Filtration vacuum filters

Cold filter plugging point EN 116 (NF M 07-042) Vacuum filtration through a calibrated filter... 

It will be a little tricky but one can also try to purify by freezing I The sassafras oil is thrown into the freezer to chill. Safrole itself freezes at -14°C so anything that starts to freeze prior to that can be cold filtered in a prechilled vacuum filtration setup. The filtrate goes back in the freezer until -14°C is reached and the mother lode of safrole freezes up. This again is filtered cold but this time the frozen mass of safrole crystals are washed with some ice cold methanol or ethanol (preferably at -14°C) to wash away the unfrozen high-boiling constituents. 

After 12-24 hours of reflux the reaction is, for the most part, complete. The reaction mix will be a dark brown. So what does one do about all those brown particles and junk. Well, usually there aren t any. The solution should be uniformly dark. If any solids can be seen it means that they are insoluble in ethanol and can be removed from solution by gravity or vacuum filtration through a coffee filter or some paper towels. If it takes a day to drip through the filter then so-be-it. The ethanol with its payload of isosafrole will... 

The soiution is aliowed to cool and the crystals of the P2P-bisulfite addition compound are then separated by vacuum filtration, washed with a little clean dH20 then washed with a couple hundred mLs of ether, DCM or benzene. The filter cake of MD-P2P-bisulfate is processed by scraping the crystals into a flask and then 300mL of either 20% sodium carbonate solution or 10% HCi soiution are added (HCI works best). The soiution is stirred for another 30 minutes during which time the MD-P2P-bisulfite complex will be busted up and the P2P will return to its happy oil form. The P2P is then taken up with ether, dried and removed of the solvent to give pure MD-P2P. Whaddya think of that ... 

After 3 hours the stirring is stopped and the solution allowed to settle. By this time just about all the foil will have turned to dust, which is going to make the next step of vacuum filtration very difficult because it will plug up the filter paper in a second. So the chemist lets it settle, then pours off the liquid through the vacuum filtration setup (see methodology section). The flask is rinsed with lOOmL methanol, the methanol poured through the grey filter cake and the filter cake discarded. All of the filtrate is placed in a flask and vacuum distilled to remove all the methanol, isopropyl alcohol and water which will leave the chemist with oil and junk in the bottom of the flask. 

The way the chemist knows that she has methylamine and not ammonium chloride is that she compares the look of the two types of crystals. Ammonium chloride crystals that come from this reaction are white, tiny and fuzzy. The methylamine hydrochloride crystals are longer, more crystalline in nature and are a lot more sparkly. The chemist leaves the methylamine crystals in the Buchner funnel of the vacuum filtration apparatus and returns the filtrate to the distillation set up so it can be reduced one last time to afford a second crop. The combined methylamine hydrochloride filter cake is washed with a little chloroform, scraped into a beaker of hot ethanol and chilled. The methylamine hydrochloride that recrystallizes in the cold ethanol is vacuum filtered to afford clean, happy product (yield=50%). 

Sterile Filtration of Gases. Primary appHcations for sterile gas filtration are the sterilization of fermentor inlet air, fermentor vent gas, vents on water for injection tanks, and vacuum break filters during lyophilization. Operational and process considerations apply. Typically, the membrane in gas... 

The polymer can easily be recovered by simple vacuum filtration or centrifugation of the polymer slurry. This can be followed by direct conversion of the filter cake to dope by slurrying the filter cake in chilled solvent and then passing the slurry through a heat exchanger to form the spinning solution and a thin-film evaporator to remove residual monomer. 

Eor most industrial inorganic sohds such as minerals etc, the increase in with Ap is not too great, and thus should the material to be filtered be too fine for vacuum filtration, pressure filtration may be advantageous and give better rates. 

Pressure filters can treat feeds with concentrations up to and in excess of 10% sohds by weight and having large proportions of difficult-to-handle fine particles. Typically, slurries in which the sohd particles contain 10% greater than 10 ]lni may require pressure filtration, but increasing the proportion greater than 10 ]lni may make vacuum filtration possible. The range of typical filtration velocities in pressure filters is from 0.025 to 5 m/h and dry sohds rates from 25 to 250 kg nY/h. The use of pressure filters may also in some cases, such as in filtration of coal flotation concentrates, eliminate the need for flocculation. 

In vacuum filters, the driving force for filtration results from the appHcation of a suction on the filtrate side of the medium. Although the theoretical pressure drop available for vacuum filtration is 100 kPa, in practice it is often limited to 70 or 80 kPa. 

Total submergence is used in the vacuum disk filter thickener (Eig. 13) in which the cake discharge, by backwashing with filtrate, occurs as each sector passes through the lowest point of the slurry tank. 

Most continuous pressure filters available (ca 1993) have their roots in vacuum filtration technology. A rotary dmm or rotary disk vacuum filter can be adapted to pressure by enclosing it in a pressure cover however, the disadvantages of this measure are evident. The enclosure is a pressure vessel which is heavy and expensive, the progress of filtration cannot be watched, and the removal of the cake from the vessel is difficult. Other complications of this method are caused by the necessity of arranging for two or more differential pressures between the inside and outside of the filter, which requires a troublesome system of pressure regulating valves. 

There are many technical problems to be considered when developing a new commercial and viable filter. However, the filtration hardware in itself is not enough, as the control of a continuous pressure filter is much more difficult than that of its equivalents in vacuum filtration the necessary development may also include an automatic, computerized control system. This moves pressure filtration from low to medium or even high technology. Disk Filters. 

Drum Filters. The rotary dmm filter, also borrowed from vacuum filtration, makes relatively poor use of the space available in the pressure vessel, and the filtration areas and capacities of such filters cannot possibly match those of the disk pressure filters. In spite of this disadvantage, however, the pressure dmm filter has been extensively developed. 

The so-called hyperbar vacuum filtration is a combination of vacuum and pressure filtration in a pull—push arrangement, whereby a vacuum pump of a fan generates vacuum downstream of the filter medium, while a compressor maintains higher-than-atmospheric pressure upstream. If, for example, the vacuum produced is 80 kPa, ie, absolute pressure of 20 kPa, and the absolute pressure before the filter is 150 kPa, the total pressure drop of 130 kPa is created across the filter medium. This is a new idea in principle but in practice requires three primary movers a Hquid pump to pump in the suspension, a vacuum pump to produce the vacuum, and a compressor to supply the compressed air. The cost of having to provide, install, and maintain one additional primary mover has deterred the development of hyperbar vacuum filtration only Andrit2 in Austria offers a system commercially. 

The ammonium sulfate and sodium chloride are simultaneously dissolved, preferably ia a heel of ammonium chloride solution. The sodium chloride is typically ia excess of about 5%. The pasty mixture is kept hot and agitated vigorously. When the mixture is separated by vacuum filtration, the filter and all connections are heated to avoid cmst formation. The crystalline sodium sulfate is washed to remove essentially all of the ammonium chloride and the washings recycled to the process. The ammonium chloride filtrate is transferred to acid resistant crystallising pans, concentrated, and cooled to effect crystallisation. The crystalline NH Cl is washed with water to remove sulfate and dried to yield a product of high purity. No attempt is made to recover ammonium chloride remaining ia solution. The mother Hquor remaining after crystallisation is reused as a heel. 

Caustic soda is removed from the carbonate—bicarbonate solution by treating with a slight excess of hard-burned quicklime (or slaked lime) at 85—90°C in a stirred reactor. The regenerated caustic soda is separated from the calcium carbonate precipitate (lime mud) by centrifuging or rotary vacuum filtration. The lime mud retains 30—35% Hquid and, to avoid loss of caustic soda, must be weU-washed on the filter or centrifuge. Finally, the recovered caustic solution is adjusted to the 10% level for recycle by the addition of 40% makeup caustic soda. 

It is known that the specific resistance for centrifuge cake, especially for compressible cake, is greater than that of the pressure or vacuum filter. Therefore, the specific resistance has to be measured from centrifuge tests for different cake thicknesses so as to scale up accurately for centrifuge performance. It cannot be extrapolated from pressure and vacuum filtration data. For cake thickness that is much smaller compared to the basket radius, Eq. (18-116 7) can be approximated by... 

When the space above the suspension is subjected to compressed gas or the space under the filter plate is under a vacuum, filtration proceeds under a constant pressure differential (the pressure in the receivers is constant). The rate of filtration decreases due to an increase in the cake thickness and, consequently, flow resistance. A similar filtration process results from a pressure difference due to the hydrostatic pressure of a suspension layer of constant thickness located over the filter medium. 

After thickening, a variety of sludge handling and disposal options are available. For example, the thickened sludge can be applied directly to land. If liquid disposal is not applicable to a specific project, the thickened sludge can be dewatered by centrifugation, vacuum filtration, or filter pressing. The dewatered residue can then be land fill or incinerated. These options are discussed further on. 

Cultures of G. polyedra (L. polyedrum) are grown at 20 5°C in a supplemented sea water medium (Hastings and Sweeney, 1957 Hastings and Dunlap, 1986), under cool-white fluorescent lighting of a 12-hr light/12-hr dark cycle. The cultures are inoculated at densities of 100 to 500 cells/ml. After 2-4 weeks, cells are harvested by vacuum filtration on a filter paper at cell densities of 7,000-15,000 cells/ml, yielding 0.3-0.7 g wet cells per liter of culture. 

A fermentation broth containing Streptomyces kanamyceticus cells is filtered by a vacuum rotary filter. The feed rate is 120kg h1 each kilogram of broth contains 60g of cells. To improve filtration, filter aids are added at a rate of 10kg-h. The concentration of kanamycin in the broth is 0.05%. The filtrate is collected at a rate of 112 kg h. The concentration of kanamycin in the filtrate is 0.045%. The filter cake contains cells, and filter aid is continuously removed from the filter cloth. 

The filtering operation can also be conveniently done in a high-quality nitrogen atmosphere dry box by vacuum filtration through a 90-mm., 60-ml., medium-porosity fritted-disk Buchner funnel. 

The precipitate is collected on filter paper (Note 7) in a Buchner funnel by vacuum filtration and is washed with 100 ml. of absolute ethanol. The solid is slurried in three 75-ml. portions of distilled water (Note 8), 100 ml. of absolute ethanol, two 100-ml. portions of reagent-grade acetone, and two 100-ml. portions of anhydrous ethyl ether. The filter cake is pressed dry in the funnel with suction by means of a piece of rubber dam, transferred to a tared, 500-ml., round-bottomed flask, and dried under reduced pressure (0.01 mm.) at room temperature for 24 hours (Note 9). The weight of the dry silver salt of succinimide is 51-54 g. (88-94%). 

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