CN103803520B - Production method for feed-grade calcium monohydrogenphosphate - Google Patents
Production method for feed-grade calcium monohydrogenphosphate Download PDFInfo
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- CN103803520B CN103803520B CN201410069447.4A CN201410069447A CN103803520B CN 103803520 B CN103803520 B CN 103803520B CN 201410069447 A CN201410069447 A CN 201410069447A CN 103803520 B CN103803520 B CN 103803520B
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- phosphoric acid
- monohydrogenphosphate
- liquid
- solution
- iron
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- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 title claims abstract description 34
- 235000019700 dicalcium phosphate Nutrition 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 150
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 93
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 75
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 55
- 229910052742 iron Inorganic materials 0.000 claims abstract description 55
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 45
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 38
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000007791 liquid phase Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000004411 aluminium Substances 0.000 claims description 32
- -1 iron ion Chemical class 0.000 claims description 18
- 238000004062 sedimentation Methods 0.000 claims description 17
- 229910019142 PO4 Inorganic materials 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 13
- 239000010452 phosphate Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 10
- 229910001385 heavy metal Inorganic materials 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 8
- 239000007790 solid phase Substances 0.000 claims description 8
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 5
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical group [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 10
- 239000011574 phosphorus Substances 0.000 abstract description 10
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 8
- 239000011575 calcium Substances 0.000 abstract description 8
- 229910052791 calcium Inorganic materials 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 7
- 239000012265 solid product Substances 0.000 abstract 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 2
- 235000019799 monosodium phosphate Nutrition 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- RXDLGFMMQFNVLI-UHFFFAOYSA-N [Na].[Na].[Ca] Chemical compound [Na].[Na].[Ca] RXDLGFMMQFNVLI-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- MWKXCSMICWVRGW-UHFFFAOYSA-N calcium;phosphane Chemical compound P.[Ca] MWKXCSMICWVRGW-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 229940045641 monobasic sodium phosphate Drugs 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- Removal Of Specific Substances (AREA)
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 is mainly used as animal-feed, is divided into anhydride and two water things, widely used mainly two water things.The main production technique of current feed grade calcium monohydrogenphosphate is that to adopt phosphoric acid by wet process first to purify as de-in defluorinate heavy, then react with Paris white or white lime and obtains.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, phosphoric acid by wet process prepares through extraction process the raffinate obtained after 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 used for the production of feed grade calcium monohydrogenphosphate, iron aluminium impurity can enter into product, high 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 highly 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 feed grade calcium monohydrogenphosphate that phosphoric acid production that iron aluminium content is higher is qualified.
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 for iron aluminium content being mixed with the solution containing monohydric phosphate, control solution ph, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid solution is evaporated system, phosphoric acid quality degree in solution is made to be 10-60%, then calcium carbonate powder is progressively added wherein until no longer include bubble generation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
By such scheme, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 0.2-20%, and aluminum ion mass percentage is 0.1-20%.
By such scheme, control solution ph is 3.4-4.7.
By such scheme, its calcium carbonate mass percentage of described calcium carbonate powder is 90-99%.
By such scheme, described monohydric phosphate is disodium-hydrogen or potassium phosphate,monobasic.
For disodium-hydrogen, 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, the iron and aluminum ions in phosphoric acid can be made to precipitate completely, the sodium dihydrogen phosphate that sedimentation filtration obtains after removing de-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: purifying phosphoric acid that iron aluminium content is high can be used for the production of feed grade calcium monohydrogenphosphate, and make calcium phosphorus index in product reach relevant Standard, 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 for iron aluminium content is mixed with the solution containing disodium-hydrogen, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 2.0%, aluminum ion mass percentage is 1.5%, and make solution ph be 4.4, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated system, phosphoric acid quality degree in solution is made to be 30%, then by calcium carbonate content be 98% calcium carbonate powder progressively join concentrated after solution in until no longer include bubble in reaction system and produce, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
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 for iron aluminium content is mixed with the solution containing disodium-hydrogen, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 0.2%, aluminum ion mass percentage is 0.1%, and make solution ph be 3.4, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated system, phosphoric acid quality degree in solution is made to be 10%, then by calcium carbonate content be 90% calcium carbonate powder progressively join concentrated after solution in until no longer include bubble in reaction system and produce, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
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 for iron aluminium content is mixed with the solution containing disodium-hydrogen, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 20%, aluminum ion mass percentage is 20%, and make solution ph be 4.7, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated system, phosphoric acid quality degree in solution is made to be 60%, then by calcium carbonate content be 99% calcium carbonate powder progressively join concentrated after solution in until no longer include bubble in reaction system and produce, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
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 for iron aluminium content is mixed with the solution containing potassium phosphate,monobasic, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 0.2%, aluminum ion mass percentage is 0.1%, and make solution ph be 3.4, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated system, phosphoric acid quality degree in solution is made to be 10%, then by calcium carbonate content be 90% calcium carbonate powder progressively join concentrated after solution in until no longer include bubble in reaction system and produce, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
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 for iron aluminium content is mixed with the solution containing potassium phosphate,monobasic, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 20%, aluminum ion mass percentage is 20%, and make solution ph be 4.7, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated system, phosphoric acid quality degree in solution is made to be 60%, then by calcium carbonate content be 99% calcium carbonate powder progressively join concentrated after solution in until no longer include bubble in reaction system and produce, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
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 for iron aluminium content is mixed with the solution containing potassium phosphate,monobasic and disodium-hydrogen, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 2%, aluminum ion mass percentage is 2%, and make solution ph be 4.0, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid is evaporated system, phosphoric acid quality degree in solution is made to be 40%, then by calcium carbonate content be 97% calcium carbonate powder progressively join concentrated after solution in until no longer include bubble in reaction system and produce, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix.
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 (2)
1. the production method of a feed grade calcium monohydrogenphosphate, it is characterized in that first phosphoric acid solution high for iron aluminium content being mixed with the solution containing monohydric phosphate, described monohydric phosphate is disodium-hydrogen or potassium phosphate,monobasic, control solution ph is 3.4-4.7, then sedimentation filtration is except de-iron aluminum precipitation thing, the water yield of bringing in liquid phase Raw phosphoric acid solution is evaporated system, phosphoric acid quality degree in solution is made to be 10-60%, then calcium carbonate powder is progressively added wherein until no longer include bubble generation in reaction system, then sedimentation filtration washing, gained solid phase prod is feed grade calcium monohydrogenphosphate, gained liquid phase is the solution containing monohydric phosphate, return the phosphoric acid solution high with iron aluminium content to mix, the phosphoric acid solution that described iron aluminium content is high 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 mass percentage is 0.2-20%, and aluminum ion mass percentage is 0.1-20%.
2., by the production method of feed grade calcium monohydrogenphosphate according to claim 1, it is characterized in that its calcium carbonate mass percentage of described calcium carbonate powder is 90-99%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410069447.4A CN103803520B (en) | 2014-02-27 | 2014-02-27 | Production method for feed-grade calcium monohydrogenphosphate |
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| CN201410069447.4A CN103803520B (en) | 2014-02-27 | 2014-02-27 | Production method for feed-grade calcium monohydrogenphosphate |
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| CN103803520A CN103803520A (en) | 2014-05-21 |
| CN103803520B true CN103803520B (en) | 2015-06-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 (4)
| 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 |
| 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 for fodder grade calcium phosphate |
| CN1183378A (en) * | 1995-10-20 | 1998-06-03 | 四川联合大学 | Method for producing feed 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4491612B2 (en) * | 2005-08-09 | 2010-06-30 | 国立大学法人 宮崎大学 | 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 |
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- 2014-02-27 CN CN201410069447.4A patent/CN103803520B/en active Active
Patent Citations (4)
| 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 | Method for producing 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 for fodder grade calcium 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 |
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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 |