Sulfuric ammonia precipitation

From 1980 s, several research groups studied the components of EFE, independently [4,5,6]. Different purification methods were employed to isolate the enzymes, including sulfuric ammonia precipitation, gel filtration, ion exchanging, high-pressure liquid chromatography (HPLC)... 

The Fumaks process removes approximately 95% of the H2S content of coke-oven gas in a single scrubbing stage. Ammonia is a better reagent than soda ash for the process since it produces less byproduct thio.sulfate. The sulfur recovery yields are 85% with ammonia and only 70% with soda ash. The sulfur is precipitated as tiny (1-2 p in diam.) rhombic sulfur... 

The second ceUulosic fiber process to be commercialized was invented by L. H. Despeissis (4) in 1890 and involved the direct dissolution of cotton fiber in ammoniacal copper oxide Uquor. This solvent had been developed by M. E. Schweizer in 1857 (5). The cuprammonium solution of ceUulose was spun into water, with dilute sulfuric acid being used to neutralize the ammonia and precipitate the ceUulose fibers. H. Pauly and co-workers (6) improved on the Despeissis patent, and a German company, Vereinigte Glanstoff Eabriken, was formed to exploit the technology. In 1901, Dr. Thiele at J. P. Bemberg developed an improved stretch-spinning system, the descendants of which survive today. 

Boron trifluoride catalyst may be recovered by distillation, chemical reactions, or a combination of these methods. Ammonia or amines are frequently added to the spent catalyst to form stable coordination compounds that can be separated from the reaction products. Subsequent treatment with sulfuric acid releases boron trifluoride. An organic compound may be added that forms an adduct more stable than that formed by the desired product and boron trifluoride. In another procedure, a fluoride is added to the reaction products to precipitate the boron trifluoride which is then released by heating. Selective solvents may also be employed in recovery procedures (see Catalysts,regeneration). 

Gas Reduction. The use of a gaseous reduciag agent is attractive because the metal is produced as a powder that can easily be separated from the solution. Carbon dioxide, sulfur dioxide, and hydrogen can be used to precipitate copper, nickel, and cobalt, but only hydrogen reduction is appHed on an iadustrial scale. In the Sherritt-Gordon process, the excess ammonia is removed duting the purification to achieve a 2 1 ratio of NH iNi ia solution. Nickel powder is then precipitated by... 

HydrometaHurgical Processes. The hydrometaHurgical treatments of oxide ores involve leaching with ammonia or with sulfuric acid. In the ammoniacal leaching process, the nickel oxide component of the ore first is reduced selectively. Then the ore is leached with ammonia which removes the nickel into solution, from which it is precipitated as nickel carbonate by heating. A nickel oxide product used in making steel is produced by roasting the carbonate. 

Qualitative Analysis. Nitric acid may be detected by the classical brown-ring test, the copper-turnings test, the reduction of nitrate to ammonia by active metal or alloy, or the nitrogen precipitation test. Nitrous acid or nitrites interfere with most of these tests, but such interference may be eliminated by acidifying with sulfuric acid, adding ammonium sulfate crystals, and evaporating to alow volume. 

The gaseous ammonia is passed through electrostatic precipitators for particulate removal and mixed with the cooled gas stream. The combined stream flows to the ammonia absorber where the ammonia is recovered by reaction with a dilute solution of sulfuric acid to form ammonium sulfate. Ammonium sulfate precipitates as small crystals after the solution becomes saturated and is withdrawn as a slurry. The slurry is further processed in centrifuge faciHties for recovery. Crystal size can be increased by employing one of two processes (99), either low differential controUed crystallization or mechanical size enlargement by continuous compacting and granulation. 

Silver Chloride. Silver chloride, AgCl, is a white precipitate that forms when chloride ion is added to a silver nitrate solution. The order of solubility of the three silver halides is Cl" > Br" > I. Because of the formation of complexes, silver chloride is soluble in solutions containing excess chloride and in solutions of cyanide, thiosulfate, and ammonia. Silver chloride is insoluble in nitric and dilute sulfuric acid. Treatment with concentrated sulfuric acid gives silver sulfate. 

The anaerobic reaction of sulfur dioxide with aqueous ammonia produces a solution of ammonium sulfite [10192-30-0]. This reaction proceeds efficientiy, even with a gas stream containing as Httie as 1 wt % sulfur dioxide. The sulfur dioxide can be regenerated at a high concentration by acidulation or by stream stripping of the ammonium sulfite solution, or the sulfite can be made to precipitate and the ammonia recovered by addition of lime (243). The process can also be modified to produce ammonium sulfate for use as fertili2er (244) (see Fertilizers). In a variant of this process, the use of electron-beam radiation cataly2es the oxidation of sulfur dioxide in the presence of ammonia to form ammonium sulfate (245). 

Arsenic pentasulfide (arsenic(V) sulfide), As S q, is stable in air up to 95°C, but at higher temperatures begins to dissociate into arsenous sulfide and sulfur. It is prepared by the fusion of arsenic with sulfur foUowed by extraction with ammonia and reprecipitation at low temperatures by addition of hydrochloric acid. Arsenic pentasulfide is precipitated at low temperatures from strongly acidic arsenate solutions by a rapid stream of hydrogen sulfide. It is hydrolyzed by boiling with water, yielding arsenous acid and sulfur. Salts derived from a number of thioarsenic acids are formed from arsenic pentasulfide and alkaH metal sulfides. 

An electrostatic precipitator is used to remove more tar from coke oven gas. The tar is then sent to storage. Ammonia liquor is also separated from the tar decanter and sent to wastewater treatment after ammonia recovery. Coke oven gas is further cooled in a final cooler. Naphthalene is removed in a separator on the final cooler. Light oil is then removed from the coke oven gas and is fractionated to recover benzene, toluene, and xylene. Some facilities may include an onsite tar distillation unit. The Claus process is normally used to recover sulfur from coke oven gas. During the coke quenching, handling, and screening operation, coke breeze is produced. The breeze is either reused on site (e.g., in the sinter plant) or sold offsite as a by-product. 

Acetylene and Potassium in Liquid Ammonia Potassium (40 g) is dissolved in 1 liter of dry liquid ammonia. Dry acetylene is then bubbled into the solution until the blue color is discharged. A solution of 15 g of estrone in 300 ml of dioxane is prepared and diluted with 300 ml of ether, cooled, and added to the potassium acetylide solution over a period of 10 min. The liquid ammonia is allowed to evaporate, an additional 500 ml of ether is added, and the mixture is allowed to stand overnight. About 3 liters of 5 % sulfuric acid is added and the organic layer separated. The water layer is re-extracted with fresh ether, and the combined ether extracts are washed twice with 5 % sodium carbonate solution, th6n several times with water, and finally evaporated under reduced pressure. The residue is dissolved in 150 ml of methanol, then an equal quantity of hot water is added and the mixture cooled. The precipitated solid is collected, washed with cold 60 % methanol and crystallized once from methanol-water to give 14.8 g (85%) of 17a-ethynylestradiol mp 143-144°. 

Disulfur dichtoridc was added to an aqueous solution of ammonia to give a yellow precipitate of sulfur contaminated with S4N4 y. Pharm. Chim. 11, 315 (1835). 

To a solution of 13.5 g of 5-(2-chlorophenyl)-3H-1,4-benzodiazepin-2(1 H)-one in 60 ml of concentrated sulfuric acid, a solution of 5.5 g of potassium nitrate in 20 ml concentrated sulfuric acid was added dropwise. The solution then was heated in a bath at 45° to 50°C for Th hours, cooled and poured on ice. After neutralizing with ammonia, the formed precipitate was filtered off and boiled with ethanol. A small amount of white insoluble material was then filtered off. The alcoholic solution on concentration yielded crystals of 7-nitro-5-(2-chlorophenyl)-3H-1,4-benzodiazepin-2(1H)-one which, after recrystallization from dichloromethane, melted at 238° to 240°C. 

Airey et al. [8] have described a method for removing sulfide prior to the determination of these anions in anoxic estuarine waters. Mercury(II) chloride was used to precipitate free sulfide from samples of anoxic water. The sulfide-free supernatant solution was used to estimate sulfide by measuring the concentration of unreacted mercury(II), as well as to determine sulfate, inorganic phosphate, and nitrate by spectrophotometric methods, in which sulfide interferes. Sulfide concentrations in the range 0.5-180 000 ig/l sulfur could be measured, while the lower limits for sulfate, ammonia, nitrite, and inorganic phosphate were 0.024, -1.0 and 1 xg/l, respectively. 

Ebara [Electron beam ammonia reaction] A dry process for removing sulfur and nitrogen oxides from flue-gas. A beam of high energy electrons is injected into the gas, to which a stoichiometric quantity of ammonia has been added. The product, a mixture of ammonium sulfate and ammonium nitrate, is collected downstream by an electrostatic precipitator or a bag filter. Developed by Ebara Corporation, Japan, and piloted in Indianapolis in 1986. 

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