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US3663168A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of producing concentrated phosphoric acid

Assignee: B D BOHNA AND CO
•
Filing: 1969-07-03
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Granted: 1972-05-16
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Expires: 1989-07-03
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Abstract

Abstract Monocalcium phosphate, advantageously in the form of single superphosphate or triple superphosphate, is mixed with sulfuric acid or ammonium bisulfate and methanol. The monocalcium phosphate and the sulfuric acid or ammonium bisulfate react to form phosphoric acid and a precipitate which contains calcium sulfate. The phosphoric acid is substantially entirely dissolved in the methanol. Next the methanol containing the dissolved phosphoric acid is separated from the solid precipitate by decantation, filtration or centrifugation. By evaporation of the methanol a phosphoric acid concentrate is obtained, or by the addition of a base to the methanolic acid solution, the corresponding phosphate salts are formed and precipitated in an easily separatable and dryable form.

Inventors

  • 👤 Allen G Rubin
  • 👤 Nicholas Kalmar

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 10:12
CPC Classifications
C; C01; C01B; C01B25/00; C01B25/16; C01B25/18; C01B25/22

Claims Analysis

Total Claims: 6
Claim 1
Independent Claim 48 words
The method of claim 1 wherein for each part by weight of the salt, there is present an amount of methanol in the range 0.8 to 10 parts, and the mixture contains in parts by weight less than 50- 60 parts of water per 100 parts of metHanol.
Claim 2
Dependent Claim 91 words
The method of claim 1 wherein the amount of acid is in the range from about 0.9 to 1.2 times the metathetical requirement; in that the amount of methanol is in the range from about 1 to 3 parts; in that the temperature is in the range from about 15* to 50* C.; in that the salt has an average diameter of less than about 1/8 -inch; and in that in parts by weight less than about 5 parts of water per 100 parts of methanol are present in the mixture.
Claim 3
Independent Claim 187 words
A method for the production of concentrated phosphoric acid which comprises reacting monocalcium phosphate with a sulfate acid by mixing the reactants and methanol while maintaining the temperature of the mixture in the range from about 15* to 50* C. for a period in the range from about 1 minute to 10 hours, wherein for each mol of the phosphate salt the amount of acid is in the range from about 1.8 to 2.4 equivalents, wherein for each part by weight of the salt, there is present an amount of methanol in the range from about 0.8 to 3 parts, wherein said acid is selected from the group consisting of sulfuric acid, ammonium bisulfate and mixtures thereof, and wherein said mixture contains in parts by weight less than about 5 parts by weight of water per 100 parts of methanol; physically separating the resulting reaction mixture into a liquid fraction and a solid fraction; and removing methanol from the liquid fraction by fractional distillation; the liquid present in said reaction mixture constituting substantially the total amount of liquid employed in said method of producing concentrated phosphoric acid.
Claim 4
Dependent Claim 51 words
The method of claim 4 further characterized in that the methanol depleted liquid fraction is heated at a temperature in the range from about 100* to 300* C., thereby further concentrating the methanol depleted fraction and producing a phosphoric acid having a P2O5 content of at least about 72 weight percent.
Claim 5
Independent Claim 191 words
The method of producing an inorganic phosphate salt which comprises reacting monocalcium phosphate with a sulfate acid by mixing the reactants and methanol while maintaining the temperature of the mixture in the range below the boiling point of methanol and above about 0* C. for a period in the range from about 1 minute to 10 hours, wherein for each mol of the phosphate salt the amount of acid is in the range of 0.5 to 2.0 times the metathetical requirement, and wherein said acid is selected from the group consisting of sulfuric acid, ammonium bisulfate and mixtures thereof; physically separating the resulting reaction mixture into a liquid fraction of phosphoric acid dissolved in methanol and a solid fraction; and then precipitating an inorganic phosphate salt selected from the group consisting of ammonium phosphate, alkali metal phosphates and alkaline earth metal phosphates from the liquid fraction of phosphoric acid dissolved in methanol by adding a base having a corresponding cation to said liquid fraction; the liquid present in said reaction mixture and said base constituting substantially the total amount of liquid employed in said method of producing an inorganic phosphate salt.
Claim 6
Independent Claim 225 words
The method of producing an inorganic phosphate salt which comprises reacting monocalcium phosphate with a sulfate acid by mixing the reactants and methanol while maintaining the temperature of the mixture in the range from about 15* to 50* C. for a period in the range from about 1 minute to 10 hours, wherein for each mol of the phosphate salt the amount of acid is in the range from about 1.8 to 2.4 equivalents, wherein for each part by weight of the salt, there is present an amount of methanol in the range from about 0.8 to 3 parts, wherein said acid is selected from the group consisting of sulfuric acid, ammonium bisulfate and mixtures thereof, and Wherein said mixture contains in parts by weight less than about 5 parts by weight of water per 100 parts of methanol; physically separating the resulting reaction mixture into a liquid fraction and a solid fraction; and then precipitating an inorganic phosphate salt selected from the group consisting of ammonium phosphate, alkali metal phosphates and alkaline earth metal phosphates from the liquid fraction of phosphoric acid dissolved in methanol by adding a base having a corresponding cation to said liquid fraction; the liquid present in said reaction mixture and said base constituting substantially the total amount of liquid employed in said method of producing an inorganic phosphate salt.

References Cited (Backward Citations)

US1838431A Cited
US2716591A Cited
US2880063A Cited
US3245777A Cited
US3408161A Cited
US3466141A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1975-05-16 1975-11-15 1976-05-16 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1979-05-16 1979-11-15 1980-05-16 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1983-05-16 1983-11-15 1984-05-16 $7700.00 Window Closed / Lapsed

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