force

(8.1.4)

where

Log mean driving force : (∆X1-∆X2) / ln (∆X1/∆X2)

∆X1 : Driving force at the top of the column = (X1-X1*) ∆X2 : Driving force at the bottom of the column = (X2-X2*) = X2
where X1* and X2* are the concentrations in the organic phase which would be in equilibrium with concentrations Y1 and Y2 ( = 0.0) in the aqueous phase, respectively. The equilibrium values can be found using the distribution coefficient for the chemicals used (Assumde that Y=KX relation holds at equilibrium for a constant K). Rate of acid transfer may be calculated using Eqs.(8.1.1) or (8.1.2) based on raffinate or extract phases, respectively.

8.1.3 Apparatus

The apparatus of this experiment is shown in Figure 8.1.1.

1.) Solvent collection tank, initially empty 2.) Solvent feed tank, initially full 3.) Organic solution pump 4.) Water pump 5.) Rotameter

6.) Water feed tank, initially full 7.) Water collection tank, initially empty 8.) Extraction column 9.) Top and bottom electrodes

Figure 8.1.1 - Liquid-liquid extraction apparatus.

8.1.4 Experimental Procedure

1.

Add 100 ml of propionic acid to 10 liters of trichloroethylene. Mix well to ensure an even concentration then fill the organic phase feed tank (bottom tank) with the mixture.

2.

Switch the level control to the bottom of the column by keeping the bottom electrodes on. (switch S2 valve on)

3.

Fill the water feed tank with 15 liters of clean demineralised water, start the water feed pump and fill the column with water at high flow rate.

4.

As soon as the water is above the top of the packing, reduce the flow rate to 0.2 lt/min.

Chapter 8: EXTRACTION

5. 6.

Start the metering pump and set at a flow rate of 0.2 lt/min. Run for 15-20 minutes until steady conditions are achieved, monitor flow rates during this period to ensure that they remain constant.

7. 8.

Take two or three batches of 15 ml samples from the feed, raffinate and extract streams. Titrate 10 ml of each sample against 0.1 M NaOH using phenolphthalein as the indicator. (To titrate the feed and raffinate needed). continuous stirring using a magnetic stirrer may be

9.

Repeat the experiment with water flow rate being increased to 0.3 lt/min.

Note : Calibration of pump is needed whenever a change in flow rates is necessary. The procedure for calibration is as follows :

The solvent metering pump is calibrated in percentage of maximum flow which varies slightly from pump to pump. The pump should be calibrated initially by setting F2 to 100%, setting valve V8 to the calibrated position and measuring the flow from the pump, using a measuring cylinder and stopwatch. Calculate the flow rate produced settings of 10% intervals (ml/min), then plot a graph of ml/min against percentage of metering pump stroke. Thereafter any selected flow may be obtained by using the graph.

8.1.5 Report Objectives

1.

Find propionic acid concentrations in each stream. Calculate the average value for each data point. Check the variances and eliminate the outliers if there are any. Carry out the following calculations using the refined data set.

2. 3.

Calculate the mass transfer coefficients based on both phases. What is the maximum possible acid transfer rate? Calculate the column efficiency using experimental and maximum acid transfer rate. What should be done to achieve the maximum acid transfer rate?

4. 5.

Repeat the calculations for all flow rates. Try to answer the following questions in your discussion and conclusion: a) Why does the mass transfer coefficient depend on the phase selected as the base? b) How does the flow rate affect MTC? Why? c) How can the efficiency of the column be increased? d) Were there any source of error in the experiment? How can this experiment be improved?

8.1.6 References

1.

Bennett, C. O., and J. E. Myers, Momentum, Heat and Mass Transfer, 3rd edition, McGrawHill, 1983.

2.

Perry, R. H., and D. Green, Perry’s Chemical Engineering Handbook, 6th. edition, McGraw-Hill, 1984.

3.

Sinnott, R. K., J. M. Coulson, and J. F. Richardson, An Introduction to Chemical

Engineering Design, 1st edition, Pergamon Press, 1983.

Chapter 8: EXTRACTION

8.3 SOLID-LIQUID EXTRACTION BY SOXHLET APPARATUS

Keywords: Leaching, solute, solvent, cocurrent, countercurrent, multiple system, triangular
diagram.

8.3.1. Object

The object of this experiment is to study the basic principles of leaching.

8.3.2. Theory

Extraction is a term used for an operation in which a constituent of a liquid is transferred to another liquid (solvent). The term solid-liquid extraction is restricted to those situations in which a solid phase is present and includes those operations frequently referred to as leaching, lixiviation and washing.

Extraction always involves two steps:

1.

Contact of the solvent with the solid to be treated so as to transfer the soluble constituent (solute) to the solvent;

2.

Separation or washing of the solution from the residual solid.

These two steps may be conducted in separate equipment or in the same piece of equipment.

Liquid always adheres to the solid which must be washed to prevent either the loss of solution if the soluble constituent is the desired material or the contamination loss of the solids if these are the desired material. The complete process also includes the separate recovery of the solute and solvent. This is done by another operation such as evaporation or distillation.

The equipment used for solid-liquid extraction is classified according to the manner in which the first step is done. The term solid bed or fixed bed refers to any operation in which the solid particles are kept in relatively fixed positions with respect to each other while the solvent flows through the bed of solid particles, whether or not the bed of solid material remains stationary with respect to the earth during the extraction. The opposite of this situation, called dispersed

contact, refers to any operation in which the solid particles, suspended in the fluid, are in motion
relative to each other and to the solvent during the time of contact.

Solid-liquid extraction

Solid-liquid extraction (leaching) is the process of removing a solute or solutes from a solid by using of liquid solvent. Leaching is widely used in chemical industries where mechanical and thermal methods of separations are not possible or practical. Extraction of sugar from sugar beets, oil from oil bearing seeds, production of a concentrated solution of a valuable solid material are typical industrial examples of leaching. Leaching process can be considered in three parts:

1. 2. 3.

Diffusion of the solvent through the pores of the solid The diffused solvent dissolves the solutes (i.e. transfer the solute to the liquid phase). Transfer of the solution from porous solid to the main bulk of the solution.

In fixed-bed contacting the solid particles are stationary in a tank, in which the solvent is allowed to percolate through the bed of undissolved solids. In leaching by the soxhlet apparatus multiple contacts of solids with the fresh solvent is performed at each stage of operation. This is equivalent to multiple cocurrent system, as described in the following diagram.

fresh solvent

solid feed solution overflow

solid underflow

Figure 8.3.1. Multiple cocurrent system

Chapter 8: EXTRACTION

8.3.3. Apparatus

The apparatus used in this experiment is shown in Figure 8.3.2

1. Water Outlet 2. Water Inlet 3. Soxhlet condenser 4. Soxhlet extractor (lower d = 1.5 cm, upper d = 4.3 cm) 5. Round bottom flask

Figure 8.3.2. Soxhlet apparatus

8.3.4. Experimental Procedure

1. 2.

Weigh 9 grams of oil containing ground seeds. Crush and dry them in an oven for 30 minutes @ 105°C and determine the moisture content. Carefully add the sample into the filter paper, do not overfill and leave at least a 1 cm gap between the sample and the top of the filter paper. Place another filter paper on top of the sample to prevent sample loss during the extraction.

3.

Place several boiling chips into a clean, dry round bottom flask. Weigh the container, with chips, and record as the tare weight of the container.

4.

Pour 325 ml hexane into the round bottom flask as a solvent. Insert filter paper & sample into the extractor, assemble the Soxhlet apparatus and start leaching and continue the process up to the end of the third siphon.

5.

When the extraction time is complete, remove the filter paper & sample and carefully transfer it into an evaporating dish. Weigh the sample. Dry it in an oven. Weigh the sample the next day again.

6.

Weigh the round bottom flask with hexane and extracted oil before distillation. Assembly distillation apparatus and distill the extract in order to separate the oil and solvent. Weigh the recovered hexane. Let the round bottom flask with recovered oil dry overnight. Weigh the container the next day again.

7. 8.
9.

8.3.5. Report Objectives

1.

Perform the necessary mass balance for hexane in order to calculate the amount of lost hexane.

2.

Perform overall mass balance considering input values are feed and solvent (hexane) and output values are inflow and outflow.

3. 4.

Calculate the moisture content, yield of extractor and percent oil recovery. Analyze the operation on a triangular diagram.

8.3.6. References

1. Brown, G. G., Unit Operations, John Wiley & Sons, 1956. 2. McCabe, W. L., and J. C. Smith, Unit Operations of Chemical Engineering, McGraw-Hill,
1956.

3. Perry, R. H., and D. Green, Perry’s Chemical Engineers’ Handbook, 6th Edition, McGrawHill, 1988.

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