Filter, calcium carbonate

Place 45 g. (43 ml.) of benzal chloride (Section IV,22), 250 ml. of water and 75 g. of precipitated calcium carbonate (1) in a 500 ml. round-bottomed flask fltted with a reflux condenser, and heat the mixture for 4 hours in an oil bath maintained at 130°. It is advantageous to pass a current of carbon dioxide through the apparatus. Filter off the calcium salts, and distil the filtrate in steam (Fig. II, 40, 1) until no more oil passes over (2). Separate the benzaldehyde from the steam distillate by two extractions with small volumes of ether, distil off most of the ether on a water bath, and transfer the residual benzaldehyde to a wide-mouthed bottle or flask. Add excess of a concentrated solution of sodium bisulphite in portions with stirring or shaking stopper the vessel and shake vigorously until the odour of benzaldehyde can no longer be detected. Filter the paste of the benzaldehyde bisulphite compound at the pump... 

Rotary kilns and, to a lesser extent, Fluo-SoHds kilns are used to calcine a wet precipitated calcium carbonate filter cake in the kraft or sulfate paper-pulp process (15). Lime is regenerated for use as a causticization reagent in recovering caustic soda for pulp digestion. Losses in lime recovery are replaced by purchased lime (see Paper Pulp). 

Naphthalenesulfonic Acid. The sulfonation of naphthalene with excess 96 wt % sulfuric acid at < 80°C gives > 85 wt % 1-naphthalenesulfonic acid (a-acid) the balance is mainly the 2-isomer (P-acid). An older German commercial process is based on the reaction of naphthalene with 96 wt % sulfuric acid at 20—50°C (13). The product can be used unpurifted to make dyestuff intermediates by nitration or can be sulfonated further. The sodium salt of 1-naphthalenesulfonic acid is required, for example, for the conversion of 1-naphthalenol (1-naphthol) by caustic fusion. In this case, the excess sulfuric acid first is separated by the addition of lime and is filtered to remove the insoluble calcium sulfate the filtrate is treated with sodium carbonate to precipitate calcium carbonate and leave the sodium l-naphthalenesulfonate/7J(9-/4-J7 in solution. The dry salt then is recovered, typically, by spray-drying the solution. 

Excess calcium hydroxide is precipitated by usiag carbon dioxide and the calcium carbonate, calcium hydroxide, and calcium phosphite are removed by filtration. The filtered solution is treated with an equivalent amount of sodium sulfate or sodium carbonate to precipitate calcium sulfate or carbonate. Sodium hypophosphite monohydrate [10039-56-2] is recovered upon concentration of the solution. Phosphinic acid is produced from the sodium salt by ion exchange (qv). The acid is sold as a 50 wt %, 30—32 wt %, or 10 wt % solution. The 30—32 wt % solution is sold as USP grade (Table 12) (63). Phosphinic acid and its salts are strong reduciag agents, especially ia alkaline solution (65). 

The white Hquor is separated from the calcium carbonate by decantation in a clarifier and is then available for a new cooking cycle. The underflow from the clarifier, which contains the calcium carbonate and is referred to as lime mud, is diluted with water and passed to a second clarifier known as the lime mud washer. The clarified weak white Hquor (weak wash) goes to storage and then enters the dissolving tank. The lime mud residue from the lime mud washer is passed to a rotary filter and subsequently to the lime kiln where calcium carbonate is converted back to calcium oxide, thus completing the lime cycle. 

Filtration. Any type of clarification is foUowed by filtration through leaf-type vertical or horizontal pressure filters. Carbonatated Hquors, containing calcium carbonate, may require addition of diatomaceous earth as a filter precoat. Phosphatated Hquors are generally filtered with the addition of diatomaceous earth as precoat and body feed. 

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. 

Modifications of the basic process are undersoftening, spHt recarbonation, and spHt treatment. In undersoftening, the pH is raised to 8.5—8.7 to remove only calcium. No recarbonation is required. SpHt recarbonation involves the use of two units in series. In the first or primary unit, the required lime and soda ash are added and the water is allowed to settie and is recarbonated just to pH 10.3, which is the minimum pH at which the carbonic species are present principally as the carbonate ion. The primary effluent then enters the second or secondary unit, where it contacts recycled sludge from the secondary unit resulting in the precipitation of almost pure calcium carbonate. The effluent setties, is recarbonated to the pH of saturation, and is filtered. The advantages over conventional treatment ate reductions in lime, soda ash, and COg requirements very low alkalinities and reduced maintenance costs because of the stabiUty of the effluent. The main disadvantages are the necessity for very careful pH control and the requirement for twice the normal plant capacity. 

Following carbonation, the product can be further purified by screening. This screening, also used to control the maximum size of the product, is followed by dewatering (qv). Rotary vacuum filters, pressure filters, or centrifuges are used in the mechanical removal of water. Final drying is accompHshed as with natural calcium carbonate in either a rotary, spray, or flash dryer. Products having mean particle sizes from submicrometers (- O-OS fiTo) to several micrometers are available. 

A carbonated slurry of cyanamide solution, solid calcium carbonate, and graphite is cooled to remove the heat of reaction. Part of the slurry is recycled to faciUtate temperature control whereas the remainder is filtered yielding cyanamide solution and a cake of calcium carbonate and graphite. The filtered solution is also recycled ia order to control the soHds content. The final concentration of cyanamide is normally maintained at 25%. 

The calcium cyanamide feed is weU mixed with the recycled slurry and filtrate ia a feed vessel. The calcium cyanamide is added at a rate to maintain a pH of 6.0—6.5 ia the cooling tank. The carbonation step can be conducted ia a turbiae absorber with a residence time of 1—2 min. After the carbonation step, the slurry is held at 30—40°C to complete the formation of calcium carbonate, after which the slurry is cooled and filtered. AH equipment for the process is preferably of stainless steel. The resulting solution is used directiy for conversion to dicyandiamide. 

The filtered cake produced from the manufacture of dicyandiamide contains about 86% calcium carbonate. American Cyanamid Co. blends the dried waste for the manufacture of calcium carbide-based desulfurized reagents as a gas releasiag agent. 

Tyj)e of dryer Applicable with dry-product recirculation True and colloidal solutions emulsions. Examples inorganic salt solutions, extracts, milk, blood, waste liquors, rubber latex, etc. Pumpable suspensions. Examples pigment slurries, soap and detergents, calcium carbonate, bentonite, clay sbp, lead concentrates, etc. does not dust. Recirculation of product may prevent sticking Examples filter-press cakes, sedimentation sludges, centrifuged sobds, starch, etc. 

Filter aids should have low bulk density to minimize settling and aid good distribution on a filter-medium surface that may not be horizontal. They should also be porous and capable of forming a porous cake to minimize flow resistance, and they must be chemically inert to the filtrate. These characteristics are all found in the two most popular commercial filter aids diatomaceous silica (also called diatomite, or diatomaceous earth), which is an almost pure silica prepared from deposits of diatom skeletons and expanded perhte, particles of puffed lava that are principally aluminum alkali siheate. Cellulosic fibers (ground wood pulp) are sometimes used when siliceous materials cannot be used but are much more compressible. The use of other less effective aids (e.g., carbon and gypsum) may be justified in special cases. Sometimes a combination or carbon and diatomaceous silica permits adsorption in addition to filter-aid performance. Various other materials, such as salt, fine sand, starch, and precipitated calcium carbonate, are employed in specific industries where they represent either waste material or inexpensive alternatives to conventional filter aids. 

Two hundred grams of eleaned and dried crab shells (Note 1) ground to a fine powder is placed in a 2-1. beaker, and an excess of dilute (approximately 6 N) commercial hydrochloric acid is added slowly to the powdered material until no further action is evident. Much frothing occurs during the addition of the acid, and care must be exercised to avoid loss of material due to foaming over the sides of the beaker. After the reaction has subsided, the reaction mixture is allowed to stand from 4 to 6 hours to ensure complete removal of calcium carbonate. The residue is then filtered, washed with water until neutral to litmus, and dried in an oven at 50-60°. The weight of dried chitin is usually about 70 g., but with some lots of crab shells it may be as low as 40 g. 

Nitrophosphate fertilizer is made by digesting phosphate rock with nitric acid. This is the nitrophosphate route leading to NPK fertilizers as in the mixed-acid route, potassium and other salts are added during the process. The resulting solution is cooled to precipitate calcium nitrate, which is removed by filtration methods. The filtrate is neutralized with ammonia, and the solution is evaporated to reduce the water content. The process of prilling may follow. The calcium nitrate filter cake can be further treated to produce a calcium nitrate fertilizer, pure calcium nitrate, or ammonium nitrate and calcium carbonate. 

During the filtration test of a water suspension containing 14.5 % calcium carbonate in a filter press (A = 0.1 m 50 mrn cake thickness temperature 23 C), the following data were obtained ... 

Determine the filter cloth resistance for the filtration of calcium carbonate under conditions given in the above questions. 

A solution of 0.3 of 3j9-acetoxy-21-ethoxy-17a-pregn-5-en-20-yn-17/3-ol in 7 ml of pure pyridine is hydrogenated over 90 mg of 2.5% palladium-on-calcium carbonate at room temperature and atmospheric pressure. The reaction mixture is filtered and evaporated and the residue recrystallized to give 80 % of the 17a-vinyl product. 

A solution of cholestane-5a,6a-diol 6-tosylate (115a, 0.15 g) in dimethylformamide (20 ml) containing calcium carbonate (0.2 g) is heated for 8 hr on a steam bath. The reaction mixture is then cooled, filtered and diluted with water. The mixture is extracted with ether and the ether extracts are washed with water and saturated salt solution, dried over anhydrous magnesium sulfate and evaporated to dryness under reduced pressure to give the A-homo-B-norketone (116a, 85 mg) mp 123-125° [a]j> 21° (CHCI3). 

About 250 ml of a reaction mixture obtained by the electrolytic reduction of nitrobenzene in sulfuric acid solution and containing about 23 grams of p-aminophenol by assay is neutralized while at a temperature of 60° to 65°C, to a pH of 4.5 with calcium carbonate. The calcium sulfate precipitate which forms is filtered off, the precipitate washed with hot water at about 65°C and the filtrate and wash water then combined. The solution is then extracted twice with 25 ml portions of benzene and the aqueous phase is treated with 0.5 part by weight, for each part of p-aminophenol present, of activated carbon and the latter filtered off. The activated carbon is regenerated by treatment with hot dilute caustic followed by a hot dilute acid wash, and reused a minimum of three times. 

The calcium carbonate precipitate was removed by filtration, and the filtered solution was found to contain 1,436 g of fructose as determined by optical rotation. A small amount of calcium bicarbonate was present as an impurity in solution and was removed by the addition of oxalic acid solution until a test for both calcium and oxalic acid was negative. The insoluble calcium oxalate precipitate was removed by filtration. 

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