Agrico Chemical Company

Freeport Mcmoran Resource Partners

John W Wen

Charles W Weston

Frederick S Mandel

This invention provides a method for removing aluminum contamination from phosphoric acid during the acidulation of phosphate rock with sulfuric acid in the presence of recycled phosphoric acid. The method of this invention involves the addition of acid soluble silica to the acidulation slurry and calls for maintaining the molar ratio of non-fluosilicate fluoride (i.e. fluoride not complexed with silica) to aluminum in the liquid phase of the acidulation slurry between 2.5 and 5.0. These conditions favor the precipitation of aluminum as calcium tetrafluoaluminate dihydrate and enable the co-removal of this compound by filtration with by-product gypsum. This invention is particularily suitable for the processing of phosphate rocks with high iron and aluminum contents, such as the nonsedimentary phosphate rocks occurring in Sri Lanka.

Removal of aluminum contamination during production of phosphoric acid

A process for the recovery of sulfur from sulfur-bearing ores employing an aqueous leaching solution containing calcium monosulfide, calcium hydrosulfide or mixtures of such calcium sulfide species. The sulfur ore is contacted in an extraction zone with the aqueous leaching solution under conditions to solubilize sulfur from the ore in the form of calcium polysulfide. Preferably, the extraction step is carried out at an elevated temperature. The loaded leaching solution is recovered from the extraction zone and applied to a sulfur-production zone. Here the loaded solution is contacted with hydrogen sulfide under conditions to react the hydrogen sulfide with the calcium polysulfide to produce calcium hydrosulfide and elemental sulfur. The calcium hydrosulfide solution is recycled for use as leaching solution in the sulfur extraction zone.

Sulfur recovery process

Phosphoric acid is produced by the wet process from phosphate rock containing fluochlorapatite. The rock is ground in a crusher (10) to a size such that from about 50% to about 90% by weight will be passed by a -200 mesh U.S.S. sieve before being passed into a digestor (14) where it is mixed with sulfuric acid and recycled phosphoric acid to form a slurry. A suitable reductant such as sulphur dioxide is added to the slurry to maintain the oxidation-reduction potential in the range from about +150 mv to about +750 mv. The gypsum by-products are then removed from the slurry at filter (16) and a portion of the acid is recycled to digestor (14). The remaining acid is either concentrated and further processed to make fertilizers or is further processed via path (20) to remove aluminum and/or iron impurities. Select amounts of fluoride and sodium containing compounds are added to the acid in a stirred reactor (30) to cause precipitation of aluminum, principally as Na.sub.2 AlF.sub.5. After about 15 to about 60 minutes of stirring at a temperature below about 70.degree. C., the precipitate is removed at filter (32) where the acid is either processed to make fertilizer or subjected to additional processing to remove iron contaminants. Iron contaminants are removed from the filter acid or from aluminum removed acid from filter (32) by adding sufficient ammonia to the acid in a stirring reactor (40) to cause precipitation of iron principally as NH.sub.4 Fe.sub.2 H.sub.8 (PO.sub.4).sub.5.AH.sub.2 O, to reduce the level of iron to desired levels. After aging in the reactor from about 2 to about 24 hours at a temperature below the boiling point of the acid, the precipitate is removed at filter (42) and the resulting iron reduced acid is concentrated and subjected to conventional processing for making fertilizers.

Process for producing wet process phosphoric acid from phosphate rocks

A method of producing purified monoammonium phosphate from wet process phosphoric acid and ammonia is provided. The ammoniation takes place in two stages, the acid being ammoniated in the first stage to a pH between about 1.5 and 2.5. This mixture is allowed to age after which the mixture is ammoniated to a pH between about 4 and 5. An impurity-containing precipitate is formed in the first and second stages of ammoniation that is easily filterable from the monoammonium phosphate solution derived from the second ammoniation stage.

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Baton Rouge, LA, United States of America

John W Wen