Phosphoric acid purification

Double-lined kraft (DLK), 16 96 Double-lined landfills, 25 877 Double mashing, 3 577 Double-neutralization phosphoric acid purification, 13 824-825 Double polarization, in sugar analysis, 23 474... 

The Kuhni contactor (Fig. 13e) has gained considerable commercial application in Europe. Its principal features are the use of a shrouded turbine impeller to promote radial discharge within the compartments and a variable hole arrangement to allow flexibility of design for different process applications. Kuhni extractors are used for extraction of petrochemicals and chemicals, phosphoric acid purification, as well as hydrometallurgical applications and wastewater treatment. Columns up to 16.5 ft in diameter have been constructed. 

The process for acid recovery from waste streams and for H2SO/j displacement from gypsum illustrated the advantages of ABC extractants, resulting from the unique combination of efficiency and reversibility. These properties, combined with selectivity in acid separation, can be applied for purification of acids. The process developed for phosphoric acid purification [35,36] illustrates this ability of ABC extractants. 

Uses Synthetic flavor and fragrance In foods and pharmaceuticals fragrance In cosmetics organic synthesis latent solvent Intermediate solvent for paints, lacquers, paint removers, cleaners, hydraulic fluids, pharmaceuticals fluorometric determinations llq. chromatography mfg. of Isobutyl esters for use In solvents, plasticizers, flavors, and perfumes extraction agent for phosphoric acid purification In food-pkg. adhesives defoamer In food-contact coatings and paper/paperboard In food-contact textiles Features Fruity flavor... 

Uses Prod, of artificial barium sulfate, other barium salts reagent (barium lake formation) lubrication oil additives boiler compounds textile dyeing pigments mfg. of white leather case hardening/heat treatment salts flux in magnesium prod. phosphoric acid purification agent... 

Figure 11.29. Prayon s Process for Phosphoric Acid Purification. 

High power costs and environmental problems have discouraged the installation of new phosphorus furnaces in the United States. Wet process phosphoric acid purification plants using solvent extraction are operating successfully in Europe, Japan, and the United States. 

Chemistry ndProperties. The chemistry of phosphoric acid manufacture and purification is highly complex, largely because of the presence of impurities in the rock. The main chemical reaction in the acidulation of phosphate rock using sulfuric acid to produce phosphoric acid is... 

Simplicity of production, high analysis, and excellent agronomic quaUty are reasons for the sustained high production and consumption of TSP. A contributing factor is that manufacture of the triple superphosphate has been an outlet for so-called sludge acid, the highly impure phosphoric acid obtained as a by-product of normal acid purification. 

Wet Process. Over 90% of the phosphoric acid produced, both in the United States and worldwide, is wet-process phosphoric acid used almost exclusively for agricultural appHcation as both fertilizers and animal feed supplements. Although constituting a small proportion of the total wet-acid production, a significant amount of phosphoric acid for food and technical appHcations is made by purification of wet-process acid. 

Solvent extraction—purification of wet-process phosphoric acid is based on preferential extraction of H PO by an organic solvent vs the cationic impurities present in the acid. Because selectivity of acid over anionic impurities is usually not sufficient, precipitation or evaporation steps are included in the purification process for removal. Cmde wet-process acid is typically concentrated and clarified prior to extraction to remove post-precipitated sludge and improve partition of the acid into the solvent. Concentration also partially eliminates fluoride by evaporation of HF and/or SiF. Chemical precipitation of sulfate (as Ba or Ca salts), fluorosiUcates (as Na salt), and arsenic (as sulfides) may also be used as a prepurification step preceding solvent extraction. 

Modem commercial wet-acid purification processes (see Fig. 4) are based on solvents such as C to Cg alcohols, ethers, ketones, amines, and phosphate esters (10—12). Organic-phase extraction of phosphoric acid is accompHshed in one or more extraction columns or, less frequently, in a series of countercurrent mixer—settlers. Generally, 60—75% of the feed acid P2 s content is extracted into the organic phase as H PO. The residual phosphoric acid phase (raffinate), containing 25—40% of the original P2O5 value, is typically used for fertilizer manufacture such as triple superphosphate. For this reason, wet-acid purification units are almost always located within or next to fertilizer complexes. 

Fig. 4. Schematic diagram of the solvent extraction purification of wet-process phosphoric acid.

The estimated world production of wet-process phosphoric acid was 24,001,000 metric tons of P20 in 1993. Capacity was 34,710,000 metric tons. Over 90% of phosphoric acid production is wet-process (agricultural-grade) acid the remainder is industrial-grades (technical, food, pharmaceutical, etc) made by the thermal route or by the purification of wet-process acid. Table 11 fists U.S. production of wet-process and industrial-grade acids. 

Trickle bed reaction of diol (12) using amine solvents (41) has been found effective for producing PDCHA, and heavy hydrocarbon codistiUation may be used to enhance diamine purification from contaminant monoamines (42). Continuous flow amination of the cycloaUphatic diol in a Hquid ammonia mixed feed gives >90% yields of cycloaUphatic diamine over reduced Co /Ni/Cu catalyst on phosphoric acid-treated alumina at 220°C with to yield a system pressure of 30 MPa (4350 psi) (43). 

B. 2-Methylcyclopenlane-l,3,5-trione hydrate. A mixture of 200 g. (0.89 mole) of the keto ester prepared above, 910 ml. of water, and 100 ml. of 85% phosphoric acid is healed under reflux for 4 hours and then cooled in an ice-salt bath to —5°. The trione mixed with oxalic acid separates and is collected by filtration and dried under reduced pressure. The dried material is extracted with boiling ether (250-300 ml.) under reflux, and the ethereal extract is separated from the undissolved oxalic acid. The original aqueous filtrate is also extracted with ether in a continuous extractor. The two extracts are combined, and ether is removed by distillation. The crude trione separates as a dark brown solid and is crystallized from ca. 250 ml. of hot water. The once-crystallized, faintly yellow product weighs 95-105 g. (74-82%), m.p. 70-74°. This product is used in the next step without further purification. A better specimen, m.p. 77-78°, which is almost colorless, can be obtained by recrystallization from hot water after treatment with Norit activated carbon. 

Haifa Also called IMI. One of the two Wet Processes for producing phosphoric acid by the acidulation of phosphate rock the other is the Dorr process. The Haifa process uses hydrochloric acid for the acidulation and solvent extraction for the purification. It is economic only where by-product hydrochloric acid is available. The overall reaction is ... 

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