CN104495775B - A kind of method producing feed-level calcium biphosphate - Google Patents
A kind of method producing feed-level calcium biphosphate Download PDFInfo
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- CN104495775B CN104495775B CN201510004309.2A CN201510004309A CN104495775B CN 104495775 B CN104495775 B CN 104495775B CN 201510004309 A CN201510004309 A CN 201510004309A CN 104495775 B CN104495775 B CN 104495775B
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- China
- Prior art keywords
- phosphoric acid
- reactive tank
- slip
- phosphate rock
- ground phosphate
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- 238000000034 method Methods 0.000 title claims abstract description 23
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 title claims abstract description 6
- 229910000389 calcium phosphate Inorganic materials 0.000 title claims abstract description 6
- 235000019691 monocalcium phosphate Nutrition 0.000 title claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 22
- 239000002367 phosphate rock Substances 0.000 claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 239000011265 semifinished product Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- CYQAYERJWZKYML-UHFFFAOYSA-N phosphorus pentasulfide Chemical compound S1P(S2)(=S)SP3(=S)SP1(=S)SP2(=S)S3 CYQAYERJWZKYML-UHFFFAOYSA-N 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 5
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 8
- 239000011574 phosphorus Substances 0.000 abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011575 calcium Substances 0.000 abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052791 calcium Inorganic materials 0.000 abstract description 4
- 239000000470 constituent Substances 0.000 abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 2
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 2
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 2
- 238000007701 flash-distillation Methods 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- 206010059410 Faecaluria Diseases 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000019730 animal feed additive Nutrition 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007952 growth promoter Substances 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Fodder In General (AREA)
Abstract
A kind of method producing feed-level calcium biphosphate, its procedure of processing is: ground phosphate rock, concentration 40% 50% purifying phosphoric acid, compound three kinds of materials of cleaner are added in reactive tank 1 stirring by (1)；Stir subsequently in reactive tank 2；(2) material after having reacted in reactive tank 2 is sent in deblending slot, removed continuously in slip by low level flash condenser and enter after impurity in neutralization chamber, add in nertralizer Paris white at this and the phosphoric acid of excess, slip is after neutralization chamber entrance accurate adjustment groove further accurate adjustment PH is to 2.8 3.0, conveying goes to be spray-dried prepared dalcium biphosphate semi-finished product, is finished product after drum drier is further dried.Advantage: it is short that the present invention has technological process, can effectively utilize part calcium constituent in phosphorus ore, reduce sulfuric acid dosage simultaneously, energy-saving and cost-reducing.
Description
Technical field
The present invention relates to the production method of a kind of feed-level calcium biphosphate.
Background technology
Feed additive is the indispensable nutritional labeling of animal feed, and it has very important effect to the growth promoter promoting animal.At present, animal feed additive mainly has two kinds, and one is dalcium biphosphate, and one is calcium hydrogen phosphate.Dalcium biphosphate is high due to water-soluble phosphorus content, can improve animal and digest and assimilate phosphorus, decrease the discharge of phosphorus in animal fecaluria, is particularly well-suited to young animal feedstuff and uses, is a developing direction of feed phosphate from now on.
Producing dalcium biphosphate at present mainly has following three kinds of methods, first pulverized limestone and thermal phosphoric acid reaction to generate the dalcium biphosphate of solid, shaped, then prepares dalcium biphosphate finished product through ripening pulverizing；It two is calcium hydrogen phosphate semi-finished product and phosphatase reaction prepares dalcium biphosphate slip, spray-dried after prepare dalcium biphosphate finished product；It three is to prepare dalcium biphosphate slip with calcium carbonate (or pulverized limestone) and the phosphatase reaction produced, spray-dried after prepare dalcium biphosphate finished product.Owing to thermal phosphoric acid cost is high, uncontested advantage, substantially produce without this method.Either phosphoric acid by wet process or thermal phosphoric acid, the calcium constituent in phosphorus ore all cannot utilize, a large amount of ardealite of phosphoric acid by wet process also by-product, causes the secondary pollution to environment.
Summary of the invention
The technical problem to be solved is to provide one can overcome drawbacks described above, both make use of the calcium constituent in phosphorus ore, has saved sulfuric acid dosage, reduces secondary environmental pollution, can realize again system quantity-produced one feed-level calcium biphosphate production method.
Processing method of the present invention is the acid decomposed by phosphoric acid ground phosphate rock by excess, and its procedure of processing is:
(1) ground phosphate rock, concentration 40%-50% purifying phosphoric acid, compound three kinds of materials of cleaner being added in reactive tank 1 stirring reaction 2.5-3.5 hour, reaction temperature controls at 100 103 DEG C；Subsequently into stirring reaction 2-3 hour in reactive tank 2, reaction temperature controls at 100-110 DEG C；Total reaction time 4-6 hour；Purifying phosphoric acid presses ground phosphate rock theoretical amount excess 50%-100%；Compound cleaner presses the theoretical amount excess 120% of fluorine in ground phosphate rock, and wherein reactive tank 1 presses theoretical amount addition, adds excessive portion in deblending slot；Compound cleaner is made up of phosphorus pentasulfide and active silica, and its quality proportioning is: phosphorus pentasulfide: active silica=2:7-9；
(2) material after having reacted in reactive tank 2 is sent in deblending slot, removed continuously in slip by low level flash condenser and enter after impurity in neutralization chamber, add in nertralizer Paris white at this and the phosphoric acid of excess, slip is after neutralization chamber enters accurate adjustment groove further accurate adjustment pH to 2.8-3.0, conveying goes to be spray-dried prepared dalcium biphosphate semi-finished product, is finished product after drum drier is further dried；
Described purifying phosphoric acid and Paris white have to comply with the prescription of calcium hydrogen phosphate fodder, and ground phosphate rock fineness is crossed 200 mesh and is more than 95%, and Paris white fineness crosses 100 mesh more than 95%；
The described low level flash condenser that passes through in deblending slot removes impurity in slip continuously, and its process conditions are gauge pressure 7MPa for controlling low level flash condenser vacuum.The described low level flash condenser that passes through in deblending slot removes impurity in slip continuously, and its process conditions are gauge pressure 7MPa for controlling the cold vacuum of low level flash distillation.
The dalcium biphosphate color utilizing the present invention to produce is canescence or light yellow.
Advantage: it is short that the present invention has technological process, can effectively utilize part calcium constituent in phosphorus ore, reduce sulfuric acid dosage simultaneously, energy-saving and cost-reducing, and existing manufacture method compared, has bigger cost advantage.
Figure of description
Fig. 1 is production technological process of the present invention.
Detailed description of the invention
Its procedure of processing is:
(1) ground phosphate rock, concentration 35% purifying phosphoric acid, compound three kinds of materials of cleaner being added stirring reaction 3 hours in reactive tank 1, reaction temperature controls at 110 DEG C；Subsequently into stirring reaction 2.5 hours in reactive tank 2, reaction temperature controls at 110 DEG C；The process conditions optimized are total reaction time 5 hours, wherein stirring reaction 3 hours in reactive tank 1, and reaction temperature controls at 103 DEG C；Stirring reaction 1.5 hours in reactive tank 2, reaction temperature controls at 108 DEG C；Concentration is that 30%-50% purifying phosphoric acid is by ground phosphate rock theoretical amount excess 80%；Compound cleaner presses the theoretical amount excess 120% of fluorine in ground phosphate rock, and compound cleaner is made up of phosphorus pentasulfide and active silica, and its quality proportioning is: phosphorus pentasulfide: active silica=2:8；
(2) material after having reacted in reactive tank 2 is sent in deblending slot, removed continuously in slip by low level flash condenser and enter after impurity in neutralization chamber, add in nertralizer Paris white at this and the phosphoric acid of excess, slip is after neutralization chamber enters accurate adjustment groove further accurate adjustment pH to 2.8-3.0, conveying goes to be spray-dried prepared dalcium biphosphate semi-finished product, being finished product after drum drier is further dried, the waste gas containing fluoride water produced in reaction makes fluorine finished product with alkali liquor absorption after absorbing again.
Purifying phosphoric acid and Paris white have to comply with the prescription of calcium hydrogen phosphate fodder, and phosphorus ore fineness is crossed 200 mesh and is more than 95%, and Paris white fineness is crossed 100 mesh and is more than 95%, and its process conditions optimized are phosphoric acid concentration 42%, by ground phosphate rock theoretical amount excess 80%.
Its process conditions optimized of described compound cleaner are by the theory excess 120% of fluorine in ground phosphate rock.Wherein the first reactive tank presses theoretical amount addition, adds excessive portion in deblending slot.
The described low level flash condenser that passes through in deblending slot removes impurity in slip continuously, and its process conditions optimized are gauge pressure 7MPa for controlling the cold vacuum of low level flash distillation.
Reaction mechanism is as follows:
7H3PO4+Ca5F
(PO4) 3 ——5Ca(H2PO4) 2+HF 。
Claims (1)
1. the method producing feed-level calcium biphosphate, it is characterised in that its processing method is the acid decomposed by phosphoric acid ground phosphate rock by excess, and its procedure of processing is:
(1) ground phosphate rock, concentration 40%-50% purifying phosphoric acid, compound three kinds of materials of cleaner being added in stirring reaction 2.5-3.5 hour in reactive tank (1), reaction temperature controls at 100 103 DEG C；Subsequently into stirring reaction 1.5 hours in reactive tank (2), reaction temperature controls at 105-110 DEG C；Total reaction time 4-6 hour；Purifying phosphoric acid presses ground phosphate rock theoretical amount excess 50%-100%；Compound cleaner presses the theoretical amount excess 120% of fluorine in ground phosphate rock, and wherein reactive tank (1) presses theoretical amount addition, adds excessive portion in deblending slot；Compound cleaner is made up of phosphorus pentasulfide and active silica, and its quality proportioning is: phosphorus pentasulfide: active silica=2:7-9；
(2) material after having reacted in reactive tank (2) is sent in deblending slot, removed continuously in slip by low level flash condenser and enter after impurity in neutralization chamber, add in nertralizer Paris white at this and the phosphoric acid of excess, slip is after neutralization chamber enters accurate adjustment groove further accurate adjustment pH to 2.8-3.0, conveying goes to be spray-dried prepared dalcium biphosphate semi-finished product, is finished product after drum drier is further dried；
Described purifying phosphoric acid and Paris white have to comply with the prescription of calcium hydrogen phosphate fodder, and ground phosphate rock fineness is crossed 200 mesh and is more than 95%, and Paris white fineness crosses 100 mesh more than 95%；
The described low level flash condenser that passes through in deblending slot removes impurity in slip continuously, and its process conditions are gauge pressure 7MPa for controlling low level flash condenser vacuum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004309.2A CN104495775B (en) | 2015-01-06 | 2015-01-06 | A kind of method producing feed-level calcium biphosphate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004309.2A CN104495775B (en) | 2015-01-06 | 2015-01-06 | A kind of method producing feed-level calcium biphosphate |
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| Publication Number | Publication Date |
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| CN104495775A CN104495775A (en) | 2015-04-08 |
| CN104495775B true CN104495775B (en) | 2016-08-31 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105921259B (en) * | 2016-05-09 | 2018-07-31 | 贵州省冶金化工研究所 | The method for producing feed-level calcium biphosphate using middle-low grade mixing rock phosphate in powder |
| CN106111532A (en) * | 2016-06-28 | 2016-11-16 | 四川省汉源化工总厂 | A kind of stage division of feed-level calcium biphosphate |
| CN108455545B (en) * | 2018-02-01 | 2021-09-10 | 连云港西都食品配料有限公司 | Preparation method of monocalcium phosphate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4222990A (en) * | 1974-10-07 | 1980-09-16 | Pennzoil Company | Production of fluoride-free phosphates |
| CN100595136C (en) * | 2008-04-11 | 2010-03-24 | 四川川恒化工股份有限公司 | Method for producing feed-grade calcium phosphate |
| CN101597040B (en) * | 2009-07-01 | 2011-05-25 | 侯炎学 | Method for producing food grade phosphoric acid with refined wet phosphoric acid and product thereof |
| CN102167301B (en) * | 2011-03-17 | 2013-02-06 | 贵州川恒化工有限责任公司 | Production method for co-production of high-water-solubility feed grade calcium phosphate and purified phosphoric acid |
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Granted publication date: 20160831 |