US4007030A
Expired / Lapsed
US
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Process for the simultaneous manufacture of phosphoric acid or the salts thereof and a complex multi-component mineral fertilizer
Assignee: Chemadx Dostaw Kompletnych Obiektov Przemyslowych
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Filing: 1976-03-02
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Granted: 1977-02-08
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Expires: 1996-03-02
Abstract
Abstract In the process according to the invention, raw phosphate rock is decomposed with an aqueous solution of sulfuric acid and ammonium sulfate recycled from the conversion step of phosphogypsum into chalk, and then the decomposition liquor stream is divided into a partial acid plant stream (Liquor I) to be converted into phosphoric acid and a partial fertilizer plant stream (Liquor II) to be processed to a multi-component mineral fertilizer. From the acid plant stream (Liquor I) constituting up to 30 per cent by weight of the total decomposition stream, ammonium sulfate is precipitated and introduced into the fertilizer plant stream (Liquor II), all the above mentioned processes of decomposition, separation and precipitation being carried out continuously. Another embodiment of the process according to the invention, wherein the partial acid plant stream (Liquor I) constitutes a partial phosphate plant stream; the said stream comprising aqueous-organic solvent phosphoric acid solution after precipitation of impurities is neutralized with ammonia, alkali metal hydroxides or alkali metal carbonates to yield crystalline phosphate salts of high purity and a homogeneous mixture of organic solvent and water which may be easily separated by distillation.
Inventors
- 👤 Jerzy Schroeder
- 👤 Jerzy Synowiec
- 👤 Tadeusz Zrubek
- 👤 Henryk Gorecki
- 👤 Zdzislaw Wolnicki
- 👤 Roman Hnatowicz
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 21:52
CPC Classifications
C; C05; C05B; C05B11/00; C05B11/04; C05B11/08; C01; C01B; C01B25/00; C01B25/16; C01B25/18; C01B25/22; C01B25/234; C01B25/46
Claims Analysis
Total Claims: 6
Claim 1
Independent Claim
208 words
A process for the simultaneous manufacture of (a) phosphoric acid and (b) a multi-component mineral fertilizer of the NPK type comprising the steps of (1) decomposing crude phosphate rock with an aqueous solution containing ammonium sulfate and sulfuric acid in a molar ratio of about 0.7 to 1.0, whereby a first precipitate of phospho-gypsum is formed; (2) filtering off said first precipitate; (3) dividing the filtrate into two streams designated Liquor I and Liquor II; Liquor I comprising not more than 30 per cent by weight of the two streams; (4) adiabatically cooling Liquor I below 30° C; (5) adding a water miscible organic solvent to the cooled Liquor I below 30° C. in the volume ratio of from about 0.8 to 1.6 of solvent to Liquor I whereby a second precipitate comprising neutral ammonium sulfate and mineral impurities is formed; (6) filtering off said second precipitate to yield an organic solvent-aqueous solution filtrate containing phosphoric acid; (7) separating said organic solvent from said phosphoric acid by distillation; (8) treating Liquor II with potassium chloride, said second precipitate comprising ammonium sulfate, and gaseous ammonia to form an ammonized reaction mixture; and (9) drying and granulating said ammonized reaction mixture to form a multi-component fertilizer of the NPK type.
Claim 2
Dependent Claim
208 words
A process for the simultaneous manufacture of (a) phosphoric acid and (b) a multi-component mineral fertilizer of the NPK type comprising the steps of (1) decomposing crude phosphate rock with an aqueous solution containing ammonium sulfate and sulfuric acid in a molar ratio of about 0.7 to 1.0, whereby a first precipitate of phospho-gypsum is formed; (2) filtering off said first precipitate; (3) dividing the filtrate into two streams designated Liquor I and Liquor II; Liquor I comprising not more than 30 per cent by weight of the two streams; (4) adiabatically cooling Liquor I below 30° C; (5) adding a water miscible organic solvent to the cooled Liquor I below 30° C. in the volume ratio of from about 0.8 to 1.6 of solvent to Liquor I whereby a second precipitate comprising neutral ammonium sulfate and mineral impurities is formed; (6) filtering off said second precipitate to yield an organic solvent-aqueous solution filtrate containing phosphoric acid; (7) separating said organic solvent from said phosphoric acid by distillation; (8) treating Liquor II with potassium chloride, said second precipitate comprising ammonium sulfate, and gaseous ammonia to form an ammonized reaction mixture; and (9) drying and granulating said ammonized reaction mixture to form a multi-component fertilizer of the NPK type.
Claim 3
Dependent Claim
264 words
A process for the simultaneous manufacture of (a) phosphate salts and (b) a multi-component mineral fertilizer of the NPK type comprising the steps of (1) decomposing crude phosphate rock with an aqueous solution containing ammonium sulfate and sulfuric acid in a molar ratio of about 0.7 to 1.0, whereby a first precipitate of phospho-gypsum is formed; (2) filtering off said first precipitate; (3) dividing the filtrate into two streams designated Liquor I and Liquor II, Liquor I comprising not more than 30 per cent by weight of the two streams; (4) adiabatically cooling Liquor I below 30° C.; (5) adding a water miscible organic solvent to the cooled Liquor I below 30° C. in the volume ratio of from about 0.8 to 1.6 of solvent to Liquor I whereby a second precipitate comprising neutral ammonium sulfate and mineral impurities is formed; (6) filtering off said second precipitate to yield an organic solvent - aqueous solution filtrate containing phosphoric acid; (7) neutralizing said organic solvent-aqueous filtrate with a basic material selected from the group consisting of ammonia, alkali metal hydroxides and alkali metal carbonates to form crystalline phosphate salts; (8) filtering off said salts leaving a filtrate of organic solvent and water; (9) separating said organic solvent and water by distillation; (10) recycling said organic solvent to step (5) and said water to step (1); (11) treating Liquor II with potassium chloride, said second precipitate comprising ammonium sulfate, and gaseous ammonium to form an ammonized reaction mixture; and (12) drying and granulating said ammonized reaction mixture to form a multi-component fertilizer of the NPK type.
Claim 4
Dependent Claim
264 words
A process for the simultaneous manufacture of (a) phosphate salts and (b) a multi-component mineral fertilizer of the NPK type comprising the steps of (1) decomposing crude phosphate rock with an aqueous solution containing ammonium sulfate and sulfuric acid in a molar ratio of about 0.7 to 1.0, whereby a first precipitate of phospho-gypsum is formed; (2) filtering off said first precipitate; (3) dividing the filtrate into two streams designated Liquor I and Liquor II, Liquor I comprising not more than 30 per cent by weight of the two streams; (4) adiabatically cooling Liquor I below 30° C.; (5) adding a water miscible organic solvent to the cooled Liquor I below 30° C. in the volume ratio of from about 0.8 to 1.6 of solvent to Liquor I whereby a second precipitate comprising neutral ammonium sulfate and mineral impurities is formed; (6) filtering off said second precipitate to yield an organic solvent - aqueous solution filtrate containing phosphoric acid; (7) neutralizing said organic solvent-aqueous filtrate with a basic material selected from the group consisting of ammonia, alkali metal hydroxides and alkali metal carbonates to form crystalline phosphate salts; (8) filtering off said salts leaving a filtrate of organic solvent and water; (9) separating said organic solvent and water by distillation; (10) recycling said organic solvent to step (5) and said water to step (1); (11) treating Liquor II with potassium chloride, said second precipitate comprising ammonium sulfate, and gaseous ammonium to form an ammonized reaction mixture; and (12) drying and granulating said ammonized reaction mixture to form a multi-component fertilizer of the NPK type.
Claim 5
Dependent Claim
61 words
The process of claim 1 further comprising treating said phospho-gypsum with ammonium carbonate solution to form a precipitate of chalk and a 40% ammonium sulfate solution; filtering off said chalk and treating the filtrate with sulfuric acid to preserve a molar ratio of ammonium sulfate to sulfuric acid of from 0.7 to 1.0; and recycling said treated filtrate to step (1).
Claim 6
Dependent Claim
61 words
The process of claim 2 further comprising treating said phospho-gypsum with ammonium carbonate solution to form a precipitate of chalk and a 40% ammonium sulfate solution; filtering off said chalk and treating the filtrate with sulfuric acid to preserve a molar ratio of ammonium sulfate to sulfuric acid of from 0.7 to 1.0; and recycling said treated filtrate to step (1).
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-02-08 | 1980-08-09 | 1981-02-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-02-08 | 1984-08-09 | 1985-02-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-02-08 | 1988-08-09 | 1989-02-08 | $7700.00 | Window Closed / Lapsed |