CN103803520A - Production method for feed-grade calcium monohydrogenphosphate - Google Patents
Production method for feed-grade calcium monohydrogenphosphate Download PDFInfo
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- CN103803520A CN103803520A CN201410069447.4A CN201410069447A CN103803520A CN 103803520 A CN103803520 A CN 103803520A CN 201410069447 A CN201410069447 A CN 201410069447A CN 103803520 A CN103803520 A CN 103803520A
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Abstract
The invention relates to a production method for feed-grade calcium monohydrogenphosphate and belongs to the field of phosphorus chemical industry. The production method comprises the following steps: firstly, mixing a phosphoric acid liquid with high iron and aluminum content with a liquid containing monohydrogenphosphate; controlling the pH (Potential of Hydrogen) value of the liquid; then settling and filtering to remove iron and aluminum sediments; evaporating water carried by the raw material phosphoric acid liquid in a liquid phase out of a system so that the mass percent content of phosphoric acid in the liquid is 10-60%; then gradually adding calcium carbonate powder until air bubbles are not generated in the reaction system; and settling, filtering and washing to obtain a solid product, namely the feed-grade calcium monohydrogenphosphate, and obtain a liquid phase, namely a calcium monohydrogenphosphate liquid; and returning the solid product and the liquid phase back to be mixed with the phosphoric acid liquid with the high iron and aluminum content. The production method for the feed-grade calcium monohydrogenphosphate has the beneficial effects that the purified phosphoric acid with the high iron and aluminum content is used for producing the feed-grade calcium monohydrogenphosphate and calcium and phosphorus content in the product reaches related national standard requirements; and the phosphoric acid raw material cost in the production process is greatly reduced.
Description
Technical field
The present invention relates to a kind of production method of feed grade calcium monohydrogenphosphate, belong to phosphorous chemical industry field.
Background technology
Feed grade calcium monohydrogenphosphate mainly, as animal-feed, is divided into anhydride and two water things, and widely used is mainly two water things.The main production technique of feed grade calcium monohydrogenphosphate is to adopt phosphoric acid by wet process first to purify as defluorinate is de-to weigh at present, then reacts and makes with Paris white or white lime.But, some phosphorus ore, sesquioxide content is higher, as the phosphorus ore of Near Kunming, yunnan, after the phosphoric acid purification of its wet production, iron aluminium content is high, the raffinate that phosphoric acid by wet process obtains after extraction process is prepared industrial phosphoric acid in addition, in its phosphoric acid, iron aluminium content is also higher, when the phosphoric acid that these iron aluminium content are high is produced for feed grade calcium monohydrogenphosphate, iron aluminium impurity can enter into product, greatly degree has influence on the quality of product, causes product cannot reach feed grade calcium monohydrogenphosphate concerned countries standard.
The phosphoric acid that iron aluminium content is higher could be used for raising the production of calcium after must reducing the iron aluminium content in phosphoric acid, but under Phosphoric Acid, makes iron and aluminum ions precipitate very difficult from the solution of high acidity.
Summary of the invention
The object of this invention is to provide a kind of production method of feed grade calcium monohydrogenphosphate, utilize the qualified feed grade calcium monohydrogenphosphate of phosphoric acid production that iron aluminium content is higher.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of production method of feed grade calcium monohydrogenphosphate, it is characterized in that first phosphoric acid solution high iron aluminium content being mixed with the solution that contains monohydric phosphate, control pH, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid solution is evaporated to system, making phosphoric acid quality degree in solution is 10-60%, then calcium carbonate powder is progressively added wherein until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
Press such scheme, the described high phosphoric acid solution of iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and mass percent concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 0.2-20%, and aluminum ion quality percentage composition is 0.1-20%.
Press such scheme, control pH is 3.4-4.7.
Press such scheme, its calcium carbonate quality percentage composition of described calcium carbonate powder is 90-99%.
Press such scheme, described monohydric phosphate is disodium-hydrogen or potassium phosphate,monobasic.
Take disodium-hydrogen as example, mechanism of the present invention is: disodium-hydrogen and phosphoric acid generate SODIUM PHOSPHATE, MONOBASIC, and the pH value of sodium dihydrogen phosphate is between 4.4～4.7, can make the iron and aluminum ions in phosphoric acid precipitate completely, sedimentation removes by filter the sodium dihydrogen phosphate obtaining after iron aluminum precipitation thing can generate calcium monohydrogenphosphate and disodium-hydrogen with Paris white generation replacement(metathesis)reaction, calcium monohydrogenphosphate is precipitation, and disodium-hydrogen recycles.
Beneficial effect of the present invention is: can use the production for feed grade calcium monohydrogenphosphate of purifying phosphoric acid that iron aluminium content is high, and make calcium phosphorus index in product reach relevant GB requirement, greatly reduce the phosphate raw material cost in production process.
Embodiment
Below in conjunction with embodiment, the present invention will be further described in detail.
Embodiment 1:
First phosphoric acid solution high iron aluminium content is mixed with the solution that contains disodium-hydrogen, the high phosphoric acid solution of described iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 2.0%, aluminum ion quality percentage composition is 1.5%, and to make pH be 4.4, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated to system, making phosphoric acid quality degree in solution is 30%, then the calcium carbonate powder that is 98% by calcium carbonate content progressively joins in the solution after concentrating until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
After above-mentioned processing, in gained feed grade calcium monohydrogenphosphate, calcium contents is 21.2%, and phosphorus content is 17.4%, reaches the requirement of product GB top grade product.
Embodiment 2:
First phosphoric acid solution high iron aluminium content is mixed with the solution that contains disodium-hydrogen, the high phosphoric acid solution of described iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 0.2%, aluminum ion quality percentage composition is 0.1%, and to make pH be 3.4, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated to system, making phosphoric acid quality degree in solution is 10%, then the calcium carbonate powder that is 90% by calcium carbonate content progressively joins in the solution after concentrating until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
After above-mentioned processing, in gained feed grade calcium monohydrogenphosphate, calcium contents is 21.1%, and phosphorus content is 18.0%, reaches the requirement of product GB top grade product.
Embodiment 3:
First phosphoric acid solution high iron aluminium content is mixed with the solution that contains disodium-hydrogen, the high phosphoric acid solution of described iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 20%, aluminum ion quality percentage composition is 20%, and to make pH be 4.7, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated to system, making phosphoric acid quality degree in solution is 60%, then the calcium carbonate powder that is 99% by calcium carbonate content progressively joins in the solution after concentrating until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
After above-mentioned processing, in gained feed grade calcium monohydrogenphosphate, calcium contents is 21.5%, and phosphorus content is 17.6%, reaches the requirement of product GB top grade product.
Embodiment 4:
First phosphoric acid solution high iron aluminium content is mixed with the solution that contains potassium phosphate,monobasic, the high phosphoric acid solution of described iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 0.2%, aluminum ion quality percentage composition is 0.1%, and to make pH be 3.4, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated to system, making phosphoric acid quality degree in solution is 10%, then the calcium carbonate powder that is 90% by calcium carbonate content progressively joins in the solution after concentrating until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
After above-mentioned processing, in gained feed grade calcium monohydrogenphosphate, calcium contents is 21.0%, and phosphorus content is 18.3%, reaches the requirement of product GB top grade product.
Embodiment 5:
First phosphoric acid solution high iron aluminium content is mixed with the solution that contains potassium phosphate,monobasic, the high phosphoric acid solution of described iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 20%, aluminum ion quality percentage composition is 20%, and to make pH be 4.7, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated to system, making phosphoric acid quality degree in solution is 60%, then the calcium carbonate powder that is 99% by calcium carbonate content progressively joins in the solution after concentrating until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
After above-mentioned processing, in gained feed grade calcium monohydrogenphosphate, calcium contents is 22.0%, and phosphorus content is 16.4%, reaches the requirement of product GB top grade product.
Embodiment 6:
First phosphoric acid solution high iron aluminium content is mixed with the solution that contains potassium phosphate,monobasic and disodium-hydrogen, the high phosphoric acid solution of described iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 2%, aluminum ion quality percentage composition is 2%, and to make pH be 4.0, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated to system, making phosphoric acid quality degree in solution is 40%, then the calcium carbonate powder that is 97% by calcium carbonate content progressively joins in the solution after concentrating until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
After above-mentioned processing, in gained feed grade calcium monohydrogenphosphate, calcium contents is 22.2%, and phosphorus content is 16.1%, reaches the requirement of product GB top grade product.
Claims (5)
1. the production method of a feed grade calcium monohydrogenphosphate, it is characterized in that first phosphoric acid solution high iron aluminium content being mixed with the solution that contains monohydric phosphate, control pH, then sedimentation removes by filter iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid solution is evaporated to system, making phosphoric acid quality degree in solution is 10-60%, then calcium carbonate powder is progressively added wherein until no longer include Bubble formation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution that contains monohydric phosphate, returning to the phosphoric acid solution high with iron aluminium content mixes.
2. by the production method of feed grade calcium monohydrogenphosphate claimed in claim 1, it is characterized in that the described high phosphoric acid solution of iron aluminium content be phosphoric acid by wet process through degree of depth defluorinate and after removing heavy metal ion and mass percent concentration 85% time, in phosphoric acid, iron ion quality percentage composition is 0.2-20%, and aluminum ion quality percentage composition is 0.1-20%.
3. by the production method of the feed grade calcium monohydrogenphosphate described in claim 1 or 2, it is characterized in that controlling pH is 3.4-4.7.
4. by the production method of the feed grade calcium monohydrogenphosphate described in claim 1 or 2, it is characterized in that described its calcium carbonate quality percentage composition of calcium carbonate powder is 90-99%.
5. by the production method of the feed grade calcium monohydrogenphosphate described in claim 1 or 2, it is characterized in that described monohydric phosphate is disodium-hydrogen or potassium phosphate,monobasic.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108928839A (en) * | 2017-05-25 | 2018-12-04 | 自贡同发荣实业有限公司 | The method of lithium phosphate production lithium chloride solution |
| CN112320778A (en) * | 2020-11-03 | 2021-02-05 | 瓮福（集团）有限责任公司 | Method for producing high-quality feed-grade calcium hydrophosphate |
Citations (5)
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| US3427125A (en) * | 1966-04-06 | 1969-02-11 | Central Glass Co Ltd | Process for preparing highly pure calcium hydrogen phosphate dihydrate |
| CN1146426A (en) * | 1996-08-23 | 1997-04-02 | 四川绵竹龙蟒矿物质饲料集团有限公司 | Production method of feed-grade monocalcium phosphate |
| CN1183378A (en) * | 1995-10-20 | 1998-06-03 | 四川联合大学 | Production method of feed calcium hydrogen phosphate |
| JP2007070217A (en) * | 2005-08-09 | 2007-03-22 | Univ Of Miyazaki | Preparation of phosphorus-containing aqueous solution from livestock manure-based incineration ash, removal of heavy metals, and recovery method of hydroxyapatite and / or calcium hydrogen phosphate |
| CN102583290A (en) * | 2012-02-18 | 2012-07-18 | 张黔生 | Low-grade phosphorite mineral dressing technology and method for producing by-product high-purity gypsum powder |
-
2014
- 2014-02-27 CN CN201410069447.4A patent/CN103803520B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3427125A (en) * | 1966-04-06 | 1969-02-11 | Central Glass Co Ltd | Process for preparing highly pure calcium hydrogen phosphate dihydrate |
| CN1183378A (en) * | 1995-10-20 | 1998-06-03 | 四川联合大学 | Production method of feed calcium hydrogen phosphate |
| CN1146426A (en) * | 1996-08-23 | 1997-04-02 | 四川绵竹龙蟒矿物质饲料集团有限公司 | Production method of feed-grade monocalcium phosphate |
| JP2007070217A (en) * | 2005-08-09 | 2007-03-22 | Univ Of Miyazaki | Preparation of phosphorus-containing aqueous solution from livestock manure-based incineration ash, removal of heavy metals, and recovery method of hydroxyapatite and / or calcium hydrogen phosphate |
| CN102583290A (en) * | 2012-02-18 | 2012-07-18 | 张黔生 | Low-grade phosphorite mineral dressing technology and method for producing by-product high-purity gypsum powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108928839A (en) * | 2017-05-25 | 2018-12-04 | 自贡同发荣实业有限公司 | The method of lithium phosphate production lithium chloride solution |
| CN112320778A (en) * | 2020-11-03 | 2021-02-05 | 瓮福（集团）有限责任公司 | Method for producing high-quality feed-grade calcium hydrophosphate |
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Effective date of registration: 20160831 Address after: 430079 999 hi tech Avenue, East Lake New Technology Development Zone, Wuhan, Hubei Patentee after: Wuhan Hua Yuan Science and Technology Ltd. Address before: 430074 Wuhan, Hongshan Province District, hung Chu street, No. 693 Patentee before: Wuhan Institute of Technology |