CN108529583A - A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate - Google Patents
A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate Download PDFInfo
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- CN108529583A CN108529583A CN201810665901.0A CN201810665901A CN108529583A CN 108529583 A CN108529583 A CN 108529583A CN 201810665901 A CN201810665901 A CN 201810665901A CN 108529583 A CN108529583 A CN 108529583A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The present invention discloses a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate.Ferric chloride solution is uniformly mixed with liquor alumini chloridi, ferro-aluminum mixed solution is obtained, adds ammonium chloride；Urea is added in ferro-aluminum mixed solution, heating is stirred to react, and iron aluminum precipitation object is obtained by filtration；Pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate, filtrate and filter residue is obtained by filtration；By filter residue plus water slurry, the pH of phosphorus acid-conditioning solution is then added, temperature reaction dries the material after washing by microwave dryer, by screening except iron obtains LITHIUM BATTERY bigger serface ferric phosphate.A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate of the present invention, simple for process, it is 60 100m to obtain specific surface area2The Large ratio surface ferric phosphate of/g, and be loose and porous structure, apparent density is 0.15 0.25g/mL, and primary particle size is 20nm or so.
Description
Technical field
The present invention relates to a kind of preparation processes of LITHIUM BATTERY bigger serface ferric phosphate, belong to new energy battery material neck
Domain.
Background technology
Ferric phosphate also known as high ferric phosphate, ferric orthophosphate, molecular formula FePO4 are a kind of white, canescence monoclinic crystals
Powder.It is the salt of iron salt solutions and sodium phosphate effect, iron therein is positive trivalent.Its main application is to manufacture LiFePO4 electricity
Pond material, catalyst and ceramics etc..
The color of the phosphate dihydrate iron of high-purity is near-white or shallow (light) yellow-white powder, with the loss of the crystallization water,
Color gradually turns yellow, and pure anhydride is in yellow-white powder.
With the large-scale use of ferric phosphate lithium cell, ferric phosphate as lithium iron phosphate positive material primary raw material,
Demand greatly improves, it is contemplated that annual demand is more than 50,000 tons.
With the progress and development of LiFePO 4 material, the LiFePO4 of high-pressure solid and high electrical performance becomes Future Development
The specific surface area of mainstream, presoma is bigger, then it is more abundant with reacting for lithium salts, and the compacting of finally obtained LiFePO4 is just
It is higher, while electrical property is also better.
The specific surface area of conventional ferric phosphate is generally 26-32m at present2Between/g, it can not meet future to ferric phosphate
The requirement of specific surface area.
Invention content
In view of this, the present invention provides a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate, it is simple for process, it obtains
It is 60-100m to specific surface area2The Large ratio surface ferric phosphate of/g, and be loose and porous structure, apparent density 0.15-0.25g/
ML, primary particle size are 20nm or so.
The present invention solves above-mentioned technical problem by following technological means：
A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate of the present invention, is following steps：
(1) ferric chloride solution is uniformly mixed with liquor alumini chloridi, obtains ferro-aluminum mixed solution, sulfuric acid regulation solution is added
PH be 0.5-1, add ammonium chloride and so that chloride ion content in solution is 4-6mol/L；
(2) urea is added in the ferro-aluminum mixed solution for obtaining step (1), is mixed evenly, then heating to temperature is
95-105 DEG C, the iron content into supernatant is stirred to react less than reaction is stopped after 50mg/L, by filtering after taking-up, obtains iron
Aluminum precipitation object；
(3) pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate,
It is 2-3 hours that the time, which is added, is 65-85 DEG C of reaction in temperature, the pH of maintenance process is 2-3, and the phosphate radical and iron aluminium of addition are heavy
The molar ratio of iron aluminium in starch is 1.05-1.1：1, it then filters, obtains filtrate and filter residue；
(4) filter residue that step (3) obtains is added into water slurry, the pH that phosphorus acid-conditioning solution is then added is 1-1.5, is warming up to
Temperature is 90-95 DEG C, and reaction is filtered after 1-2 hours, washs, the material after washing is dried by microwave dryer, through sieving
Divide except iron obtains LITHIUM BATTERY bigger serface ferric phosphate.
The molar ratio of iron aluminium is 4-6 in the step (1):1.
The urea being added in the step (2) is 5-6 times of iron aluminium total mole number, and the filtrate obtained after filtering is by concentration
Crystallization obtains ammonium chloride, and return to step (1) uses.
In the step (3) in mixed solution phosphoric acid a concentration of 1-1.2mol/L, a concentration of 0.2- of ammonium dihydrogen phosphate
0.3mol/L, it is 5.5-6.5 that obtained filtrate, which is added ammonium hydroxide and adjusts the pH of solution, is then filtered, and ammonium hydroxide, which is added, in filtrate is adjusted
The pH of solution is 7.0-7.3, obtains ammonium dihydrogen phosphate by condensing crystallizing, return to step (3) uses, and obtained aluminium hydroxide is heavy
The addition dissolving with hydrochloric acid that forms sediment obtains aluminium chloride, and return to step (1) uses.
Make that solid content is 25-30% in the step (4) when filter residue pulp, the mother liquor of filtering and the washings of washing are mixed
After conjunction after nanofiltration membrane concentrates, phosphoric acid solution use is done in return.
Drying temperature in the step (4) when microwave drying is 80-85 DEG C.
By the way that iron aluminium to be formed to the co-precipitation of iron aluminium, phosphoric acid is added so that iron and phosphatase reaction obtain ferric phosphate, and aluminium
It can be gradually dissolved into solution, to form loose porous ferric phosphate precipitation so that large specific surface area, while being turned by precipitation
Change, the small ferric phosphate of primary particle size is converted to precipitate by the small iron hydroxide of primary particle size, obtained ferric phosphate it is primary
Grain size only has 20nm or so.The ferric phosphate large specific surface area of the present invention simultaneously, activity is high, with lithium salts mixed process, reaction fills
Point, the reaction time is short, and obtained LiFePO4 compacted density is high, and chemical property is good.
The waste water generated during the present invention is each can be returned by condensing crystallizing or other processing, obtained product
It returns and uses, to reduce manufacturing cost.
The beneficial effects of the invention are as follows：Simple for process, it is 60-100m to obtain specific surface area2The Large ratio surface ferric phosphate of/g,
And be loose and porous structure, apparent density 0.15-0.25g/mL, primary particle size is 20nm or so, and narrow particle size distribution.
Specific implementation mode
Below with reference to specific embodiment, the present invention is described in detail, a kind of LITHIUM BATTERY Large ratio surface of the present embodiment
The preparation process of product ferric phosphate, is following steps：
(1) ferric chloride solution is uniformly mixed with liquor alumini chloridi, obtains ferro-aluminum mixed solution, sulfuric acid regulation solution is added
PH be 0.5-1, add ammonium chloride and so that chloride ion content in solution is 4-6mol/L；
(2) urea is added in the ferro-aluminum mixed solution for obtaining step (1), is mixed evenly, then heating to temperature is
95-105 DEG C, the iron content into supernatant is stirred to react less than reaction is stopped after 50mg/L, by filtering after taking-up, obtains iron
Aluminum precipitation object；
(3) pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate,
It is 2-3 hours that the time, which is added, is 65-85 DEG C of reaction in temperature, the pH of maintenance process is 2-3, and the phosphate radical and iron aluminium of addition are heavy
The molar ratio of iron aluminium in starch is 1.05-1.1：1, it then filters, obtains filtrate and filter residue；
(4) filter residue that step (3) obtains is added into water slurry, the pH that phosphorus acid-conditioning solution is then added is 1-1.5, is warming up to
Temperature is 90-95 DEG C, and reaction is filtered after 1-2 hours, washs, the material after washing is dried by microwave dryer, through sieving
Divide except iron obtains LITHIUM BATTERY bigger serface ferric phosphate.
The molar ratio of iron aluminium is 4-6 in the step (1):1.
The urea being added in the step (2) is 5-6 times of iron aluminium total mole number, and the filtrate obtained after filtering is by concentration
Crystallization obtains ammonium chloride, and return to step (1) uses.
In the step (3) in mixed solution phosphoric acid a concentration of 1-1.2mol/L, a concentration of 0.2- of ammonium dihydrogen phosphate
0.3mol/L, it is 5.5-6.5 that obtained filtrate, which is added ammonium hydroxide and adjusts the pH of solution, is then filtered, and ammonium hydroxide, which is added, in filtrate is adjusted
The pH of solution is 7.0-7.3, obtains ammonium dihydrogen phosphate by condensing crystallizing, return to step (3) uses, and obtained aluminium hydroxide is heavy
The addition dissolving with hydrochloric acid that forms sediment obtains aluminium chloride, and return to step (1) uses.
Make that solid content is 25-30% in the step (4) when filter residue pulp, the mother liquor of filtering and the washings of washing are mixed
After conjunction after nanofiltration membrane concentrates, phosphoric acid solution use is done in return.
Drying temperature in the step (4) when microwave drying is 80-85 DEG C.
Embodiment 1
A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate, is following steps：
(1) ferric chloride solution is uniformly mixed with liquor alumini chloridi, obtains ferro-aluminum mixed solution, sulfuric acid regulation solution is added
PH be 0.8, add ammonium chloride and so that chloride ion content in solution is 5.1mol/L；
(2) urea is added in the ferro-aluminum mixed solution for obtaining step (1), is mixed evenly, then heating to temperature is
99 DEG C, the iron content into supernatant is stirred to react less than reaction is stopped after 50mg/L, by filtering after taking-up, it is heavy to obtain iron aluminium
Starch；
(3) pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate,
It is 2.3 hours that the time, which is added, is 80 DEG C of reactions in temperature, the pH of maintenance process is 2.8, phosphate radical and the iron aluminum precipitation object of addition
In iron aluminium molar ratio be 1.08：1, it then filters, obtains filtrate and filter residue；
(4) filter residue that step (3) obtains is added into water slurry, the pH that phosphorus acid-conditioning solution is then added is 1.2, is warming up to temperature
Degree is 93 DEG C, and reaction is filtered after 1.5 hours, washs, the material after washing is dried by microwave dryer, and iron is removed by screening
Obtain LITHIUM BATTERY bigger serface ferric phosphate.
The molar ratio of iron aluminium is 5 in the step (1):1.
The urea being added in the step (2) is 5.5 times of iron aluminium total mole number, and the filtrate obtained after filtering is by concentration
Crystallization obtains ammonium chloride, and return to step (1) uses.
In the step (3) in mixed solution phosphoric acid a concentration of 1.1mol/L, ammonium dihydrogen phosphate it is a concentration of
0.25mol/L, it is 6.1 that obtained filtrate, which is added ammonium hydroxide and adjusts the pH of solution, is then filtered, and ammonium hydroxide, which is added, in filtrate adjusts solution
PH be 7.1, obtain ammonium dihydrogen phosphate by condensing crystallizing, return to step (3) uses, and salt is added in obtained aluminum hydroxide precipitation
Acid dissolving obtains aluminium chloride, and return to step (1) uses.
Make that solid content is 28% in the step (4) when filter residue pulp, the mother liquor of filtering is mixed with the washings of washing
Afterwards after nanofiltration membrane concentrates, phosphoric acid solution use is done in return.
Drying temperature in the step (4) when microwave drying is 83 DEG C.
Finally obtained ferric phosphate index is as follows：
| Index | Iron content | Iron phosphorus molar ratio | D10 | D50 | D90 |
| Numerical value | 28.96% | 0.997 | 210nm | 550nm | 730nm |
| BET | Ca | Mg | Na | Apparent density | Primary particle size |
| 75m2/g | 6ppm | 4ppm | 3ppm | 0.18g/mL | 22nm |
Embodiment 2
A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate, is following steps：
(1) ferric chloride solution is uniformly mixed with liquor alumini chloridi, obtains ferro-aluminum mixed solution, sulfuric acid regulation solution is added
PH be 0.7, add ammonium chloride and so that chloride ion content in solution is 5.5mol/L；
(2) urea is added in the ferro-aluminum mixed solution for obtaining step (1), is mixed evenly, then heating to temperature is
102 DEG C, the iron content into supernatant is stirred to react less than reaction is stopped after 50mg/L, by filtering after taking-up, obtains iron aluminium
Sediment；
(3) pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate,
It is 2.5 hours that the time, which is added, is 75 DEG C of reactions in temperature, the pH of maintenance process is 2.5, phosphate radical and the iron aluminum precipitation object of addition
In iron aluminium molar ratio be 1.08：1, it then filters, obtains filtrate and filter residue；
(4) filter residue that step (3) obtains is added into water slurry, the pH that phosphorus acid-conditioning solution is then added is 1.3, is warming up to temperature
Degree is 93 DEG C, and reaction is filtered after 1.5 hours, washs, the material after washing is dried by microwave dryer, and iron is removed by screening
Obtain LITHIUM BATTERY bigger serface ferric phosphate.
The molar ratio of iron aluminium is 4.6 in the step (1):1.
The urea being added in the step (2) is 5.6 times of iron aluminium total mole number, and the filtrate obtained after filtering is by concentration
Crystallization obtains ammonium chloride, and return to step (1) uses.
In the step (3) in mixed solution phosphoric acid a concentration of 1.1mol/L, ammonium dihydrogen phosphate it is a concentration of
0.25mol/L, it is 6.3 that obtained filtrate, which is added ammonium hydroxide and adjusts the pH of solution, is then filtered, and ammonium hydroxide, which is added, in filtrate adjusts solution
PH be 7.2, obtain ammonium dihydrogen phosphate by condensing crystallizing, return to step (3) uses, and salt is added in obtained aluminum hydroxide precipitation
Acid dissolving obtains aluminium chloride, and return to step (1) uses.
Make that solid content is 29% in the step (4) when filter residue pulp, the mother liquor of filtering is mixed with the washings of washing
Afterwards after nanofiltration membrane concentrates, phosphoric acid solution use is done in return.
Drying temperature in the step (4) when microwave drying is 82 DEG C.
Finally obtained ferric phosphate index is as follows：
| Index | Iron content | Iron phosphorus molar ratio | D10 | D50 | D90 |
| Numerical value | 28.95% | 0.998 | 225nm | 559nm | 778nm |
| BET | Ca | Mg | Na | Apparent density | Primary particle size |
| 78m2/g | 8ppm | 3ppm | 5ppm | 0.17g/mL | 21nm |
Embodiment 3
A kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate, is following steps：
(1) ferric chloride solution is uniformly mixed with liquor alumini chloridi, obtains ferro-aluminum mixed solution, sulfuric acid regulation solution is added
PH be 0.75, add ammonium chloride and so that chloride ion content in solution is 5.2mol/L；
(2) urea is added in the ferro-aluminum mixed solution for obtaining step (1), is mixed evenly, then heating to temperature is
99 DEG C, the iron content into supernatant is stirred to react less than reaction is stopped after 50mg/L, by filtering after taking-up, it is heavy to obtain iron aluminium
Starch；
(3) pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate,
It is 2.7 hours that the time, which is added, is 82 DEG C of reactions in temperature, the pH of maintenance process is 2.5, phosphate radical and the iron aluminum precipitation object of addition
In iron aluminium molar ratio be 1.07：1, it then filters, obtains filtrate and filter residue；
(4) filter residue that step (3) obtains is added into water slurry, the pH that phosphorus acid-conditioning solution is then added is 1.6, is warming up to temperature
Degree is 93 DEG C, and reaction is filtered after 1.5 hours, washs, the material after washing is dried by microwave dryer, and iron is removed by screening
Obtain LITHIUM BATTERY bigger serface ferric phosphate.
The molar ratio of iron aluminium is 5.2 in the step (1):1.
The urea being added in the step (2) is 5.3 times of iron aluminium total mole number, and the filtrate obtained after filtering is by concentration
Crystallization obtains ammonium chloride, and return to step (1) uses.
In the step (3) in mixed solution phosphoric acid a concentration of 1.1mol/L, ammonium dihydrogen phosphate it is a concentration of
0.25mol/L, it is 5.9 that obtained filtrate, which is added ammonium hydroxide and adjusts the pH of solution, is then filtered, and ammonium hydroxide, which is added, in filtrate adjusts solution
PH be 7.2, obtain ammonium dihydrogen phosphate by condensing crystallizing, return to step (3) uses, and salt is added in obtained aluminum hydroxide precipitation
Acid dissolving obtains aluminium chloride, and return to step (1) uses.
Make that solid content is 28% in the step (4) when filter residue pulp, the mother liquor of filtering is mixed with the washings of washing
Afterwards after nanofiltration membrane concentrates, phosphoric acid solution use is done in return.
Drying temperature in the step (4) when microwave drying is 83 DEG C.
Finally obtained ferric phosphate index is as follows：
| Index | Iron content | Iron phosphorus molar ratio | D10 | D50 | D90 |
| Numerical value | 30.01% | 1.00 | 225nm | 568nm | 729nm |
| BET | Ca | Mg | Na | Apparent density | Primary particle size |
| 83m2/g | 4ppm | 6ppm | 2ppm | 0.19g/mL | 24nm |
Ferric phosphate product mix lithium carbonate in embodiment 1,2,3 is sintered and prepares LiFePO4, while using normal
The liquid phase synthesis ferric phosphate mixed carbonic acid lithium of rule, which is sintered, prepares LiFePO4, and performance comparison is as follows：
Finally illustrate, the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although with reference to compared with
Good embodiment describes the invention in detail, it will be understood by those of ordinary skill in the art that, it can be to the skill of the present invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the right of invention.
Claims (6)
1. a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate, which is characterized in that be following steps：
(1) ferric chloride solution is uniformly mixed with liquor alumini chloridi, obtains ferro-aluminum mixed solution, the pH of sulfuric acid regulation solution is added
For 0.5-1, adds ammonium chloride and so that the chloride ion content in solution is 4-6mol/L；
(2) urea is added in the ferro-aluminum mixed solution for obtaining step (1), is mixed evenly, and it is 95- to then heat to temperature
105 DEG C, the iron content into supernatant is stirred to react less than reaction is stopped after 50mg/L, by filtering after taking-up, obtains iron aluminium
Sediment；
(3) pure water pulp is added in iron aluminum precipitation object, then is added in pulp material after phosphoric acid is mixed with ammonium dihydrogen phosphate, is added
Time is 2-3 hours, is 65-85 DEG C of reaction in temperature, the pH of maintenance process is 2-3, phosphate radical and the iron aluminum precipitation object of addition
In iron aluminium molar ratio be 1.05-1.1：1, it then filters, obtains filtrate and filter residue；
(4) filter residue that step (3) obtains is added into water slurry, the pH that phosphorus acid-conditioning solution is then added is 1-1.5, is warming up to temperature
It it is 90-95 DEG C, reaction is filtered after 1-2 hours, washs, the material after washing is dried by microwave dryer, is removed by screening
Iron obtains LITHIUM BATTERY bigger serface ferric phosphate.
2. a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate according to claim 1, it is characterised in that：It is described
The molar ratio of iron aluminium is 4-6 in step (1):1.
3. a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate according to claim 1, it is characterised in that：It is described
The urea being added in step (2) is 5-6 times of iron aluminium total mole number, and the filtrate obtained after filtering obtains chlorination by condensing crystallizing
Ammonium, return to step (1) use.
4. a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate according to claim 1, it is characterised in that：It is described
In step (3) in mixed solution phosphoric acid a concentration of 1-1.2mol/L, a concentration of 0.2-0.3mol/L of ammonium dihydrogen phosphate obtains
Filtrate be added ammonium hydroxide adjust solution pH be 5.5-6.5, then filter, by filtrate be added ammonium hydroxide adjust solution pH be 7.0-
7.3, ammonium dihydrogen phosphate is obtained by condensing crystallizing, return to step (3) uses, and dissolving with hydrochloric acid is added in obtained aluminum hydroxide precipitation
Aluminium chloride is obtained, return to step (1) uses.
5. a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate according to claim 1, it is characterised in that：It is described
Make when filter residue pulp in step (4) solid content be 25-30%, the mother liquor of filtering mixed with the washings of washing after by nanofiltration
After membrane filtration concentration, phosphoric acid solution use is done in return.
6. a kind of preparation process of LITHIUM BATTERY bigger serface ferric phosphate according to claim 1, it is characterised in that：It is described
Drying temperature in step (4) when microwave drying is 80-85 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642235A (en) * | 2019-10-25 | 2020-01-03 | 湖北万润新能源科技发展有限公司 | Preparation method of core-shell structure battery-grade anhydrous iron phosphate |
| CN115259119A (en) * | 2022-07-06 | 2022-11-01 | 北京水木方科技有限公司 | Method for continuously preparing battery-grade iron phosphate by using ferrous chloride |
| CN115535981A (en) * | 2022-09-13 | 2022-12-30 | 中国科学院广州地球化学研究所 | Method for preparing hydroxyapatite with large specific surface area at normal temperature |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692488A (en) * | 2009-09-11 | 2010-04-07 | 河南新飞科隆电源有限公司 | Method for synthesizing iron phosphate with doped metallic elements |
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2018
- 2018-06-26 CN CN201810665901.0A patent/CN108529583A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692488A (en) * | 2009-09-11 | 2010-04-07 | 河南新飞科隆电源有限公司 | Method for synthesizing iron phosphate with doped metallic elements |
Non-Patent Citations (1)
| Title |
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| 赵玉萍: "《土壤化学》", 30 June 1991 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642235A (en) * | 2019-10-25 | 2020-01-03 | 湖北万润新能源科技发展有限公司 | Preparation method of core-shell structure battery-grade anhydrous iron phosphate |
| CN115259119A (en) * | 2022-07-06 | 2022-11-01 | 北京水木方科技有限公司 | Method for continuously preparing battery-grade iron phosphate by using ferrous chloride |
| CN115259119B (en) * | 2022-07-06 | 2024-02-27 | 北京水木方科技有限公司 | Method for continuously preparing battery-grade ferric phosphate by using ferrous chloride |
| CN115535981A (en) * | 2022-09-13 | 2022-12-30 | 中国科学院广州地球化学研究所 | Method for preparing hydroxyapatite with large specific surface area at normal temperature |
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