US3389959A - Manufacture of triple superphosphate - Google Patents
Manufacture of triple superphosphate Download PDFInfo
- Publication number
- US3389959A US3389959A US452347A US45234765A US3389959A US 3389959 A US3389959 A US 3389959A US 452347 A US452347 A US 452347A US 45234765 A US45234765 A US 45234765A US 3389959 A US3389959 A US 3389959A
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- United States
- Prior art keywords
- triple superphosphate
- rock
- manufacture
- triple
- superphosphate
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- YYRMJZQKEFZXMX-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca+2].OP(O)(O)=O.OP(O)(O)=O YYRMJZQKEFZXMX-UHFFFAOYSA-N 0.000 title description 19
- 239000002426 superphosphate Substances 0.000 title description 19
- 238000004519 manufacturing process Methods 0.000 title description 9
- 238000000034 method Methods 0.000 description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 229910019142 PO4 Inorganic materials 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 239000010452 phosphate Substances 0.000 description 8
- 239000002367 phosphate rock Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000011435 rock Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000011874 heated mixture Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B1/00—Superphosphates, i.e. fertilisers produced by reacting rock or bone phosphates with sulfuric or phosphoric acid in such amounts and concentrations as to yield solid products directly
- C05B1/04—Double-superphosphate; Triple-superphosphate; Other fertilisers based essentially on monocalcium phosphate
Definitions
- the oven heating step may be for any suitable period but ordinarily 30 minutes is a sufficient time for such heating.
- the wet process superphosphoric acid having at least 65 weight perphosphqnc 1d had a total P205 of 720% an cent P 0 equivalent and at a P O /CaO ratio of about ortho, phosphonc and content of 385% P205 and a 1.0 to 1.1, and heating the mixture to a temperature in 15 fiuonne confent of 1 the range of about 25045? F, and storing the heated
- the reaction cond1t1ons are set out as follows: mass for reaction to form triple superphosphate. While the o superphosphoric acid may be mixed with the phosphate lmtlalTemp" rock at room temperatures, the superphosphoric acid is No.1 No.2 No.3 preferably heated to about 250450 F.
- An object of the invention is to provide for the pro- 1 25323Ethaner;o;::::::::::::::::::::: 4533" G13 4 11? duction of triple superphosphate from low grade phosphate "I 3 2 3:3 8:2 rock WhlCh has heretofore been considered unsuitable for Percent Water Soluble P20 40.1 45.1 45.3 triple superphosphate production.
- Another object is to gfgggggl if; 3% 6 provide a process in which superphosphonc aClCl 1s em- Percent Available of Total P2 90.5 95.1 93.9 ployed effectively for the benefieiation of low grade phos- Percent cmversm P205 8&9 phate ore or rock and to produce triple superphosphate of substantially greater than 46% P 0 analysis.
- Yet another EXAMPLE H object is to provide a process employing effective Superphosphoric acid was heated in 100 ml. beakers on P O /CaO ratios and initial heating steps by which triple a hotplate to 300 F.
- the acid had a total of 71.05 weight superphosphate is produced having a relatively high P 0 percent of P 0 43.3% ortho and 0.17% insoluble P 0 analysis from low grade phosphate of less than 62 BPL.
- the hot acid was mixed with low grade phosphate rock
- Other'specific objects and advantages will appear as the at a P O /CaO ratio of 1.0.
- the rock was Bartow, Fla. specification proceeds. phosphate rock having 0.1% H 0, 40.15% CaO, 28.1%
- Three sets of the above samples were placed in ovens process superphosphoric acid having at least 65% P 0 regulated to the following temperatures: 431 F., 345 F. weight percent and thereafter the mixture is stored in a and 277 F. After being heated for 30 minutes at the den, as in a conventional triple superphosphate process, above temperatures, the samples were stored for nine days for reaction to form a triple superphosphate product.
- the mixing operation may be carried on at room tempera- While in the foregoing specification I have set forth ture, I prefer to heat the superphosphoric acid to temperaspecific embodiments of the invention in considerable detures above 100 F. and preferably to the temperature tail for the purpose of illustrating the invention, it will range of 250-450" F. If desired, the superphosphoric acid be understood that such details may be varied widely may be preliminarily heated to about 300 F. and low by those skilled in the art without departing from the grade phosphate rock may be mixed with the hot acid spirit of my invention.
- the Iclaim: mixture may be heated, as by placing in ovens, to the 1.
- the steps of acidulating low-grade phosphate the heated mixture then stored in a den, say for about ore having less than 62 BPL, with wet process supernine days, etc., to produce the triple superphosphate product.
- triple superphosphate the steps of acidulating low-grade phosphate ore having a BPL less than 62 with wet process superphosphoric acid having in excess of 70 weight percent P 0 equivalent and at a P O /CaO ratio of about 1.0, heating the same to a temperature in the range of 250450 F. and storing the heated mass for reaction to form triple superphosphate.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Description
United States Patent 3 389 959 MANUFACTURE OF rmiu: SUPERPHOSPHATE Donald E. Lee, Atlanta, Ga., assignor, by mesne assignments, to Armour Agricultural Chemical Company, a
The oven heating step may be for any suitable period but ordinarily 30 minutes is a sufficient time for such heating.
Specific examples illustrative of the process maybe set out as follows:
cor oration of Delaware No Drawing. Filed Apr. 30, 1965, Ser. No. 452,347 EXAMPLE I 3 Claims- A low grade phosphate rock (61.4 BPL), which heretofore has been considered unsuitable for triple superphosphate production, was mixed with 65 weight percent P 0 ABSTRACT OF THE DISCLOSURE wet rrocess superphosphoric acid. The phosphate rock Triple superphosphate is prepared by acidulating lowwas mm Bartow Fla-4 and contamed grade phosphate ore having less than 62 BPL wi h wet CaO, 28. 10% P O and 3.40% fluorine. The wet process superphosphoric acid having at least 65 weight perphosphqnc 1d had a total P205 of 720% an cent P 0 equivalent and at a P O /CaO ratio of about ortho, phosphonc and content of 385% P205 and a 1.0 to 1.1, and heating the mixture to a temperature in 15 fiuonne confent of 1 the range of about 25045? F, and storing the heated The reaction cond1t1ons are set out as follows: mass for reaction to form triple superphosphate. While the o superphosphoric acid may be mixed with the phosphate lmtlalTemp" rock at room temperatures, the superphosphoric acid is No.1 No.2 No.3 preferably heated to about 250450 F. and then mixed 20 Rock Room 100 110 with the rock and the mixture then heated to 250450 F. Acid 150 7 180 before being stored in a den for reaction to form triple set Time,sec superphosphate. Den 50 37 40 o I I a This invention relates to the manufacture of triple super- The product analysls is set out m the followmg table phosphate and more particularly to the beneficiation of TABLEI low grade phosphate rock or ore through the production No.1 No.2 No.3
rocess. p An object of the invention is to provide for the pro- 1 25323Ethaner;o;::::::::::::::::::: 4533" G13 4 11? duction of triple superphosphate from low grade phosphate "I 3 2 3:3 8:2 rock WhlCh has heretofore been considered unsuitable for Percent Water Soluble P20 40.1 45.1 45.3 triple superphosphate production. Another object is to gfgggggl if; 3% 6 provide a process in which superphosphonc aClCl 1s em- Percent Available of Total P2 90.5 95.1 93.9 ployed effectively for the benefieiation of low grade phos- Percent cmversm P205 8&9 phate ore or rock and to produce triple superphosphate of substantially greater than 46% P 0 analysis. Yet another EXAMPLE H object is to provide a process employing effective Superphosphoric acid was heated in 100 ml. beakers on P O /CaO ratios and initial heating steps by which triple a hotplate to 300 F. The acid had a total of 71.05 weight superphosphate is produced having a relatively high P 0 percent of P 0 43.3% ortho and 0.17% insoluble P 0 analysis from low grade phosphate of less than 62 BPL. The hot acid was mixed with low grade phosphate rock Other'specific objects and advantages will appear as the at a P O /CaO ratio of 1.0. The rock was Bartow, Fla. specification proceeds. phosphate rock having 0.1% H 0, 40.15% CaO, 28.1%
In one embodiment of the invention a low grade phOS- P 0 and 3.4% fluorine. phate rock of less than 62 BPL is treated with wet Three sets of the above samples were placed in ovens process superphosphoric acid having at least 65% P 0 regulated to the following temperatures: 431 F., 345 F. weight percent and thereafter the mixture is stored in a and 277 F. After being heated for 30 minutes at the den, as in a conventional triple superphosphate process, above temperatures, the samples were stored for nine days for reaction to form a triple superphosphate product. in the conventional triple superphosphate den for further In the foregoing process, I employ a P O /CaO ratio of reaction and at the end of nine days the triple superphos- 0.9 to 1.1, the ratio of 1.0 or 1.1 being preferred. While phate products analyzed as follows:
TABLE II Temp,, Percent P205 Percent Free Percent Avail Percent Cone Percent F. Acid able of Total version of Rock Total C. I. Avail. Water Sol. P105 P205 the mixing operation may be carried on at room tempera- While in the foregoing specification I have set forth ture, I prefer to heat the superphosphoric acid to temperaspecific embodiments of the invention in considerable detures above 100 F. and preferably to the temperature tail for the purpose of illustrating the invention, it will range of 250-450" F. If desired, the superphosphoric acid be understood that such details may be varied widely may be preliminarily heated to about 300 F. and low by those skilled in the art without departing from the grade phosphate rock may be mixed with the hot acid spirit of my invention. preferably at a P O /CaO ratio of 1.0. Thereafter, the Iclaim: mixture may be heated, as by placing in ovens, to the 1. In a process for the manufacture of triple superhigher range of temperatures preferably 250-450 F. and phosphate, the steps of acidulating low-grade phosphate the heated mixture then stored in a den, say for about ore having less than 62 BPL, with wet process supernine days, etc., to produce the triple superphosphate product.
phosphoric acid having at least 65 weight percent P 0 equivalent and at a P O /CaO ratio of about 1.0 to 1.1,
heating the same to a temperature in the range of about 250-450 F. and storing the heated mass for reaction to form triple superphosphate.
2. In a process for the manufacture of triple superphosphate, the steps of acidulating low-grade phosphate ore having a BPL less than 62 with wet process superphosphoric acid having in excess of 70 weight percent P 0 equivalent and at a P O /CaO ratio of about 1.0, heating the same to a temperature in the range of 250450 F. and storing the heated mass for reaction to form triple superphosphate.
3. In a process for the manufacture of triple superphosphate from low grade phosphate rock, the steps of mixing phosphate rock having a BPL below 62, With wet process superphosphoric acid of about 72 weight percent P 0 equivalentand a P O /CaO ratio of about 1.0, heating the mixture to a temperature of about 25 0- 450 F. fora period of about 30 minutes, and then storing the heated mass in a den for reaction to form triple superphosphate.
References Cited UNITED STATES PATENTS Knox 2 3 109 Carpenter et a1; 23 109 Block 23%1 09 Block 23-109 Bridger 7l-'-41 Baumann 71 34
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US452347A US3389959A (en) | 1965-04-30 | 1965-04-30 | Manufacture of triple superphosphate |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US452347A US3389959A (en) | 1965-04-30 | 1965-04-30 | Manufacture of triple superphosphate |
Publications (1)
Publication Number | Publication Date |
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US3389959A true US3389959A (en) | 1968-06-25 |
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US452347A Expired - Lifetime US3389959A (en) | 1965-04-30 | 1965-04-30 | Manufacture of triple superphosphate |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3518072A (en) * | 1966-11-03 | 1970-06-30 | John G Kronseder | Beneficiation treatment of phosphate rock for preparation of fertilizers and other products |
EP0003424A1 (en) * | 1978-01-23 | 1979-08-08 | Albright & Wilson Limited | Phosphate fertilizers and process for preparing them |
US4405575A (en) * | 1982-04-23 | 1983-09-20 | Henderson Albert E | Method of defluorinating phosphates |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2160700A (en) * | 1938-08-22 | 1939-05-30 | Victor Chemical Works | Crystalline anhydrous monocalcium phosphate |
US2271361A (en) * | 1939-04-25 | 1942-01-27 | Virginia Carolina Chem Corp | Process of production of anhydrous monocalcium phosphate |
US2296494A (en) * | 1939-09-14 | 1942-09-22 | Blockson Chemical Co | Manufacture of anhydrous di-calcium phosphate |
US2296495A (en) * | 1939-09-14 | 1942-09-22 | Blockson Chemical Co | Manufacture of anhydrous monocalcium phosphate |
US2522500A (en) * | 1949-04-20 | 1950-09-19 | Tennesse Valley Authority | Production of phosphatic fertilizers |
US3212874A (en) * | 1963-01-10 | 1965-10-19 | Int Minerals & Chem Corp | Process for the production of phosphate fertilizer |
-
1965
- 1965-04-30 US US452347A patent/US3389959A/en not_active Expired - Lifetime
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2160700A (en) * | 1938-08-22 | 1939-05-30 | Victor Chemical Works | Crystalline anhydrous monocalcium phosphate |
US2271361A (en) * | 1939-04-25 | 1942-01-27 | Virginia Carolina Chem Corp | Process of production of anhydrous monocalcium phosphate |
US2296494A (en) * | 1939-09-14 | 1942-09-22 | Blockson Chemical Co | Manufacture of anhydrous di-calcium phosphate |
US2296495A (en) * | 1939-09-14 | 1942-09-22 | Blockson Chemical Co | Manufacture of anhydrous monocalcium phosphate |
US2522500A (en) * | 1949-04-20 | 1950-09-19 | Tennesse Valley Authority | Production of phosphatic fertilizers |
US3212874A (en) * | 1963-01-10 | 1965-10-19 | Int Minerals & Chem Corp | Process for the production of phosphate fertilizer |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3518072A (en) * | 1966-11-03 | 1970-06-30 | John G Kronseder | Beneficiation treatment of phosphate rock for preparation of fertilizers and other products |
EP0003424A1 (en) * | 1978-01-23 | 1979-08-08 | Albright & Wilson Limited | Phosphate fertilizers and process for preparing them |
US4405575A (en) * | 1982-04-23 | 1983-09-20 | Henderson Albert E | Method of defluorinating phosphates |
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