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US3975178A Expired / Lapsed US ⏱️ 0.0 years remaining

Purification of wet-process phosphoric acid with methanol and ammonia

Assignee: Tennessee Valley Authority
•
Filing: 1974-05-28
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Granted: 1976-08-17
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Expires: 1994-05-28
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Abstract

Abstract Our invention relates to an improved process for the partial purification of wet-process phosphoric acid with co-production of impure phosphoric acid or solid fertilizer materials containing most of the impurities originally present in the crude acid. The crude acid is treated with methanol and ammonia to precipitate most of the metallic and fluorine impurities as solid ammonium metallic phosphates and fluorine compounds that filter and settle rapidly. The solids are separated from the reaction mixture and methanol is distilled from the resulting clarified solution to form concentrated partially purified acid. The solid ammonium metallic phosphates are fertilizer materials. Alternately, the reaction slurry is separated into a clarified liquid fraction and a settled slurry fraction. Methanol is distilled from the settled fraction which causes most of the impurities to redissolve yielding an impure phosphoric acid.

Inventors

  • 👤 John F. McCullough
  • 👤 Leland L. Frederick

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 02:15
CPC Classifications
C; C05; C05B; C05B7/00; C01; C01B; C01B25/00; C01B25/16; C01B25/18; C01B25/234

Claims Analysis

Total Claims: 8
Claim 1
Independent Claim 242 words
The improved method for the partial purification of crude phosphoric acid prepared from phosphate rock and sulfuric acid and containing 50 to 55 percent P 2 O 5 with co-production of solid fertilizer material, said solid fertilizer material containing 44-55 % P 2 O 5 and 4-7% nitrogen and containing the substantial portion of the metallic and fluorine impurities originally present in the crude phosphoric acid, which improved method consists essentially of the steps of: 1. mixing said crude acid with methanol and ammonia while maintaining the temperature of the resulting mixture between 35°C and the boiling point for a period of time from 15 minutes to 90 minutes, wherein the mole ratio NH 3 :P 2 O 5 of said mixture is maintained from 0.26 to 0.40 and the weight ratio methanol:P 2 O 5 of said mixture is maintained from 2.5 to 4.2; 2. subsequently separating the reaction mixture into a clarified liquid fraction consisting of aqueous phosphoric acid and ammonium phosphate dissolved in methanol and a solid fraction containing 44-55% P 2 O 5 and 4-7% nitrogen and containing the major portion of the metallic and fluorine compounds originally present in the crude phosphoric acid; 3. subsequently separating the methanol from said clarified liquid fraction to obtain partially purified concentrated phosphoric acid; 4. subsequently removing phosphoric acid adhering to said solid fraction by washing with methanol and then evaporating methanol from washed solids to recover said solid fertilizer material.
Claim 2
Dependent Claim 242 words
The improved method for the partial purification of crude phosphoric acid prepared from phosphate rock and sulfuric acid and containing 50 to 55 percent P 2 O 5 with co-production of solid fertilizer material, said solid fertilizer material containing 44-55 % P 2 O 5 and 4-7% nitrogen and containing the substantial portion of the metallic and fluorine impurities originally present in the crude phosphoric acid, which improved method consists essentially of the steps of: 1. mixing said crude acid with methanol and ammonia while maintaining the temperature of the resulting mixture between 35°C and the boiling point for a period of time from 15 minutes to 90 minutes, wherein the mole ratio NH 3 :P 2 O 5 of said mixture is maintained from 0.26 to 0.40 and the weight ratio methanol:P 2 O 5 of said mixture is maintained from 2.5 to 4.2; 2. subsequently separating the reaction mixture into a clarified liquid fraction consisting of aqueous phosphoric acid and ammonium phosphate dissolved in methanol and a solid fraction containing 44-55% P 2 O 5 and 4-7% nitrogen and containing the major portion of the metallic and fluorine compounds originally present in the crude phosphoric acid; 3. subsequently separating the methanol from said clarified liquid fraction to obtain partially purified concentrated phosphoric acid; 4. subsequently removing phosphoric acid adhering to said solid fraction by washing with methanol and then evaporating methanol from washed solids to recover said solid fertilizer material.
Claim 3
Dependent Claim 42 words
A method according to claim 1 wherein the mole ratio NH 3 :P 2 O 5 of said mixture is maintained from 0.30 to 0.38 and the weight ratio methanol:P 2 O 5 of said mixture is maintained from 2.8 to 4.0.
Claim 4
Dependent Claim 20 words
A method according to claim 1 wherein the temperature of said mixture is maintained from 45°C to the boiling point.
Claim 5
Dependent Claim 20 words
A method according to claim 1 wherein the temperature of said mixture is maintained from 55°C to the boiling point.
Claim 6
Dependent Claim 17 words
A method according to claim 1 wherein the residence time is from 30 minutes to 90 minutes.
Claim 7
Dependent Claim 17 words
A method according to claim 1 wherein the residence time is from 45 minutes to 90 minutes.
Claim 8
Dependent Claim 14 words
A method according to claim 1 wherein the ammonia is supplied as anhydrous ammonia.

References Cited (Backward Citations)

GB464370A Cited
US3479139A Cited
FR1518774A Cited
US3635669A Cited
US3663168A Cited
US3764657A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-08-17 1980-02-16 1980-08-17 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-08-17 1984-02-16 1984-08-17 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-08-17 1988-02-16 1988-08-17 $7700.00 Window Closed / Lapsed

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