2 Centrifugation Celeste l. todaro 1.0 INTRODUCTION The solids-liquid separation process can be accomplished by filtration or centrifugation. Centrifuges magnify the force of gravity to separate phases, solids from liquids or one liquid from another. There are two general types of centrifuges Sedimentation Centrifuges-where a heavy phase settles out from a lighter phase, therefore requiring a density Filtering Centrifuges-where the solid phase is retained by a medium like a filtercloth, for example, that allows the id phase to pass through 2.0 THEORY Centrifuges operate on the principle that a mass spinning about a central axis at a fixed distance is acted upon by a force. The force exerted on any mass is equivalent to the weight of the mass times its acceleration rate in the direction of the force 558
12 Centrifugation Celeste L. Todaro 1.0 INTRODUCTION The solids-liquid separation process can be accomplished by filtration or centrifugation. Centrifuges magnify the force of gravity to separate phases, solids from liquids or one liquid from another. There are two general types of centrifuges: Sedimentation Centrifuges-where a heavy phase settles out from a lighter phase, therefore requiring a density difference and Filtering CentriBges-where the solid phase is retained by a medium like a filtercloth, for example, that allows the liquid phase to pass through. 2.0 THEORY Centrifuges operate on the principle that a mass spinning about a central axis at a fixed distance is acted upon by a force. The force exerted on any mass is equivalent to the weight of the mass times its acceleration rate in the direction of the force. 558
Centrifugation 559 Eq(1) m- mass a acceleration rate This acceleration rate is zero without a force acting upon it, however it will retain a certain velocity, v. If forced to move in a circular path, a vector velocity v/r exists as its direction is continually changing a= centrifugal acceleration Eq1(3) v= velocit w= angular velocity Should a mass be rotated within a cylinder, the resulting force at the cylinder wall is called a centrifugal force, F F=mw2?r this is away from the center of rotation. The equal and opposite force Eq,(5) is the centripetal force. This is the force required to keep the mass on its circular path Ifa cylindrical bowl holding a slurry is left to stand, the solids will settle out under the force of l g or gravity. By spinning the bowl the solids will settle under the influence of the centrifugal force generated as well as the force of gravity which is now negligible. Solids will collect at the wall with a liquid layer on top. This is an example of a sedimentation in a solid bowl syster
Centrifugation 559 F=ma m = mass a = acceleration rate F = force This acceleration rate is zero without a force acting upon it, however, it will retain a certain velocity, v. If forced to move in a circular path, a vector velocity v/r exists as its direction is continually changing. where a, = centrifugal acceleration v = velocity r = radius w = angular velocity Should a mass be rotated within a cylinder, the resulting force at the cylinder wall is called a centrifugal force, F,. Eq. (4) F, = mw2r this is away from the center of rotation. The equal and opposite force: is the centripetal force. This is the force required to keep the mass on its circular path. Ifa cylindrical bowl holding a slurry is left to stand, the solids will settle out under the force of 1 g orgravity. By spinning the bowl the solids will settle under the influence of the centrifugal force generated as well as the force of gravity which is now negligible. Solids will collect at the wall with a liquid layer on top. This is an example of a sedimentation in a solid bowl system
560 Fermentation and Biochemical engineering Handbook By perforating the bowl or basket and placing a filtercloth on the inside wall, one has now modeled a filtering centrifuge similar in principle to an ordinary household washing machine This amplification of the force of gravity is commonly referred to as the number of gs. The centrifugal acceleration(a )referenced to g is w2r/g ven e equation Eq(6) Relative Centrifugal Force(G)=1.42 x 10-5n2D where n= speed in revolutions/minute D,= diameter of the bowl in inches The driving force for separation is a function of the square of the rotational speed and the diameter of the bowl; however, there are restrictions in the design of centrifuges that will limit these variables An empty rotating centrifuge will exhibit a stress in the bowl called a elf-stress, S where w= angular velocity r= radius of the bowl Pm= density of the bowl material The contents of the bowl also generate a stress or pressure on the inner wall of the bowl. Assuming the radius of the bowl (r)is equal to the outer radius of the bowl contents(r2), we have Eq(8) S=w22(r2-n12)c/r where Pc=density of contents of the bowl r1=inner radius of the bowl contents(solids and liquid) r2=outer radius of the bowl contents(solids and liquid
560 Fermentation and Biochemical Engineering Handbook By perforating the bowl or basket and placing a filtercloth on the inside wall, one has now modeled a filtering centrifuge similar in principle to an ordinary household washing machine. This amplification ofthe force ofgravity is commonly referred to as the number of g's. The centrifugal acceleration (a,) referenced to g is w2r/g which is given by the equation: Relative Centrifugal Force (G) = 1.42 x n2 Di n = speed in revolutions/minutes Di = diameter of the bowl in inches The L.iving force for separation is a function of the square oL the rotational speed and the diameter of the bowl; however, there are restrictions in the design of centrifuges that will limit these variables. An empty rotating centrifuge will exhibit a stress in the bowl called a self-tress, S, . where w = angular velocity ri = radius of the bowl pm = density of the bowl material The contents of the bowl also generate a stress or pressure on the inner wall of the bowl. Assuming the radius of the bowl (ri) is equal to the outer radius of the bowl contents (r2), we have where t = thickness of the bowl p, = density of contents of the bowl r1 = inner radius of the bowl contents (solids and liquid) r2 =outer radius of the bowl contents (solids and liquid)
561 The total stress in the bowl wall is Sr=s+S 2-1 with D,= 2r, and in common units Eq,(9) Sr=41×0n2DD Centrifuges are designed such that S, is 45 to 65% of ST ST P lb/ft) Increasing the bowl speed and its diameter increases the g force, but also increases the self stress and the stress induced by the process bowl. The design is, therefore, really limited by the material of construction available, however, for a given bowl stress, the centrifugal acceleration is an inverse function of bowl diameter. For example, doubling the rotational speed and halving the bowl diameter, doubles the acceleration while keeping the total stress relatively constant. It is for this reason that the smallest diameter centrifuges operate at the highest g forces. Tubular centrifuges operate at 2-5 inches diameter withg forces over 60,000. Disk centrifuges operate at 7-24 inches at 14,000 to 5500 gs, while continuous decanter centrifuges with helical conveyors are designed with bowl diameters of 6-54 inches and g forces of 5, 500-770 gs. Filtering centrifuges with diameters of 12 to 108 inches have corresponding g forces of 2000 to 260 3.0 EQUIPMENT SELECTION pon review of Table l, it is evident that there are several types of equipment that can be used for the same application. There are also many
Centrifugation 561 The total stress in the bowl wall is: with Di = 2ri and in common units: Eq. (9) Centrifbges are designed such that S, is 45 to 65% of &. Increasing the bowl speed and its diameter increases the g force, but also increases the self stress and the stress induced by the process bowl. The design is, therefore, really limited by the material of construction available, however, for a given bowl stress, the centrifugal acceleration is an inverse function of bowl diameter. For example, doubling the rotational speed, and halving the bowl diameter, doubles the acceleration while keeping the total stress relatively constant. It is for this reason that the smallest diameter centrifuges operate at the highest g forces. Tubular centrifuges operate at 2-5 inches diameter withg forces over 60,000. Disk centrifuges operate at 7-24 inches at 14,000 to 5500 g’s, while continuous decanter centrifuges with helical conveyors are designed with bowl diameters of 6-54 inches and g forces of 5,500-770 g’s. Filtering centrifuges with diameters of 12 to 108 inches have corresponding g forces of 2000 to 260. 3.0 EQUIPMENT SELECTION Upon review of Table 1, it is evident that there are several types of equipment that can be used for the same application. There are also many
562 Fermentation and Biochemical Engineering Handbook equipment vendors that can be consulted. In consulting with vendors to narrow the choices, proprietary information may be divulged regarding the nature of one's process. Be sure to sign a secrecy agreement to protect all confidential information Table 1. Product Recovery Fermentation FERMENTER ROTARY VACUUM NTER MEMBRANE DRUM FILTER BOWL OR FILTRATION (LIQUID τH一2 OLVENT CARBON XTRACTION EXCHANGE ABSORP TION WASTE CRYSTALLIZATION OR(SMALL SCALEOREVAPORATOR PRODUCT OR CENTRIFUGE OR PEELER FILTER CENTRIFUGE FILTER DIRECT NDIRECT DRYER DRYER PRODUCT
562 Fermentation and Biochemical Engineering Handbook equipment vendors that can be consulted. In consulting with vendors to narrow the choices, proprietary information may be divulged regarding the nature of one’s process. Be sure to sign a secrecy agreement to protect all confidential information. Table 1. Product Recovery Fermentation DRUM FILTER CENTRIFUGE FILTRATION INCINERATED (LIQUID) OR ANIMAL (WASTE) FEEDSTOCK EXTRACTION EXCHANGE ABSORPTION 11- WASTE I LIQUID PRODUCT SOLIDS-LIQUID LIQUID-LIQUID CHROMATOGRAPHY -1 CRYSTALLIZATION OR [TIORFl (SMALL SCALE HIGH PURITY PRODUCT dk 1 OR FI OR F] I FILTER DRY FINAL
Centrifugation 563 3. 1 Pilot Testing Preliminary data taken in the laboratory regarding the separation characteristics of a product can be beneficial when beginning the equipment selection process. If one is retrofitting an existing unit with an identical system, it will not be as complex and time consuming as designing a"grass oots" facility. Pland data can then be helpful. however, should the process be altered one should evaluate the effect on centrifugation Careful attention should be taken to ensure that the existing tank design, peripheral pumps, piping and agitators do not provide shear that will cause particle degradation. Capital dollars spent in this area on crystall tion studies, the selection of the correct pumps, etc, will directly impact the capacity of your equipment as particle degradation will significantly affect throughput and final residual moisture adversely, as it does filtration.( See Ch. 8 for a more detailed discussion If a process is existing and in-plant expertise is available to optimize the equipment, it would be advisable to do so before a purchase. Upon review of the existing design, sufficient improvements can often be made in an older piece of equipment thereby avoiding a more costly investment. Vendors usually offer this type of assistance at no charge from their office or at a daily rate in the field 3.2 Data Collection The first step collect pertinent information to the process including a process flow sheet, product information and completion of a typical questionnaire, as shown in Table 2 Knowledge of the most critical aspect of the process can guide the sometimes difficult selection process. For example, the requirement of a very dry product with strict impurity levels suggests a filtering centrifuge. A product with a feed rate of 150 gpm, without wash requirements, would lead us to a continuous sedimentation centrifuge A simple Buchner funnel test will indicate fast, medium or slow filtration. Slow filtering materials that have inordinate quantities of particles passing the filter paper will be submicron and difficult to capture in a filtering system. Therefore, a sedimentation centrifuge should be considered A phenomenon called"cake cracking" can occur and will be evident in this simple test. Not all materials exhibit this. It depends upon the surface tension of the product and its tendency to shrink as dewatering occurs Amorphous, thixotropic materials will exhibit this more than rigid solids
Centrifugation 563 3.1 Pilot Testing Preliminary data taken in the laboratory regarding the separation characteristics of a product can be beneficial when beginning the equipment selection process. If one is retrofitting an existing unit with an identical system, it will not be as complex and time consuming as designing a “grass roots” facility. Pland data can then be helpful. However, should the process be altered, one should evaluate the effect on centrifugation. Careful attention should be taken to ensure that the existing tank design, peripheral pumps, piping and agitators do not provide shear that will cause particle degradation. Capital dollars spent in this area on crystallization studies, the selection of the correct pumps, etc., will directly impact the capacity of your equipment as particle degradation will significantly affect throughput and final residual moisture adversely, as it does filtration. (See Ch. 8 for a more detailed discussion.) If a process is existing and in-plant expertise is available to optimize the equipment, it would be advisable to do so before a purchase. Upon review of the existing design, sufficient improvements can often be made in an older piece of equipment thereby avoiding a more costly investment. Vendors usually offer this type of assistance at no charge from their office or at a daily rate in the field. 3.2 Data Collection The first step is to collect pertinent information to the process, including a process flow sheet, product information and completion of a typical questionnaire, as shown in Table 2. Knowledge of the most critical aspect of the process can guide the sometimes difficult selection process. For example, the requirement ofa very dry product with strict impurity levels suggests a filtering Centrifuge. A product with a feed rate of 150 gpm, without wash requirements, would lead us to a continuous sedimentation centrifuge. A simple Buchner funnel test will indicate fast, medium or slow filtration. Slow filtering materials that have inordinate quantities of particles passing the filter paper will be submicron and difficult to capture in a filtering system. Therefore, a sedimentation centrifuge should be considered. A phenomenon called “cake cracking” can occur and will be evident in this simple test. Not all materials exhibit this. It depends upon the surface tension of the product and its tendency to shrink as dewatering occurs. Amorphous, thixotropic materials will exhibit this more than rigid solids
564 Fermentation and Biochemical Engineering Handbook Table 2. Product Questionnaire: Centrifuges, Filter Press. (Courtesy Heinkel Filtering Systems Inc) SEPARATION PROBLF 如日〓日s日日 日 日〓日=日 日"日 wala drived des thenad poem
564 Fermentation and Biochemical Engineering Handbook Table 2. Product Questionnaire: Centrifbges, Filter Press. (Courtesy Heinkel Filtering Systems Inc.)
Centrifugation 565 If the cake cracks, a liquid level must be maintained on top of the cake before washing to prevent channeling of the wash liquors. a crude estimate of the wash ratio, gallons of wash per pound of dry cake, can also be made in the laboratory The filter cake developed on a buchner funnel will have certain characteristics; the product may appear to have a defined crystal structure or be more amorphous. Microscope studies will indicate the shape of particles, which will be helpful in trial runs. Needle crystals, for example may break easily at high filling speeds, and during discharge on a basket centrifuge with plough platelets tend to pack in compressible beds and may be better suited to sedimentation than filtration. A particle size distribution will help in this analysis and is also required for cloth selection. (See Ch. 6) Cake compressibility is the ability of a cake to reduce its volume, i.e porosity, when stress is applied. The resulting cake will display an increase hydraulic resistance. This is not necessarily caused by an average change in porosity, as a porosity gradient can occur by the redistribution of the solid material. Rigid granular particles tend to be incompressible and filter well even with thick cakes. Materials that are easily deformed such as amorphous or thixotropic materials will respond well to mechanical pressureor operation with thin cakes. ( See Ch. 6 on Cake Compressibility. Laboratory test tube centrifuges can determine if there is a sufficient density difference between the two phases to consider sedimentation as an alternative. If there is a sharp separation, one can anticipate the same in the field. One can also answer the following questions. Do the solids settle or float? Is the solid phase granular or amorphous? What is the moisture content? The characteristics of the solids indicate the solids discharge design required, i.e., scroll in decanters, or in disk centrifuges, flow-through nozzles or wall valves A laboratory centrifuge such as the Beaker design( Heinkel) can also simulate the operation of a filtering centrifuge and verify product character istics, filtration rates and wash requirements. various filter cloths can also be tried only one liter sampl With these data summarized, one can now discuss the application with vendors or consultants with expertise in centrifuge operations to help simplify the selection process. Pilot plant testing can be done with 10-25 gallons at the vendor's facility or with a rental unit for an in-plant trial. Ifsufficient material is available, semiwork tests are recommended as more data can be taken for scaleup. Equipment manufacturers should be questioned about how they are scaling up, whether it is based upon volume, filtercloth area, etc and what accuracy can be expected. Critical to a trials success is how representative
Centrifugation 565 If the cake cracks, a liquid level must be maintained on top of the cake before washing to prevent channeling of the wash liquors. A crude estimate of the wash ratio, gallons of wash per pound of dry cake, can also be made in the laboratory. The filter cake developed on a Buchner funnel will have certain characteristics; the product may appear to have a defined crystal structure or be more amorphous. Microscope studies will indicate the shape ofparticles, which will be helpful in trial runs. Needle crystals, for example, may break easily at high filling speeds, and during discharge on a basket centrifuge with plough platelets tend to pack in compressible beds and may be better suited to sedimentation than filtration. A particle size distribution will help in this analysis and is also required for cloth selection. (See Ch. 6.) Cake compressibility is the ability of a cake to reduce its volume, Le., porosity, when stress is applied. The resulting cake will display an increase in hydraulic resistance. This is not necessarily caused by an average change in porosity, as a porosity gradient can occur by the redistribution of the solid material. Rigid granular particles tend to be incompressible and filter well even with thick cakes. Materials that are easily deformed such as amorphous or thixotropic materials will respond well to mechanical pressure or operation with thin cakes. (See Ch. 6 on Cake Compressibility.) Laboratory test tube centrifiges can determine if there is a sufficient density difference between the two phases to consider sedimentation as an alternative. If there is a sharp separation, one can anticipate the same in the field. One can also answer the following questions. Do the solids settle or float? Is the solid phase granular or amorphous? What is the moisture content? The characteristics ofthe solids indicate the solids discharge design required, i.e., scroll in decanters, or in disk centrifuges, flow-through nozzles or wall valves. A laboratory centrifige such as the Beaker design (Heinkel) can also simulate the operation of a filtering centrifuge and verify product characteristics, filtration rates and wash requirements. Various filter cloths can also be tried using only one liter samples. With these data summarized, one can now discuss the application with vendors or consultants with expertise in centrifuge operations to help simplify the selection process. Pilot plant testing can be done with 10-25 gallons at the vendor’s facility or with a rental unit for an in-plant trial. If sufficient material is available, semiworks tests are recommended as more data can be taken for scaleup. Equipment manufacturers should be questioned about how they are scaling up, whether it is based upon volume, filtercloth area, etc., and what accuracy can be expected. Critical to a trial’s success is how representative
566 Fermentation and Biochemical Engineering Handbook a slurry sample is. This is especially important with fermentation processes that change over timeand in-plant trial of reasonable scale may bemandatory There can be clear advantages to using a centrifuge over a filter, such as a drier product or a more effective separation. This will be dependent upon the application. However, there can be applications where a nutsche or even several types of centrifuges appear, from small scale testing, to yield similar product quality results. Ultimately, the decision will depend upon"operabil ity, that is installation, maintenance, and day-to-day operation. For these purposes, it is strongly recommended that the plant invest the time and relatively small capital costs for a rental unit to run an in-plant test on the product. Production scale rental units can be operated by taking a side stream from an existing process. This facilitates comparisons of the new equipment to existing plant operations. Rental cost for one month will be approximately three percent of the purchase price of the test equipment, credit for part of the rental is usually offered against the purchase of a production unit. Rental periods may be limited, however lease options are available 3.3 Materials of Construction Various materials are available as with all process equipment, ranging from carbon steel coated with rubber, Halar or Kynar, to stainless steel 304 316 and higher grades, or more expensive alloys such as titanium, Hastelloy C-22, C276, or C4. These grades of Hastelloy will, however, double the capital outlays Coatings should be avoided if possible as product"A "can diffuse into the surface and potentially reverse its path. It therefore has the potential to contaminate product"B. Being permeable, they are also subject to peeling Coatings can be used most effectively on stationary parts dedicated to liquid use that are therefore, not exposed to maintenance tools, etc Working with an existing process will provide the most reliable data for choosing the most economical material for the service required. a new process may require a corrosion study by an in-plant metallurgist, if questionable. Test coupons are a relatively inexpensive way to conduct testing on a small scale and can be obtained from equipment vendors or from the materials manufacturers themselves. Companies such as Haynes, Allegheny, etc, will also have descriptions of the suitability of thei different alloys for various processes. An overview of corrosion testing and materials is presented in Perry's Chemical Engineer's Handbook, Sixth Edition. Sec. 23
566 Fermentation and Biochemical Engineering Handbook a slurry sample is. This is especially important with fermentation processes that change over time and in-plant trial of reasonable scale may be mandatory. There can be clear advantages to using a centrifbge over a filter, such as a drier product or amore effective separation. This will be dependent upon the application. However, there can be applications where a nutsche or even several types of centrifbges appear, from small scale testing, to yield similar product quality results. Ultimately, the decision will depend upon “operability,” that is installation, maintenance, and day-today operation. For these purposes, it is strongly recommended that the plant invest the time and relatively small capital costs for a rental unit to run an in-plant test on the product. Production scale rental units can be operated by taking a side stream from an existing process. This facilitates comparisons ofthe new equipment to existing plant operations. Rental cost for one month will be approximately three percent of the purchase price of the test equipment, credit for part of the rental is usually offered against the purchase of a production unit. Rental periods may be limited, however lease options are available. 3.3 Materials of Construction Various materials are available as with all process equipment, ranging from carbon steel coated with rubber, Halar or Kynar, to stainless steel 304, 3 16 and higher grades, or more expensive alloys such as titanium, Hastelloy C-22, C276, or C4. These grades of Hastelloy will, however, double the capital outlays. Coatings should be avoided if possible as product “A” can diffuse into the surface and potentially reverse its path. It therefore has the potential to contaminate product “B.” Being permeable, they are also subject to peeling. Coatings can be used most effectively on stationary parts dedicated to liquid use that are, therefore, not exposed to maintenance tools, etc. Working with an existing process will provide the most reliable data for choosing the most economical material for the service required. A new process may require a corrosion study by an in-plant metallurgist, if questionable. Test coupons are a relatively inexpensive way to conduct testing on a small scale and can be obtained from equipment vendors or from the materials manufacturers themselves. Companies such as Haynes, Allegheny, etc., will also have descriptions of the suitability oftheir different alloys for various processes. An overview of corrosion testing and materials is presented in Perry S Chemical Engineer s Handbook, Sixth Edition, Sec. 23
Centrifugation 567 4.0 COMPONENTS OF THE CENTRIFUGE Centrifuges consist of the following components Rotor(bowl or basket) that rotates and contains the Solids discharge unloading system, plough, scroll, inverting basket, nozzle system, etc Drive system to rotate the bowl including main bear ing shaft with seals, etc and motor for electric or hydraulic operation Enclosure to contain rotor 5.0 SEDIMENTATION CENTRIFUGES Sedimentation centrifuges are commonly known as solid bowl sys tems, i.e., perforated bowls that are used to separate materials such as cream frommilk, sludges from water in waste water treatment plants, and, ofcourse, the biotechnology materials The basic principle of sedimentation is that a fluid consisting of two or more phases is subjected to a centrifugal-force field As the heavier phase travels away from the axis of rotation, there is an ever increasing centrifugal force. The centrifuge increases the settling rate to clarify one phase, while simultaneously concentrating the other(usually solids). There is no flow of liquid througha cake, hence difficult filtrations are typical applications. He quickly phases separate will depend upon many factors. Capacities and performance are dictated by the particle size, distribution, solids concentra tion, and particle shape. Adjustments for these changing factors can be achieved only through experiment, testing the particular application with its 6.0 TUBULAR-BOWL CENTRIFUGES Used often in the laboratory, this unit is limited to 4.5 kgs. of solids loading with an estimated 10-15 gallons/hour liquid feed rate. Applications include stripping small bacteria or viruses from a culture medium
Centrifugation 567 4.0 COMPONENTS OF THE CENTRIFUGE Centrifuges consist of the following components: - Rotor (bowl or basket) that rotates and contains the product Solids discharge unloading system, plough, scroll, inverting basket, nozzle system, etc. Drive system to rotate the bowl including main bearing shaft with seals, etc., and motor for electric or hydraulic operation - Frame to support unit - Enclosure to contain rotor - - 5.0 SEDIMENTATION CENTRIFUGES Sedimentation centrijkges are commonly known as solid bowl systems, i.e., perforated bowls that are used to separate materials such as cream frommilk, sludges from water in waste water treatmentplants, and, ofcourse, the biotechnology materials. The basic principle of sedimentation is that a fluid consisting of two or more phases is subjected to a centrifugal-force field. As the heavier phase travels away from the axis of rotation, there is an ever increasing centrifugal force. The centrifuge increases the settling rate to clarify one phase, while simultaneously concentrating the other (usually solids). There is no flow of liquid through a cake, hence difficult filtrations are typical applications. How quickly phases separate will depend upon many factors. Capacities and performance are dictated by the particle size, distribution, solids concentration, and particle shape. Adjustments for these changing factors can be achieved only through experiment, testing the particular application with its deviations. 6.0 TUBULAR-BOWL CENTRIFUGES Used often in the laboratory, this unit is limited to 4.5 kgs. of solids loading with an estimated 10-15 gallonshour liquid feed rate. Applications include stripping small bacteria or viruses from a culture medium