CN1064330C - Method for leaching phosphate from low-grade powdered rock phosphate - Google Patents
Method for leaching phosphate from low-grade powdered rock phosphate Download PDFInfo
- Publication number
- CN1064330C CN1064330C CN97121643A CN97121643A CN1064330C CN 1064330 C CN1064330 C CN 1064330C CN 97121643 A CN97121643 A CN 97121643A CN 97121643 A CN97121643 A CN 97121643A CN 1064330 C CN1064330 C CN 1064330C
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- CN
- China
- Prior art keywords
- phosphate
- leaching
- grade
- low
- calcium
- 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 - Fee Related
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- 238000002386 leaching Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002367 phosphate rock Substances 0.000 title claims abstract description 14
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 6
- 239000010452 phosphate Substances 0.000 title claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 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 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011575 calcium Substances 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims abstract description 9
- 235000019700 dicalcium phosphate Nutrition 0.000 claims abstract description 9
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 5
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 5
- 239000004571 lime Substances 0.000 claims abstract description 5
- 239000008267 milk Substances 0.000 claims abstract description 5
- 210000004080 milk Anatomy 0.000 claims abstract description 5
- 235000013336 milk Nutrition 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000004579 marble Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000000643 oven drying Methods 0.000 claims abstract description 3
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims abstract 2
- 238000007865 diluting Methods 0.000 claims abstract 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims description 2
- 239000004568 cement Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 230000003301 hydrolyzing effect Effects 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- 238000006115 defluorination reaction Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 239000000606 toothpaste Substances 0.000 abstract description 2
- 229940034610 toothpaste Drugs 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 3
- 239000002686 phosphate fertilizer Substances 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- -1 potassium fluorosilicate Chemical compound 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for leaching and synthesizing phosphate by low-grade powdered rock phosphate, which is characterized in that the low-grade powdered rock phosphate is leached by sulfuric acid, and 2 percent of SiO is added2And 4% of KCl for defluorination, calcining marble, digesting, diluting to obtain lime milk containing 15% of calcium, adding into phosphoric acid, stirring, press-filtering, oven-drying and pulverizing to obtain feed-grade calcium hydrogen phosphate, if sectional synthesis is adopted, firstly synthesizing feed-grade calcium hydrogen phosphate, and then synthesizing calcium hydrogen phosphate for toothpaste, medicine and food.
Description
The invention relates to a method for directly synthesizing calcium hydrophosphate by deep processing and leaching low-grade phosphorite.
At present, the phosphorus and phosphate deficiency in north China is in short supply, especially the feed grade calcium hydrophosphate in recent years. The traditional process for producing calcium hydrogen phosphate is to synthesize calcium hydrogen phosphate by removing impurities from phosphoric acid. In the research of secondary defluorination for producing feed-grade calcium hydrophosphate, which is published in the fourth stage 1-4 of 1991 of inorganic salt industry, the process of the method is to leach phosphate fertilizer and synthesize calcium hydrophosphate by secondary impurity removal. The disadvantages are that: the phosphate fertilizer is firstly bought and synthesized by water immersion and secondary impurity removal, the process is complex and needs two manufacturers to complete the process. The cost is high.
The invention aims to provide a method for directly synthesizing calcium hydrophosphate by leaching low-grade powdered rock phosphate and removing impurities.
The technical solution of the invention comprises the following steps:
leaching: with P2O5Heating 20% of phosphate rock powder at a solid-liquid ratio of 1: 2, stirring at 80-100 ℃, adding industrial sulfuric acid for leaching, and dripping sulfuric acid until the pH value is equal to 2, wherein the main reaction formula is as follows:
and (3) fluorine removal: 2% SiO is added in the later stage of leaching2And 4% KCl to convert fluorine to potassium fluorosilicate, which has the formula:
preparing calcium: the marble is calcined, heated and hydrolyzed, passes through a cement bridge, a drum sieve, a hydrocyclone and a 200-mesh sieve, and is diluted to lime milk containing 15 percent of calcium.
Synthesizing: adding lime milk into 35-40 deg.C phosphoric acid, stirring, adding acid until pH is 6.8, aging for 30 min, press filtering, rapidly oven drying, pulverizing to obtain feed grade calcium hydrogen phosphate, and synthesizing by stages to obtain feed grade calcium hydrogen phosphate, wherein the filtrate contains part of phosphoric acid and calcium, and preparing into toothpaste, medicine and food grade calcium hydrogen phosphate.
And (4) leaching the low-grade phosphate rock powder twice or three times until the concentration of phosphoric acid reaches 20-40%.
The invention has the advantages that:
1. further develops low-grade phosphorite resources, changes the indigestion products into delicateness commodities, and drives raw materials such as marble, coal and the like to be commercialized at the same time.
2. The products are transported in a long distance, are three local commodities which are locally processed and digested from the raw materials in the north, and reduce the product cost.
3. The low-grade ground phosphate rock is leached and then simultaneously subjected to impurity removal, so that the calcium hydrophosphate is directly synthesized, the process is simple, the cost is low, and the effect is quick.
Claims (2)
1. The method for leaching phosphate from low-grade powdered rock phosphate is characterized by comprising the following steps: the method comprises the following steps:
leaching: with P2O5Heating 20% of phosphate rock powder at a solid-to-liquid ratio of 1: 2, stirring at 80-100 ℃, adding industrial sulfuric acid for leaching, and dripping sulfuric acid until the pH value is equal to 2;
and (3) fluorine removal: 2% SiO is added in the later stage of leaching2And 4% KCl to make fluorine become potassium fluosilicate, and precipitate in the filter residue;
preparing calcium: calcining marble, heating, hydrolyzing, sieving with a cement bridge, a drum sieve, a hydrocyclone, a 200-mesh sieve, and diluting to lime milk containing 15% of calcium;
synthesizing: adding lime milk into phosphoric acid at 35-40 deg.C, stirring, stopping adding acid until pH is 6.8, aging for 30 min, press filtering, rapidly oven drying, and pulverizing to obtain feed grade calcium hydrogen phosphate.
2. The method for leaching phosphate from low-grade powdered rock phosphate according to claim 1, characterized in that: and (4) leaching the low-grade phosphate rock powder twice or three times until the concentration of phosphoric acid reaches 20-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121643A CN1064330C (en) | 1997-11-20 | 1997-11-20 | Method for leaching phosphate from low-grade powdered rock phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121643A CN1064330C (en) | 1997-11-20 | 1997-11-20 | Method for leaching phosphate from low-grade powdered rock phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1218003A CN1218003A (en) | 1999-06-02 |
| CN1064330C true CN1064330C (en) | 2001-04-11 |
Family
ID=5176344
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97121643A Expired - Fee Related CN1064330C (en) | 1997-11-20 | 1997-11-20 | Method for leaching phosphate from low-grade powdered rock phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1064330C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302129B (en) * | 2008-05-22 | 2011-11-30 | 东莞市施普旺生物科技有限公司 | Calcium hydrophosphate suspending agent |
| CN103723698B (en) * | 2013-11-25 | 2015-07-15 | 瓮福（集团）有限责任公司 | Method for reducing content of magnesium in feed grade calcium hydrophosphate |
| CN106882778A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method that toothpaste grade calcium hydrophosphate is prepared in micro passage reaction |
| CN114106837B (en) * | 2021-11-25 | 2023-11-21 | 中化农业（临沂）研发中心有限公司 | Saline-alkali soil conditioner containing polyphosphate and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4485078A (en) * | 1982-03-16 | 1984-11-27 | Agrico Chemical Company | Process for producing wet process phosphoric acid from phosphate rocks containing fluochlorapatite and related minerals |
| CN1048015A (en) * | 1990-02-17 | 1990-12-26 | 云南易门矿务局 | Low ratio acid wet method is produced calcium hydrophosphate fodder |
| CN1113880A (en) * | 1994-06-01 | 1995-12-27 | 龚家竹 | Method for extracting phosphoric acid and solution containing phosphate by sulfuric acid method |
-
1997
- 1997-11-20 CN CN97121643A patent/CN1064330C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4485078A (en) * | 1982-03-16 | 1984-11-27 | Agrico Chemical Company | Process for producing wet process phosphoric acid from phosphate rocks containing fluochlorapatite and related minerals |
| CN1048015A (en) * | 1990-02-17 | 1990-12-26 | 云南易门矿务局 | Low ratio acid wet method is produced calcium hydrophosphate fodder |
| CN1113880A (en) * | 1994-06-01 | 1995-12-27 | 龚家竹 | Method for extracting phosphoric acid and solution containing phosphate by sulfuric acid method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1218003A (en) | 1999-06-02 |
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