Unit Operation-I (PHARM-231)

UNIT-II Filtration & Centrif !ation

Unit-II
Filtration and Centrifugation : Theory of filtration, filter aids, filter media, industrial filters including filter press, rotary filter, edge filter. Factors affecting filtration, Principles of centrifugation, industrial centrifugal filters and centrifugal sedimenters.

FILTRATION Filtration is a mechanical or physical operation which is used for the separation of solids from fluids (liquids or gases) by interposing a medium through which only the fluid can pass. Oversi e solids in the fluid are retained, but the separation is not complete! solids will be contaminated with some fluid and filtrate will contain fine particles (depending on the pore si e and filter thic"ness). Filtration may be defined as a process of separation of solids from a fluid by passing the same through a porous medium that retains the solids, but allows the fluid to pass through.

The suspension is to be filtered is "nown as slurry. The porous medium used to retain solid is "nown as filter medium. The accumulated solids on filter medium are "nown as filter ca"e, while the clear liquid passing through the filter is filtrate. #hen solids are present in a very low concentration, i.e. not e$ceeding %.&' w(v, the process of its separation from liquid is called clarification. Process of Filtration: ) typical filtration operation is shown in figure.

The pores of the filter medium are smaller than the si e of particles to be separated. Filter medium (for e$ample filter paper or muslin cloth) is placed on a support (a sieve). #hen slurry (feed) is passed over the filter medium, the fluid flows through the filter medium, the fluid flows through the filter medium by virtue of pressure differential across the filter. *ravity is acting on the liquid column. Therefore, solids are trapped on the surface of the filter medium.
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Once the preliminary layer of particles is deposited, further filtration is brought about wherein the filter medium serves only as support. The filter will wor" efficiently only after an initial deposit. +n an industrial scale, large quantities of suspensions are mechanically handled. )fter a particular point of time, the resistance offered by the filter ca"e is high that virtually filtration is stopped. For this reason, a positive pressure is applied on the filter ca"e (upstream) or negative pressure (suction) is applied below the filter medium (downstream). Applications Filtration is used to separate particles and fluid in a suspension, where the fluid can be a liquid, a gas or a supercritical fluid. ,epending on the application, either one or both of the components may be isolated. Filtration, as a physical operation is very important in chemistry for the separation of materials of different chemical composition. ) solvent is chosen which dissolves one component, while not dissolving the other. -y dissolving the mi$ture in the chosen solvent, one component will go into the solution and pass through the filter, while the other will be retained. This is one of the most important techniques used by chemists to purify compounds. Filtration is also important and widely used as one of the unit operations of chemical engineering. +t may be simultaneously combined with other unit operations to process the feed stream, as in the biofilter, which is a combined filter and biological digestion device. Filtration differs from sieving, where separation occurs at a single perforated layer (a sieve). +n sieving, particles that are too big to pass through the holes of the sieve are retained. +n filtration, a multilayer lattice retains those particles that are unable to follow the tortuous channels of the filter. Oversi e particles may form a ca"e layer on top of the filter and may also bloc" the filter lattice, preventing the fluid phase from crossing the filter (blinding). .ommercially, the term filter is applied to membranes where the separation lattice is so thin that the surface becomes the main one of particle separation, even though these products might be described as sieves. Filtration differs from adsorption, where it is not the physical si e of particles that causes separation but the effects of surface charge. /ome adsorption devices containing activated charcoal and ion e$change resin are commercially called filters, although filtration is not their principal function. a) Production of sterile products b) Production of bul" drugs c) Production of liquid oral formulations d) )ffluent and waste water treatment Methods or Mechanis of Filtration

There are many different methods of filtration! all aim to attain the separation of substances. /eparation is achieved by some form of interaction between the substance or ob0ects to be removed and the filter. The substance that is to pass through the filter must be a fluid, i.e. a liquid or gas. 1ethods of filtration vary depending on the location of the targeted material, i.e. whether it is dissolved in the fluid phase or suspended as a solid. /ome of the mechanisms are2 !" #training: /imilar to sieving, i.e. the particles of larger si e cannot pass through the smaller pore si e of the filter medium.
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$" I pinge ent: /olids having a momentum move along the path of streamline flow and stri"e (impinge) the filter medium. Thus, the solids are retained on the filter medium. %" &ntangle ent: Particles become entwined (entangled) in the mass of fibres (of cloth with a fine hairy surface or porous felt) due to smaller si e of particles than the pore si e. Thus the solids are retained on the filter medium. '" Attracti(e forces: /olids are retained on the filter medium as a result of attractive forces between particles and filter medium, as in case of electrostatic precipitation. +n practice, filtration may combine various mechanisms. T)P&# OF FILTRATION -ased on mechanism, two types of filtration are broadly identified. !" #urface *screen" filtration: +t is screening action by which pores or holes of the medium prevents the passage of solids. $" +epth filtration: +n this process, slurry penetrates to a point where the diameter of solid particles is greater than that of tortuous void or channel. +ifferences ,et-een #urface and +epth filtration #.No. ! $ % ' / #urface Filtration The si e of particles retained is slightly higher than the mean pore si e of medium. 1echanical strength of the filter medium is less, unless it is made of stainless steel. +t has low capacity. The si e of particles retained is more predictable. 3quipment is e$pensive because it should require ancillary equipment such as edge clamps, which 0 should be much finer tolerances. 3$ample is cellulose membrane filter. +epth Filtration The si e of particles retained is much smaller than the pores trough which fluid passes. 1echanical strength is high. +t has high capacity. The si e of particles retained is less predictable. .heaper because ancillary equipment is not required. 3$amples are ceramic filters and sintered (bed) filters. Ca1e filtration: ) filter consists of a coarse woven cloth through which a concentrated suspension of rigid particles is passed so that they bridge the holes and form a bed. 3$ample is filter ca"e made from diatomite (%&&4m). T2&OR) OF FILTRATION The flow of a liquid through a filter follows the basic rules that govern the flow of any liquid through the medium offering resistance. The rate of flow may be e$pressed as2 Rate 3 dri(ing force 4 resistance

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The rate of filtration may be e$pressed as volumes (litres) per unit time (dv(dt). The driving force is the pressure differential between the upstream and downstream of the filter. The resistance is not constant. +t increases with an increase in the deposition of solids on the filter medium. Therefore filtration is not steady state. The rate of flow will be greatest at the beginning of the filtration process, since the resistance is minimum. Once the filter ca"e is formed, its surface acts as filter medium and solids continuously deposit adding to the thic"ness of the ca"e. The resistance to flow is related to several factors as mentioned below. 5esistance to movement 6 pressure upstream 7 pressure downstream ( length of capillaries Poiseuille5s e6uation: Poiseuille considered that filtration is similar to the streamline flow of a liquid under pressure through capillaries. 7 3 89Pr' 4:L; #here, 8 6 rate of flow, i.e., volume of liquid flowing in unit time, m9(s :P 6 pressure difference across the filter, Pa r 6 radius of the capillary in the filter bed, m ; 6 thic"ness of the filter ca"e (capillary length), m < 6 viscosity of the filtrate, Pa.s +arc<5s e6uation: Poiseuille=s law assumes that the capillaries found in the filter are highly irregular and non>uniform. Therefore, if the length of capillary is ta"en as the thic"ness of the bed, a correction factor for radius is applied so that the rate equation is closely appro$imated and simplified. The factor influencing the rate of filtration has been incorporated into an equation by ,arcy, which is2 7 3 =A9P 4 ; L #here, ? 6 permeability coefficient of the ca"e, m@ depends upon the characteristic of ca"e, such as porosity, specific surface area and compressibility ) 6 surface area of the porous bed (filter medium), m@ =o>en<-Car an e6uation: Poiseuille=s equation is made applicable to porous bed, based on a capillary type structure by including additional parameters. Thus the resultant equation, which is widely used for filtration is ?o eny>.armen equation.

FILT&R AI+# Filter aids forms a surface deposit which screens out the solids and also prevents the plugging of the supporting filter medium. Characteristics: a) .hemically inert to the liquid being filtered and free from impurities.
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b) ;ow specific gravity, so that filter aids remain suspended in liquid. c) Porous rather than dense, so that previous ca"e can be formed. d) 5ecoverable. +isad(antages: The filter aids remove the colored substance by absorbing them. /ometimes active principles such as al"aloids are adsorbed on the filter aid. 5arely, filter aids are a source of contaminants such as soluble iron salts, which can provo"e degradation of sensitive ingredients. ;iquid retained in the pores of the filter ca"e is lost in the manufacturing process. 3$ample2 ?eiselguhr, Talc, .harcoal, )sbestos, Paper pulp, -entonite and fuller earths etc. .ertain filter aids may be used to aid filtration. These are often incompressible diatomaceous earth or "ieselguhr, which is composed primarily of silica. )lso used are wood cellulose and other inert porous solids such as the cheaper and safer perlite. These filter aids can be used in two different ways. They can be used as a pre coat before the slurry is filtered. This will prevent gelatinous>type solids from plugging the filter medium and also give a clearer filtrate. They can also be added to the slurry before filtration. This increases the porosity of the ca"e and reduces resistance of the ca"e during filtration. +n a rotary filter, the filter aid may be applied as a precoat! subsequently, thin slices of this layer are sliced off with the ca"e. The use of filter aids is usually limited to cases where the ca"e is discarded or where the precipitate can be separated chemically from the filter. Filter flas" (suction flas", with sintered glass filter containing sample). Aote the almost colourless filtrate in the receiver flas". FILT&R M&+IA The filter medium act as a mechanical support for the filter ca"e and is also responsible for the collection of solids. Characterstics: %) +t should have sufficient mechanical strength. @) +t must be inert, for e$ample it should not show chemical or physical interaction. 9) +t should not absorb the dissolved material. B) +t should allow the ma$imum passage of liquid,while retaining the solids. +t means that it must offer low resistance to flow. The resistance offered by the filter medium is not significant in large scale operations and can be neglected. Mtaerials: %) #oven materials such as felt or cloth2 made of wool, cotton, sil", glass, metal or synthetic fibres. @) Perforated sheet metal2 /tainless steel filter in metafilter (edge filter). 9) -ed of granular solid built up on a supporting medium2 *ranular solids such as gravel, sand, aasbestos, paper, pulp and "eisulguhr.
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B) Perforated porous solid unit2 /intered glass, sintered metal, earthenware and porous plastics. C) 1emebrane filter media2 pore si e range> %&& 4m to even less than &.@ 4m. a) /urface type cartridge2 .artridge of corrugated and resin papers, ceramic and porcelain filter candles are used. b) ,epth type cartridge2 made up of cotton, asbestos or cellulose. &?a ples of filtration include %. The coffee filter to "eep the coffee separate from the grounds @. D3P) filters in air conditioning to remove particles from air 9. -elt filters to e$tract precious metals in mining. B. Furnaces use filtration to prevent the furnace elements from fouling with particulates. C. Pneumatic conveying systems often employ filtration to stop or slow the flow of material that is transported, through the use of a baghouse. E. +n the laboratory, a -Fchner funnel is often used, with a filter paper serving as the porous barrier. G. )n e$periment to prove the e$istence of microscopic organisms involves the comparison of water passed through ungla ed porcelain and unfiltered water. #hen left in sealed containers the filtered water ta"es longer to go foul, demonstrating that very small items (such as bacteria) can be removed from fluids by filtration. H. +n the "idney, renal filtration is the filtration of blood in the glomerulus, followed by selective reabsorbtion of many substances essential for the body. CLA##IFICATION OF FILTRATION &@UIPM&NT Classification ,ased on the application of e?ternal force: !" Pressure filters- Plate and frame filter press and metafilter. $" 7acuu filters- Filter leaf %" Centrifugal filters Classification ,ased on the operation of filtration: !" Continuous filtration- ,ischarge and filtrate are separated steadily and uninterrupted. $" +iscontinuous filtration- ,ischarge of filtered solids is intermittent. Filtrate is removed continuously. The operation should be stopped to collect the solids. Classification ,ased on the nature of filtration: !" Ca1e filters- 5emove large amount of solids (sludge or crystals). $" Clarif<ing filters- 5emove small amount of solids %" Cross-flo- filters- Feed of suspension flows under pressure at fairly high velocity across the filter medium.

FILT&R L&AF
Principle: Filter leaf is an apparatus consisting of a longitudinal drainage screen covered with a filter cloth. The mechanism is surface filtration and acts as sieve or strainer. 8acuum or pressure can be applied to increase the rate of filtration.

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Construction: The general arrangement of filter leaf is shown in figure.

+t consists of narrow frame enclosing a drainage screen or grooved plate. The frame may be of any shape, circular, square or rectangular. The whole unit is covered with filter cloth. The outlet for the filtrate connects to the interior of the frame through suction. Aor1ing: The filter leaf is immersed in the slurry. 8acuum system is connected with to the filtrate outlet. The slurry passes through the filter cloth. Finally filtrate enters the drainage canal and goes through the outlet into the receiver. )ir is passed to flow in reverse direction which facilitates removal of ca"e. Uses: The filter leaf is satisfactory, if the solid content of the slurry is not too high, about C', i.e., dilute suspensions. Ad(antages: %) Filter leaf is versatile piece of equipment. +t is a simplest form of filter used for batch process. @) ) number of units can be connected in parallel to increase surface area of filtration. 9) Pressure difference can be obtained either with vacuum or using pressure up to the order of H&& ?.Pa. B) ;abour costs for operating the filter leaf are faily moderate. C) The efficiency of washing is high. E) /lurry can be filtered from any vessel.

ROTAR) +RUM FILT&R

Principle: 5otary drum filter functions on the principle of filtering slurry through sieve>li"e mechanism on a rotating drum surface, under the conditions of vacuum. +n addition, compression, drying (using hot air) and removing the filter ca"e (using a "nife) are possible. Construction: The construction of rotary drum filter is shown in figure. +t consists of a metal cylinder mounted hori ontly. The drum may be up to 9 metres in diameter and 9.C metres in length and gives a surface area of @& metre square. The curved surface is a perforated plate, which supports a filter cloth. The drum is rapidly partitioned dividing the annular space into separate compartments. 3ach of it is connected by an internal pipe to the centre of the drum through a rotating valve.

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UNIT-II Filtration & Centrif !ation

Aor1ing: The drum is rotated at a speed les then one revolution per minute. The drum 0ust enters the slurry in the trough. )s it dips, vacuum is applied in this segment so that the solid is build up on the surface. The liquid passes through the filter cloth into an internal pipe and valve. Finally the filtrate is collects in collecting tan". )s the drum leaves the slurry section, it enters the drainage one. Dere e$cess of the liquid is drawn inside. /pecial ca"e compression rollers may be included in this stage, so that the ca"e is consolidated by the compression of ca"e. This improves the efficiency of washing and drying process. )s the drum leaves the drainage one, it enters the water wash section. #ater is sprayed on ca"e. ) separate section of vacuum is applied on the panel in order to suc" the wash liquid and air through the ca"e of solids. #ash liquid is drawn through the filter into a separate collecting tan". Then the ca"e enters t drying one, where hot air is blown on the ca"e. The ca"e may have the moisture content less than one percent. Finally the ca"e is removed using doctor "nife and discharged. )ll these steps are completed in one rotation of the drum. Aow the drum is ready to receive a fresh lot of slurry. Uses: ,rum filter is used for continous operation and is utili ed to filter slurries containing high proportion of solids upto %C to 9& percent. +n the production of penicillins, the e$tract is separated mycelium (cell mass) by drum filters. These are used for collecting calcium carbonate, starch and magnesium carbonate. Ad(antages: %) .a"e is removed simultaneously during operation. Therefore, suitable for use with concentrated slurries. @) The labour costs are very low on account of automatic and continuous operation of the rotary filter. 9) The filter has large surface area. B) The speed of rotation can be varied and the ca"e thic"ness can be controlled. For e$ample, if the solids from an impenetrable ca"e, the thic"ness may be limited to less than C mm. on the other hand, if the solids are coarse and form a porous ca"e, the thic"ness of %&& mm or more, can be obtained.

&+B& FILT&R *M&TAFILT&R"

Principle: 1etafilter functions as strainer (surface filtration) for the separation of particles. +n this method, metal rings contain semicircular pro0ections, which are arranged as a nest to form channels on the edges. This channel

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offers resistance (strainer) to the flow of solids (coarse particles). The clear liquid is collected into a receiver from the top. Construction: The construction and assembly of metafilter is shown in figure. The metafilter consists of a series of metal rings. These are threaded so that a channel is formed on the edges. +t contains a grooved drainage column. On which a series of metal rings are pac"ed. These rings are usually made of stainless steel and have dimensions of about %C.& mm internal diameter and @@.& mm e$ternal diameter. 3ach metal ring has a number of semicircular pro0ections (&.H mm in thic"ness) on one side of the surface. The pro0ections are arranged the same way up. These rings are tightened on the drainage column with nut. Therefore, metafilter is also "nown as edge filters.

Aor1ing: These filters are placed in a vessel and may be operated by pumping the slurry under pressure or occasionally by the application of reduced pressure to the outlet side. The slurry passes through the channels formed on edges between the rings. The clear liquid rises up and collected from the outlet receiver. 1etafilter functions as strainer (surface filtration). For the separation of fine particles, a bed of suitable material such as "eisulguhr is first build up. The pac" of rings serves essentially as a base on which the true filter medium is supported. Uses: 1etafilter can be used for2 %) .larification of syrups @) Filtration of in0ection solutions 9) .larification of insulin liquors B) Filtration of viscous liquids can be achieved by applying pressure. Ad(antages: %) 1etafilter can be used under high pressures, without danger of bursting the filter medium.
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@) 5unning costs are low, as separate filter medium is not used. The volume of residual hold up in filter is less. 9) +t can be constructed from a material that can provide e$cellent resistance to corrosion and avoid contamination of sensitive products. B) +t is e$tremely versatile filter. +t can be used for the filtration of very fine particles using filter aids. ;arge particles can be separated by building up of a bed of same particles. C) 5emoval of ca"e is carried out effectively, by simply bac">flushing with water. E) .hange over from one batch to another or one product to another is easy. G) /terile products can be handled.

FACTOR# AFF&CTINB FILTRATION

/ome factors influencing the filtration are2 %) Properties of the liquids 7 density, viscosity and corrosiveness. @) Properties of the solids 7 particle shape, particle si e, particle charge, density, particle si e distribution, rigidity or compressibility of solids under pressure and tendency of particle to flocculate or adhere together. 9) Proportion of solids in the slurry 7 rate at which the filter ca"e is formed, especially in the early stages of filtration. B) Ob0ectives 7 whether the solids or the liquids or both are to be collected. C) Temperature of suspension.

C&NTRIFUBATION
.entrifugation is a unit operation employed for separating the constituents present in dispersion with the aid of centrifugal force. .entrifugal force is used to provide the driving force for the separation. +t replaces gravitation forces in sedimentation. .entrifugation is particularly useful when separation by ordinary filtration is difficult. For e$ample, separating highly viscous mi$tures and colloidal dispersions (particle si e less than C mm), in which difference in densities is less. .entrifugation provides a convenient method of separating either two immiscible liquids or a solid from a liquid. The equipment used for the separation is "nown as centrifuge.

PRINCIPL&# OF C&NTRIFUBATION
The centrifuge consists of essentially a container in which a mi$ture of solid and liquid or two liquids is placed and rotated at high speeds. The mi$ture is separated into its constituent parts by the action of centrifugal force on their densities. ) solid or liquid of higher specific gravity is thrown outward with greater force. Therefore, it is retained at the bottom of the container leaving a clear supernatant layer of pure liquid. The speed of centrifuge is commonly e$pressed in terms of the number of revolutions per minute of the rotor.

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T2&OR) OF C&NTRIFUBATION
+n a colloidal dispersion, the dispersed phase may be either a solid or a liquid. Particles having a si e above C 4m sediment at the bottom due to gravitation force. +n such cases, separation of solids is possible by simple filtration. +f particles are of the order of C 4m or less, they undergo -rownian motion. Dence, they do not sediment under gravity. Therefore, a stronger force, centrifugal force is applied in order to separate them. The sedimentation also depends on the densities of the dispersed phase and dispersion medium. +f the difference in the densities of these phases is less, again separation is difficult. -y applying centrifugal force, it is possible to facilitate (increase the rate of sedimentation) the separation process.

APPLICATION#
%) Production of bul" drugs @) Production of biological products 9) -iopharmaceutical analysis of drugs B) 3valuation of suspensions and emulsions C) ,etermination of molecular weight of colloids.

CLA##IFICATION OF C&NTRIFUB&#
.entrifuges are classified on their mechanisms of separation. A" #&+IM&NTATION C&NTRIFUB&: /edimentation centrifuge is a centrifuge that produces sedimentation of solids based on the difference in the densities of two or more phases of the mi$ture. The efficiency depends on the velocity of rotation to which the mi$ture is sub0ected. 3$amples are hori ontal continuous centrifuge, conical disc centrifuge and supercentrifuge. Iltracentrifugation2 #hen e$tremely fine solid matter is to be separated from a liquid for e$ample in colloidal research, ultracentrifuge is used. +n this instrument, a relatively small rotor is operated at speeds e$ceeding %,&&,&&& revolutions per minute and with forces up to one million times gravity. .entrifiuges have replaced the gravity separators to considerable e$tent in production operations because of their effectiveness in separation. Uses: %) /uspensions containing low concentrations of solids can be separated quic"ly. @) ;anolin is recovered from the wool by scouring process. 9) Olive and fish liver oils are purified by removing dirt and water. B) The liquid(liquid phases are separated in the e$traction of drugs, for e$ample, manufacture of antibiotics. C) -acterial en ymes are prepared by removing bacteria. E) -lood plasma is separated from whole blood. G) /tarch is collected after washing and purification stage.
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H) +n the manufacture of insulin, liquor is clarified so as to remove the precipitated proteins. Ad(antages: %) .entrifuges are compact and occupy very small space. @) The separating efficiency is very high, so that the particles are deposited very rapidly. +t is suitable, if the sediment is a fluid deposit or sludge. 9) Two immiscible liquids are easily separated on a continuous proce. B) -y controlling the speed of rotation and rate of flow, coarse particles are separated, while finer particles remain in the suspension. +isad(antages: %) The construction of sedeimentation centrifuges is complicated. @) +ts capacity is limited.

C" FILTRATION C&NTRIFUB&: Filtration centrifuge is a centrifuge in which solids pass through the porous medium based on difference in the densities of the solid and liquid phases. +n this type the container contains a porous wall through which the liquid phase may pass and on which the solid phase is retained. 3$amples are perforated bas"et centrifuge and semi>continuous centrifuge. The solids that form a porous ca"e can be separated in the filtration centrifuge. Aormally perforated wall is covered with filter medium such as canvas or metal cloth. Uses: %) #hen solid recovery is the primary goal, centrifugation must be considered as an alternative to simple filtration. @) +t is also used for removing unwanted solids from liquid. For e$ample, precipitated proteins are removed from insulin. Ad(antages: %) +t can handle slurries with high proportion of solids and even those having paste li"e consistency. @) The final product has very low moisture content. 9) +n this method the dissolved solids are separated as ca"e. +isad(antages: %) The entire cycle is complicated resulting in considerable labour costs. @) +t is a batch process or semi>continuous type. 9) The solids may form a hard ca"e, due to the centrifugal force, which is difficult to remove.

&@UIPM&NT# IN+U#TRIAL C&NTRIFUBAL FILT&R#

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!" P&RFORAT&+ CA#=&T C&NTRIFUB& Principle: Perforated bas"et (bowl) centrifuge is a filtration centrifuge. The separation is through a perforated wall based on the difference in densities of solid and liquid phases. The bowl contains a perforated side>wall. ,uring centrifugation, the liquid phase passes through the perforated wall, while solid phase is retained in the bowl. The solid is removed after cutting the sediment by a blade after stopping the centrifuge.

Construction:

+t consists of a bas"et, made of steel (sometimes covered with vulcanite or lead) o copper or monel or any other suitable metal. The bas"et material of construction should be such that it offers the greatest resistance to corrosion. The bas"et may have a diameter of &.J& metres and a capacity of &.&HC metre cube. The diameter of perforation should be selected based on the si e of crystals to be separated. +n case, the si e of perforations is bigger than that of particles, a filter cloth is employed. The bas"et is suspended on vertical shaft and is driven by motor using suitable power systems such as belt pulleys, water turbines and electric motors. The bas"et may require about C ?# power for running. /ometimes, steel hoops are used e$ternally to strengthen the bas"et. /urrounding the bas"et, a casing (stationary) is provided which collects the filtrate and discharges it at the outlet. Aor1ing: The material is "ept in the bas"et when the bas"et is stationary. The amount of material should be optimum. Otherwise, during centrifugation it puts a great strain on the bas"et. The loading of material must be done to give even distribution. Power is applied to rotate the bas"et and ma$imum speed must be attained quic"ly. The bas"et runs at %&&& revolutions per minute. The power required for running is small compared to the power required for starting and bringing it to the full speed. ,uring centrifugation, the liquid passes through the perforated wall, while the solid phase retains the bas"et. The liquid leaves the bas"et and is collected at the outlet. The ca"e is then spun to dry as much as possible. /ometimes higher speeds are used so that the ca"e will be completely dried. )fter a definite period of time, the power is turned off. -y applying a bra"e he centrifuge is stopped. The bas"et is brought to rest. The solid ca"e is cut using a blade and then unloaded. Uses: %) +t is e$tensively used for separating crystalline drugs (such as aspirin) from mother liquor. @) it is also used for removing unwanted solids from a liquid. e.g. precipitated proteins are removed from insulin.
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9) /ugar crystals are also separated by this centrifuge. Ad(antages: %) +t is very compact and occupies very little space. @) +t can handle slurries with a high proportion of solids and even those having paste li"e consistency. 9) The final product has very low moisture content. B) The dissolved solids are separated from the ca"e. C) The process is rapid. +isad(antages: %) The entire cycle is complicated resulting in considerable labour costs. @) +t is a batch process. 9) +f the machine is used for prolonged operation, there is considerable wear and tear of the equipment. B) The solids may form hard ca"e due to centrifugal force, which is difficult to simultaneously.

$" #&MI-CONTINUOU# C&NTRIFUB& OR #2ORT C)CL& AUTOMATIC CATC2 C&NTRIFUB& Principle: /emi>continuous centrifuge is a filtration centrifuge. The separation is through a perforated wall based on the difference in the densities of solid and liquid phases. The bowl contains a perforated side>wall. ,uring centrifugation, solid phase is retains in bowl. The solid is washed and removed by cutting the sediment using a blade. +t is a short cycle autaomatic batch centrifuge. Construction:

+t consists of a vertical perforated bas"et, which is supported from a hori ontal shaft driven by a motor. From the open side of the bas"et, provisions are made at the centre to introduce feed and wash pipe through hori ontal tubes. ) feeler (not shown) rides over the feed, which is connected to the diaphragm valve through air supply. The feeler controls the thic"ness of the feed. Dydraulic cylinder attachment is made in such manner that the discharge chute enters from sides of bas"et, when discharge of crystals is desirable.
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Unit Operation-I (PHARM-231)

UNIT-II Filtration & Centrif !ation

Aor1ing: the perforated bas"et is allowed to rotate and slurry is introduced from the side pipe. ,uring centrifugation, the slurry passes through the perforated wall. The solids are retained in the bas"et, while filtrate leaves the bas"et, which is collected at outlet. Further, the ca"e is washed with water. The wash escapes from the bas"et through the filtrate outlet. )fter achieving the desired thic"ness (C& to G& mm), the feeler cuts off the air supply to a diaphragm valve that automatically shuts of the entry of slurry. The hydraulic cylinder is actuated, which lifts the "nife along with the discharge chute. The "nife does not cut the ca"e completely down to the screen, but leaves a layer of crystals that acts as a filter medium for further separation in the ne$t cycle. The residual crystals may be given a brief wash before starting the ne$t cycle. Through a timer and air supply mechanisms, diaphragm controls all the steps. Therefore, the entire cycle is semiautomatic. The discharged crystals may contain @ to B' of moisture.

Ad(antages: This batch centrifuge is used when solids can be drained fast from the bowl. +isad(antages: ,uring discharge, considerable brea"age of crystals is possible. 1any moving parts involved
ma"ing the construction and functioning complicated.

C&NTRIFUBAL #&+IM&NT&R#
!" 2ORIDONTAL CONTINUOU# C&NTRIFUB& Principle: This is a sedimentation centrifuge. The separation is based on the differences in the densities of solid and liquid phases without a porous barrier. #hen slurry is introduced through the shaft of the screw elements in thee conical bowl, sedimentation of solids ta"es place due to centrifugal action. The solids are lifted up by the screw element, while the liquid phase is continuously drained. Construction:

+t consists of cylindrical or conical bowl mounted hori ontally and capable of rotating at C& to EC rps. The bowl has diameter of about &.C meters. #ithin the bowl, a screw conveyer is placed which rotates in the same direction as the bowl, but at slightly slower speed. Aor1ing: the bowl and screw conveyer are allowed to rotate using suitable power supply. The slurry is introduced through the shaft. The liquid moves into the wider portion the bowl. /edimentation of solids ta"es place due to centrifugal action. The solids are lifted by screw elements, while the liquid phase is continuously drained. The solid

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Unit Operation-I (PHARM-231)

UNIT-II Filtration & Centrif !ation

material is carried towards outlet by the conveyer and is discharged continuously. The solids are conveyed to a dry Kbeach= where they get dried. Uses: +t is used when high proportion of solids is present in slurry. Ad(antages: %) +t is very fle$ible in operation. @) +t is capable of handling solids as large as %& to %C mm or as small as a few microns. 9) +t can be used for slurries with concentrations ranging from &.C to C&'.

$" CONICAL +I#C C&NTRIFUB& Principle: +t is a sedimentation centrifuge. The separation is based on the difference in the densities between the phases under the influence of centrifugal force. +n this, a number of cone>shaped plates are attached to a central shaft (which has the provision for feed) at different elevations. ,uring centrifugation, the dense solids are thrown outwards to the underside of the cone shaped casing, while the lighter clarified liquid passes over the bowl and recovered from top of the cone. Construction:

+t consists of a shallow form of bowl containing a series of conical discs attached to the centre shaft at different elevations. The discs are made up of thin sheet of metal or plastic separated by narrow spaces. 1atching holes in the discs about half way between the a$is and the wall of the bowl from channel through which the liquid passes. ) concentric tube is placed surrounding the central drive shaft. Aor1ing: .entrifuge is allowed to rotate. ;ow speed and short time of centrifugation is sufficient to give high degree of clarification. The feed is introduced through the concentric tube surrounding the shaft. The feed flows down and enters into the spaces between the discs (shown by the arrows). ,uring centrifugation, the liquid flows into the channels (holes at the centre of disc) and upward past the discs. These substances move along the surfaces of the discs to the limits of the inner and outer layers. The solids and heavy liquids are thrown outwards and move underside of discs.
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Unit Operation-I (PHARM-231)

UNIT-II Filtration & Centrif !ation

Then the solids deposit at the bottom of the cone, which is removed intermittently. The lighter liquid moves to the upper side of the discs. The liquid rises to the top and escapes from the outlet. Uses: %) Two immiscible liquids can be easily separated by continuous process. 3.g. manufacture of antibiotics. @) /uspensions containing low quantity of solids can be separated quic"ly. 9) /tarch is collected after washing and purification stages. B) +n the manufacture of insulin, the liquor is clarified to remove the precipitated proteins. C) .oncentration of one fluid phase as in separation of cream from mil", concentration of rubber late$, removing solids from lubricating oils, in"s and beverages are possible. Ad(antages: %) .onical disc centrifuges are compact occupying a very small space. @) The separating efficiency is very high, so that the particles are deposited very rapidly. 9) -y controlling speed of rotation the rate of flow, particles are separated into two si e fractions. +isad(antages: %) .onstruction is complicated for cleaning. @) +ts capacity is limited. 9) +t is not suitable for hard ca"e forming sediment of solids. %" #UP&RC&NTRIFUB& Principle: /upercentrifuge is a sedimentation centrifuge. The separation is based on the differences in the densities between two immiscible liquids. .entrifugation is done in the bowl of small centrifuge. ,uring centrifugation, the heavier liquid is thrown against the wall, while the lighter liquid remains as an inner layer. The two layers are simultaneously separated using modified weirs. Construction: +t consists of a long hollow cylindrical bowl of small diameter. +t is suspended from a fle$ible spindle at the top and guided at the bottom by loose>fit bushing. +t can be rotated on its longitudinal a$is. Provision is made at the bottom for the feed inlet using pressure system. Two liquid outlets are provided at the different heights at the top of the bowl, for simultaneous recovery of separated liquids using modified weirs.

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Unit Operation-I (PHARM-231)

UNIT-II Filtration & Centrif !ation

Aor1ing: The centrifuge is allowed to rotate on its longitudinal a$is at a high frequency usually about @&&& rpm with the help of drive>assembly. The feed is introduced from the bottom of the centrifuge using a pressure system. ,uring centrifugation, two liquid phases separate based on difference in their densities. De heavier liquid is thrown against the wall, while lighter liquid forms an inner layer. -oth liquids rise to the top of the vertical bowl. The liquid>liquid interface (neutral one) is maintained by a hydraulic balance. These two layers are simultaneously separately removed from different heights through modified weirs. Thus the supercentrifuge can wor" for continuous separation of immiscible liquid phases.

Uses: +t is used for separating liquid phases of emulsions in foods and pharmaceuticals.

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