GB726848A - Process for the production of an ammonium-citrate soluble fertilizer containing mainly secondary calcium phosphate - Google Patents

Process for the production of an ammonium-citrate soluble fertilizer containing mainly secondary calcium phosphate

Info

Publication number
GB726848A
GB726848A GB8564/53A GB856453A GB726848A GB 726848 A GB726848 A GB 726848A GB 8564/53 A GB8564/53 A GB 8564/53A GB 856453 A GB856453 A GB 856453A GB 726848 A GB726848 A GB 726848A
Authority
GB
United Kingdom
Prior art keywords
phosphate
solution
precipitation
ammonia
ammonium nitrate
Prior art date
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.)
Expired
Application number
GB8564/53A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Patheon Austria GmbH and Co KG
Original Assignee
Chemie Linz AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Chemie Linz AG filed Critical Chemie Linz AG
Publication of GB726848A publication Critical patent/GB726848A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B11/00Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
    • C05B11/04Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
    • C05B11/06Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)

Abstract

Secondary calcium phosphate is prepared by precipitation with ammonia from a mineral acid solution of raw phosphate in the presence of 0.5 to 4 per cent. by weight of a magnesium compound soluble in the solution, based on the weight of the raw phosphate. The preferred mineral acid is nitric acid. The magnesium compound may be added to the phosphate, to the acid or the acid solution, or to the ammonia solution employed for precipitation. The precipitation may be effected at above 55 DEG C. to form an anhydrous phosphate, or the phosphate precipitated at lower temperatures may be dried at temperatures rising to 300 DEG C. The mother liquor remaining after separation of the secondary calcium phosphate may be treated with ammonia and carbon dioxide or ammonium carbonate to precipitate the calcium and magnesium content, leaving a useful solution of ammonium nitrate. Alternatively, the latter precipitation may take place at the same time as the precipitation of the phosphate, in which case the solution resulting from the acid attack and containing the magnesium compound is neutralized with ammonia until a pH of 4 has been reached and the precipitation is continued with ammonia gas and carbon dioxide gas until a pH of 7 to 8 has been reached. The combined precipitate is then filtered off. Any excess ammonium carbonate remaining in the mother liquor may be neutralized with nitric acid to again obtain ammonium nitrate solution. The precipitation of the phosphate with or without the remaining calcium may take place in stages in agitator vessels in commercial operation. According to examples (i) phosphate mixed with calcined magnesite is dissolved in nitric acid, and precipitation effected at about 40 DEG C. with an ammoniacal precipitating solution containing ammonium nitrate until a pH of 4 is reached. Secondary calcium phosphate containing water of crystallisation is precipitated and separated. (ii) As in (i) above except that the magnesite is added to the solution resulting from the acid attack on the phosphate. (iii) Phosphate is treated with nitric acid at 40 DEG C. with agitation, and the temperature then raised to 50 DEG C., whereupon a precipitating solution containing ammonia, ammonium nitrate and magnesium nitrate is added; after precipitation at a pH of 4, the filter cake obtained contains anhydrous secondary calcium phosphate and all the fluorine and other impurities of the raw phosphates. The mother liquor containing ammonium nitrate, calcium nitrate and magnesium nitrate is precipitated at 60 DEG C. with ammonium carbonate solution of a pH of 7 to 8 to obtain a precipitate of calcium carbonate containing a small amount of magnesium. The ammonium nitrate solution remaining may be in part recirculated to prepare the precipitating solution; both the calcium carbonate and the ammonia nitrate solution, after evaporation, are suitable for making calcium ammonium nitrate. (iv) Phosphate is dissolved in nitric acid at 40 DEG C. and calcined magnesite is then added. Precipitation is effected with ammonia/ammonium nitrate solution of 60 DEG C. at a pH of 4 and the precipitation is thereafter continued at the same temperature with ammonium carbonate solution until a pH of 7 to 8 has been reached. The mixture is filtered and the precipitate washed and dried at 100 DEG C. The ammonium nitrate solution remaining may again be recycled to the process after having been saturated with ammonia gas.ALSO:A fertilizer comprising secondary calcium phosphate is prepared by precipitation with ammonia from a mineral acid solution of raw phosphate in the presence of 0.5 to 4 per cent. by weight of a magnesium compound soluble in the solution, based on the weight of the raw phosphate. The preferred mineral acid is nitric acid. The magnesium compound may be added to the phosphate, to the acid or the acid solution, or to the ammonia solution employed for precipitation. The precipitation may be effected at above 55 DEG C. to form an anhydrous phosphate, or the phosphate precipitated at lower temperatures may be dried at temperatures rising to 300 DEG C. The mother liquor remaining after separation of the secondary calcium phosphate may be treated with ammonia and carbon dioxide or ammonium carbonate to precipitate the calcium and magnesium content leaving a useful solution of ammonium nitrate. Alternatively, the latter precipitation may take place at the same time as the precipitation of the phosphate, in which case the solution resulting from the acid attack and containing the magnesium compound is neutralized with ammonia until a pH of 4 has been reached and the precipitation is continued with ammonia gas and carbon dioxide gas until a pH of 7 to 8 has been reached. The combined precipitate is then filtered off. Any excess ammonium carbonate remaining in the mother liquor may be neutralized with nitric acid to again obtain ammonium nitrate solution. The precipitation of the phosphate with or without the remaining calcium may take place in stages in agitator vessels in commercial operation. According to examples, (i) phosphate mixed with calcined magnesite is dissolved in nitric acid, and precipitation effected at about 40 degrees C. with an ammoniacal precipitating solution containing ammonium nitrate until a pH of 4 is reached. Secondary calcium phosphate containing water of crystallisation is precipitated and separated.; (ii) as in (1) above except that the magnesite is added to the solution resulting from the acid attack on the phosphate; (iii) phosphate is treated with nitric acid at 40 DEG C. with agitation, and the temperature then raised to 50 DEG C. whereupon a precipitating solution containing ammonia, ammonium nitrate and magnesium nitrate is added; after precipitation at a pH of 4 the filter cake obtained contains anhydrous secondary calcium phosphate and all the fluorine and other impurities of the raw phosphates. The mother liquor containing ammonium nitrate, calcium nitrate and magnesium nitrate is precipitated at 60 DEG C. with ammonium carbonate solution at a pH of 7 to 8 to obtain a precipitate of calcium carbonate containing a small amount of magnesium. The ammonium nitrate solution remaining may be in part recirculated to prepare the precipitating solution, both the calcium carbonate and the ammonium nitrate solution, after evaporation, are suitable for making calcium ammonium nitrate; (iv) phosphate is dissolved in nitric acid at 40 DEG C. and calcined magnesite is then added. Precipitation is effected with ammonia/ammonium nitrate solution of 60 DEG C. at a pH of 4 and the precipitation is thereafter continued at the same temperature with ammonium carbonate solution until a pH of 7 to 8 has been reached. The mixture is filtered and the precipitate washed and dried at 100 DEG C. The ammonium nitrate solution remaining may again be recycled to the process after having been saturated with ammonia gas.
GB8564/53A 1952-03-27 1953-03-27 Process for the production of an ammonium-citrate soluble fertilizer containing mainly secondary calcium phosphate Expired GB726848A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AT726848X 1952-03-27

Publications (1)

Publication Number Publication Date
GB726848A true GB726848A (en) 1955-03-23

Family

ID=3680009

Family Applications (1)

Application Number Title Priority Date Filing Date
GB8564/53A Expired GB726848A (en) 1952-03-27 1953-03-27 Process for the production of an ammonium-citrate soluble fertilizer containing mainly secondary calcium phosphate

Country Status (1)

Country Link
GB (1) GB726848A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1121081B (en) * 1958-06-10 1962-01-04 Companie De Saint Gobain Process for the production of multi-nutrient fertilizers
EP1240109A1 (en) * 1999-12-09 2002-09-18 The Burnham Company Methods for treating wastewater sludge
CN111204779A (en) * 2020-03-10 2020-05-29 余荣华 Fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1121081B (en) * 1958-06-10 1962-01-04 Companie De Saint Gobain Process for the production of multi-nutrient fertilizers
EP1240109A1 (en) * 1999-12-09 2002-09-18 The Burnham Company Methods for treating wastewater sludge
CN111204779A (en) * 2020-03-10 2020-05-29 余荣华 Fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer

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