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EXTRACTION and SUGAR INDUSTRY APPLICATIONS

EXTRACTION
1-LEACHING(SOLID EXTRACTION) a) GENERAL INFORMATION b) FACTORS INFLUENCING THE RATE OF EXTRACTION c) LEACHİNG EQUİPMENT 2- LIQUID-LIQUID EXTRACTION a) EXTRACTION PROCESS b) CLASSIFICATION OF EXTRACTION EQUIPMENT - STAGE-WISE EQUIPMENT FOR EXTRACTION - DIFFERENTIAL CONTACT EQUIPMENT FOR EXTRACTION EXTRACTION IN SUGAR INDUSTRY APPLICATIONS 1- THE FİXED-BED OR ROBERT DİFFUSİON BATTERY 2- CONTİNUOUS DİFFUSİON BATTERİES

EXTRACTION
Extraction is the method of removing one constituent from a solid or liquid by means of a liquid solvent.Extraction techniques fall into two categories.The first is called leaching or solid extraction and the is second called liquid extraction.

such as a pigment .The process may be used either for the production of a concentrated solution of a valuable solid material. .or in order to remove an insoluble solid .LEACHING (SOLID EXTRACTION) A-GENERAL INFORMATION Leaching is concerned with the extraction of soluble constituent from a solid by means of a solvent.from a soluble material with which it is contaminated.

.and therefore the higher is the rate of transfer of material and the smaller is the distance the solute must diffuse within the solid. Agitation of the fluid:Agitation of the solvent is important because this increases the eddy diffusion and therefore the transfer of material from the surface of particles to tha bulk of the solution.There are four important factors to be considered: Particle size: The smaller the size .the greater is the interfacial area between the solid and liquid. Temperature:In most cases.the diffusion coefficient will be expected to increase with rise in temperature and this will also improve the rate of extraction. Solvent:The liquid chosen should be a good selective solvent and its viscosity should be sufficiently low for it to circulate freely.B-FACTORS INFLUENCING THE RATE OF EXTRACTION The selection of the equipment for an extraction process is influenced by the factors which are responsible for limiting the extraction rate.the solubility of the material which is being extracted will increase with temperature to give a higher rate of extraction.Further .

Both methods may be either batch or continuous.permeable mass throughout the leaching operation . .LEACHİNG EQUİPMENT When the solids form an open .With impermeable solids or materials that dissintegrate during leaching.solvent may be percolated through an unagitated bed of solids.the solids are dispersed into the solvent and are later separated from it.

it flows through the several tanks in series and is finally withdrawn from the tank that has been freshly charged.sprayed with solvent until their solute content is reduced to the economical minimum. In some cases the rate of the solution is so rapid that one passage of solvent through the material is sufficient .Leaching by percolation through stationary solid beds Stationary solid-bed leaching is done in a tank with a perforated false bottom to support the solids and permit drainage of the solvent.In this method.but countercurrent flow of solvent through a battery of tanks is more common.and excavated. .such a series of tanks is called an extraction battery.Solids are loaded into the tank. fresh solvent is fed to the tank containing the solid that is most nearly extracted.

.Moving-bed leaching In the machines that are used for this type of leaching. the solids are moved through the solvent with little or no agitation.The bollman extractor (figure a) contains a bucket elevator in a closed casing.As solids and solvent flow cocurrently down the right-hand side of the machine .There are perforations in the bottom of each bucket.the buckets are loaded with flaky solids such as soybeans and are sprayed with appropriate amounts of half miscella as they travel downward.the solvent extracts more oil from beans.Half miscella is the intermediate solvent containing some extracted oil and some small solid particles.At the top right-hand corner of the machine .

Bollman extractor .Simultaneously the fine solids are filtered out of the solvent.a stream of pure solvent percolates countercurrently through them.Fully extracted beans are dumped from the buckets at the top of the elevator into a hopper from which they are removed by paddle conveyors.As the partially extracted beans rise through the left side of the machine . so that clean full miscella can be pumped from the right –hand sump at the bottom of the casing.It collects in the left-hand sump and is pumped to the half-miscella storage tank.

The basket rotates slowly about a vertical axis.Solids are admitted to each compartment at the feed point. and a discharge point at which the floor of the compartment opens to discharge the extracted solids. Rotocel extractor . and the solids in each preceeding compartment are washed with the effluent from the succeeding one.The empty compartment moves to the feed to point to receive its next load of solids.In the Rotocel extractor. a drainage section. fresh solvent is fed only to the last compartment before the discharge point.To give countercurrent extraction.illusrated in figure b. a horizontal basket is divided into walled compartments with a floor that is permeable to the liquid.the compartments then successively pass a number of solvent sprays.

either before or during leaching . are treated by dispersing them in the solvent by mechanical agitation in a tank or flow mixer.The leached residue is then separate from the strong solution by settling or filtration.Dispersed –solid leaching Solids that form impermeable beds. Small quantities can be leached batchwise in this way in an agitated vessel with a bottom drawoff for settled residue. .

It is possible to combine stages 1 and 2 into a single piece of equipment such as a column which is then operated continuously. 2-Seperation of the resulting two phases. 3-Removal and recovery of the solvent from each phase. it is essential that the liquid-mixture feed and solvent are at least partially if not completely immiscible and. In this operation. Such an operation is known as differential contacting.LIQUID-LIQUID EXTRACTION The separation of the components of a liquid mixture by treatment with a solvent in which one or more of the desired components is preferentially soluble is known as liquid-liquid extraction. Liquid-liquid extraction is also carried out in stagewise equipment. following by settling in a separate vessel by gravity. three stages are involved: 1-Bringing the feed mixture and the solvent into intimate contact. . in essence. the prime example being a mixersettler unit in which the main features are the mixing of the two liquid phases by agitation.

. in the production of anhydrous acetic acid in the extraction of phenol from coal tar liquors. It may also be used to obtain. relatively pure compounds such as benzene. and xylene from catalytically produced reformates in the oil industry. for example. and in the metallurgical and biotechnology industries. toluene.Important applications of liquid-liquid extraction include the separation of aromatics from kerosene-based fuel oils to improve their burning qualities and the separation of aromatics from paraffin and naphthenic compounds to improve the temperature-viscosity characteristics of lubricating oils.

In the single-stage batch process illustrated in the figure.single-stage batch extraction . the solvent and solution are mixed together and then allowed to separate into the two phases-the extract E containing the required solute in the added solvent and the raffinate R. With this simple arrangement mixing and seperation occur in the same vessel. Fig.EXTRACTION PROCESSES All liquid-liquid extraction operations. the weaker solution with some associated solvent. may be carried out either as a batch or continuous process.

A continuous two-stage operation is shown in figure. Fig. where the mixers and separators are shown as separate vessels.Multiple-contact system with fresh solvent .

CLASSIFICATION OF EXTRACTION EQUIPMENT Essentially there are two types of design by which effective multistage operation may be obtained: 1-Stage-wise contactors. in which equipment includes a series of physical stages in which the phases are mixed and separated. 2-Differential contactors. in which the phase are continuously brought into contact with complete phase separation only at the exits from the unit. and. .

the solution and solvent are mixed by some form of agitator in the mixer.STAGE-WISE EQUIPMENT FOR EXTRACTION The mixer settler In the mixer-settler. and the liquid densities and the form of the dispersion are important parameters. . and then transferred to the settler where the two phases separate to give an extract and a raffinate. In the settler the separation is often gravitycontrolled.

The impeller has sweptback vanes with double shrouds. and the two phases meet in the draught tube. Figure.This arrangement gives a good performance and is mechanically neat.Thus WARWICK and SCUFFHAM give details of a design. A baffle on the top of the agitator reduces air intake and a baffle on the inlet to the settler is important in controlling the flow pattern.Combined mixer-settler units Recent work has emphasised the need to consider the combined mixersettler operation. shown in the figure in which the two operations are effected in the one combined unit.Mixer-settler .

The centrally situated mixer is designed to give the required hold up.In segmented mixersettler specially designed KnitMesh pads are used to speed up the rate of coalescence.The segmented mixersettler.Segmented mixer-settler . Figure. each fed by individual pipework. and the mixer is pumped at the required rate to the settler which is formed in segments around the mixer.

Kühni mixer-settles column . and each with a mixing and settling zone as shown in the figure.Kuhni have recently developed a mixersettler column which is a series of mixersettlers in the form of a column. Fig. The unit consists of a number of stages installed one on the top of another. each hydraulically separated.

though since the baffles can be positioned very close together at 75-150 mm.Baffle-plate column . The efficiency of each plate is very low. it is possible to obtain several theoretical stages in a reasonable height.Baffle-plate columns These are simple cylindrical columns provided with baffles to direct the flow of the dispersed phase. Figure. as shown in the figure.

The Scheibel column One of the problems with perforated plate and indeed packed columns is that redispersion of the liquids after each stage is very poor. in which a series of agitators is mounted on a central rotating shaft. shown in the figure. To overcome this.Scheibel column . Between the agitators is fitted a wire mesh section which successfully breaks up any emulsions. SCHEIBEL and KARR introduced a unit. Figure.

Although spray towers are simple in construction. In the former case (a) the light phase enters from a distributor at the bottom of the column and the droplets rise through the heavier phase. finally coalescing to form a liquid-liquid interface at the top of the tower. in which case interface is held at the bottom of the tower as shown in (b). Alternatively the heavier phase may be dispersed. . they are inefficient because considerable recirculation of the continuous phase takes place.DIFFERENTIAL CONTACT EQUIPMENT FOR EXTRACTION Spray columns Two methods of operating spray columns are shown in next figure. Either the light or heavy phase may be dispersed. As a result true countercurrent flow is not maintained and up to 6 m may be required for the height of one theoretical stage.

Figure.Spray towers .

suspensions. and considerably increases mass transfer rates compared with those obtained with spray columns because of the continuous coalescence and break-up of the drops. .Packed columns The packing increasing the interfacial area. They have proved to be satisfactory in the petroleum industry. or high viscosity liquids. Packed columns are unsuitable for use with dirty liquids.

Rotary annular columns and rotary disc-columns With these columns mechanical energy is provided to form the dispersed phase. The equipment is particularly suitable for installations where a moderate number of stages is required.Rotary annular column . Figure. and where the throughput is considerable. A well dispersed system is obtained with this arrangement. The figure shows a rotary annular column.

. VAN DUCK and others have devised methods of providing the whole of the continuous phase with a pulsed motion.Pulsed columns In order to prevent coalescence of the dispersed drops. This may be done. either by some mechanical device.Pulsed packed columns have been used in the nuclear industry. The pulsation markedly improves performance of packed columns. or by the introduction of compressed air. There are advantages in using gauze-type packings since the pulsation operation often breaks ceramic rings.

In the Podbielniak contactor. the large drops then being driven out by centrifugal force.the heavy phase is driven outwards by centrifugal force and the light phase is displaced inwards. Referring to the next figure. . the heavy phases enters at D. The two liquids intermix in zone E where they are flowing countercurrently through the perforated concentric elements are separated in the spaces between. a centrifugal extractor may be used in which the mixing and the separation stages are contained in the same unit which operates as a differential contactor. In zones F and G the perforated elements are surfaces on which the small droplets of entrained liquid can coalesce. passes to J and is driven out at B.Centrifugal extraction If separation is difficult in a mixer-settler unit. The light phase enters at A and is displaced inwards towards to shaft and leaves at C.

Figure.Podbielniak contactor .

High shear forces are thus generated giving high extraction rates. with the heavy phase flowing countercurrently. has a vertical spindle and the rotor is fitted with concentric cylindrical inserts with helical wings forming a series of spiral passages. Fig. The two phases are fed into the bottom.Working principle of Alfa-Laval centrifugal extractor . the light phase being led to the periphery from which it flows inwards along the spiral.The Alfa-Laval contactor shown in the figure.

The processing starts by slicing the beets into thin chips. The extraction takes place in diffusers. The slicing is done with sharp knives which cut a V selection slice 4 to 5 mm thickness to increase the surface area of the beet to make it easier to extract the sugar. Beets are washed and seperated from any remaining beet leaves before processing. The two well known diffusers for sucrose extraction are The fixed-bed or Robert diffusion battery and Continuous diffusion batteries or Silver continuous diffuser. .EXTRACTION IN SUGAR INDUSTRY APPLICATIONS Extraction is needed for sucrose extraction from beets and cane.

for the extraction of certain pharmaceuticals from barks and seeds. but is also used for the extraction of tanning extracts from tanbark.Since each cell is filled and discharged completely .The piping is so arranged that the fresh water comes in contact with the most nearly extracted material. .THE FİXED-BED OR ROBERT DİFFUSİON BATTERY This was developed primarily in the beet-sugar industry. and the strongest solution leaves from contact with the fresh material. and similar processes. It consists of a row of vessels filled with the material to be extracted and through which water flows in series.

each cell in the battery changes its position in the cycle.Two main headers are necessary . Figure shows that is a diagrammatic illustration of the principle of a diffusion battery. .one at a time.One handles water and the other handles solution. as circumstances may dictate.In figure shows that the valves that are open are shown as circles and the valves that are closed are shown in solid black.For every vessel or cell there is a heater.and therefore the piping must be so arranged that water can be fed to any cell.and for every cell there must be three valves.The arrangement of valves and piping became standardized in the beet industry and is generally found an all forms of diffusion battery. and the thick liquor drawn off from any cell. because the diffusion process takes place more rapidly at higher temperatures.

Fig.Diagram of diffusion battery .

up through its heater. down through the heater of cell 3.It would not be convenient to pass the solution down through cell 3 because of the air which would be entrapped. and the process continued. therefore additional heating is desirable.and up through cell 3. and out tı the process. Cell 1 is nearly exhausted and the cell 3 has just been charged.By this time another cell to the right of those shown has been filled.When liquid appears at this vent.The operation shown in figure continued until cell 1 is completely extracted.Consider figure.Liquid now flows down through cell 3. cell 1 is dumped.Water is introduced into cell 1 and flows down through cell 2. and up through its heater.In a diffusion battery for beet cossettes there may be from 10 to 15 cells.The space between the cossettes in cell 3 is therefore filled with air. the liquid flows from the heater of the cell 2 through the solution line. A vent at the top of this cell discharges air. .Consequently. the valves are quickly changed to the position shown in figure.and the charge is cold. water is introduced to cell 2.

Cossettes are intoduced into the battery through chute C and are carried together with the liquid in the direction indicated by the arrows.At the end of the first trough is a Wheel D with inclined perforated buckets on the inside.The battery consists essentially of a series of closed troughs A.A’.It is so arranged that the screw B discharges the cossettes into this wheel.The figure shows only three units. and discharged through chute E which takes them into the second trough A. but actually the battery consists of 20 to 24 units arranged in two tiers. Here the helix carries them in the opposite direction discharges them from this to another wheel which in turn forwards them to another trough A’’. and so on until they are exhausted and leave the battery. one above the other. .drained free from juice lifted. where they are picked up by the buckets. each provided with a helical screw B.CONTİNUOUS DİFFUSİON BATTERİES The next figure shows the Silver Continuous diffuser.A’’.

Silver continuous diffuser:A. feed chute. D. transfer chute for chips. C. transfer Wheel.conveyor for moving cossettes.A’.A’’. . B. E. extraction trougs.