Occidental Petroleum

Occidental Research Corporation

James H Moore

Fernando N Ore

John D Ellis

Subhas K Sikdar

Hydrofluoric acid and/or other fluorine compounds are recovered by reacting fluosilicic acid with a sodium-containing compound to form an alkaline aqueous slurry comprising precipitated amorphous silica and dissolved sodium fluoride. The precipitated amorphous silica is separated from the alkaline aqueous slurry leaving an aqueous solution of sodium fluoride. The sodium fluoride solution can be used as such or reacted with other substances (such as alumina, to form synthetic cryolite). Sodium fluoride is recovered from the aqueous solution (as by evaporation or extraction) and used per se or reacted with sulfuric acid to produce hydrogen fluoride.

Process for producing fluorine compounds and amorphous silica

Phosphoric acid is prepared from phosphate rock and sulfuric acid by using a reaction train comprising a dissolving slurry and a crystallization slurry maintained at different sulfate levels. Both inter and intra vessel circulation are used at high rates to minimize reagent concentration gradients and temperature gradients and provide a suitable crystallization environment. Preferably, the intra vessel circulation is substantially in plug flow, as through a draft tube.

Phosphoric acid process with high circulation rates

The invention comprises a multi-vessel reaction apparatus useful for reacting phosphate rock and sulfuric acid in which the reaction slurry undergoes intra- and inter- vessel circulation (preferably through a draft tube). The solution portion of the slurry in a first vessel or set of vessels (the 'dissolver') is preferably maintained at at lower sulfate ion concentration and the solution portion of the slurry in the second vessel or system of vessels (the 'crystallizer') is preferably maintained at a positive sulfate ion concentration. Also preferred are means for maintaining the second vessel or set of vessels at a reduced pressure. Most preferred is that means be included in at least one said vessel for incorporating a crystal modifier (e.g. a sulfonic acid, a sulfonic acid salt, tall oil fatty acids or alkoxylated or esterified tall oil fatty acids) in the crystallizer. The system can be used in the anhydrite, hemihydrate or gypsum types of processes.

Apparatus useful for wet process phosphoric acid production

Hydrofluoric acid is recovered from fluosilicic acid by reacting fluosilicic acid with sodium hydroxide to form a first slurry having a pH of from about 11 to about 14, the first slurry containing sodium metasilicate and precipitated sodium fluoride. Sodium fluoride is recovered from the first slurry leaving a first solution which is reacted with sodium fluosilicate or fluosilicic acid or both to form a second slurry comprising silica and dissolved sodium fluoride. The reaction occurs under such conditions that the second slurry contains precipitated amorphous silica. The precipitated amorphous silica is separated from the second slurry leaving a second solution of sodium fluoride. Sodium fluoride is recovered from the second solution. Recovered sodium fluoride is reacted with sulfuric acid to produce hydrogen fluoride.

Recovery of hydrofluoric acid from fluosilicic acid with high pH

Phosphate rock and sulfuric acid are reacted under conditions which result in the formation of calcium sulfate hemihydrate and phosphoric acid of about 35% to about 55% P.sub.2 O.sub.5. A two vessel reaction system is used in which the reaction slurry undergoes intra- and inter- vessel circulation (preferably through a draft tube). The solution portion of the slurry in the first vessel (the 'dissolver') is preferably maintained at a negative sulfate concentration (i.e. excess Ca.sup.+2) and the solution in the second vessel (the 'crystallizer') is preferably maintained at a positive sulfate ion concentration. Also preferred is that the second vessel be maintained at a reduced pressure, (e.g. to provide evaporation cooling). Better filtration rates can thus be obtained due to the favorable shape, dominant size and size distribution of the hemihydrate crystals. Most preferred is that a crystal modifier (e.g. a sulfonic acid, a sulfonic acid salt, tall oil fatty acids or alkoxylated or esterified tall oil fatty acids) be present in the crystallizer. Surprisingly, the sulfuric acid used in the process can be less (e.g., 0.5-10%) than the stoichiometric amount to convert the calcium in the feed phosphate rock to calcium sulphate.

Hemihydrate type phosphoric acid process

Phosphate rock and sulfuric acid are reacted under conditions which result in the formation calcium sulfate hemihydrate and phosphoric acid of about 30% to about 55% P.sub.2 O.sub.5. A two vessel reaction system is used in which the reaction slurry undergoes inter- and intra- vessel circulation. This results in excellent dispersion of reactants and minimization of temperature and concentration gradients throughout the slurry.

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La Verne, CA, United States of America

James H Moore