CN114229814A - Production method of lithium iron phosphate precursor - Google Patents
Production method of lithium iron phosphate precursor Download PDFInfo
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- CN114229814A CN114229814A CN202111457200.6A CN202111457200A CN114229814A CN 114229814 A CN114229814 A CN 114229814A CN 202111457200 A CN202111457200 A CN 202111457200A CN 114229814 A CN114229814 A CN 114229814A
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- iron phosphate
- lithium iron
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- phosphate precursor
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 34
- 239000002243 precursor Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 16
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 16
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 16
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 235000019837 monoammonium phosphate Nutrition 0.000 claims abstract description 6
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010902 jet-milling Methods 0.000 claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 abstract description 11
- 229910000398 iron phosphate Inorganic materials 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000005955 Ferric phosphate Substances 0.000 abstract description 3
- 229940032958 ferric phosphate Drugs 0.000 abstract description 3
- 229910000399 iron(III) phosphate Inorganic materials 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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Classifications
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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
-
- 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
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
A production method of a lithium iron phosphate precursor comprises the following steps: adding ferrous sulfate solution, ammonium dihydrogen phosphate solution, and oxygen water into the solution containing the base solution at the same time with a volume of 100m3Stirring in a reaction kettle for reaction, controlling the reaction temperature, controlling the reaction time, adding a phosphoric acid solution to control the pH of a reaction system after the reaction is finished, keeping the temperature, performing solid-liquid separation, washing, drying and calcining to obtain a lithium iron phosphate precursor, and performing jet milling and packaging to obtain a finished product of the lithium iron phosphate precursor. According to the invention, the lithium iron phosphate precursor ferric phosphate is produced by controlling the process conditions, and meanwhile, a large-volume reaction kettle is adopted, so that the batch uniformity and the stability are good, and meanwhile, the single kettle yield is 3m higher3The reaction kettle is 30 times higher, and the energy consumption of each ton of iron phosphate is reduced by more than 50%.
Description
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to a production method of a lithium iron phosphate precursor.
Background
The lithium iron phosphate material is used as the anode material of the lithium ion battery and is widely applied to the aspects of energy storage equipment, electric tools, power batteries for automobiles, mobile power supplies and the like. When preparing lithium iron phosphate, a lithium iron phosphate precursor ferric phosphate is generally prepared, and then the lithium iron phosphate precursor is sintered at a high temperature to obtain the lithium iron phosphate positive electrode material. At present, the production method of the lithium iron phosphate precursor is mainly to add a phosphorus source and an iron source into 3m3And 6m3The iron phosphate obtained by the method has the problems of insufficient batch uniformity, high energy consumption per unit of lithium iron phosphate precursor, huge cost and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a production method of a lithium iron phosphate precursor with good batch uniformity and low energy consumption.
The invention is realized by the following technical scheme.
A method for producing a lithium iron phosphate precursor, characterized by comprising:
(1) raw materials: ferrous sulfate solution with concentration of 1.0-1.5mol/L, ammonium dihydrogen phosphate solution with concentration of 1.1-1.6mol/L, hydrogen peroxide and 85% phosphoric acid solution;
(2) reaction: the flow rate is 12-15m3The flow rate of the ferrous sulfate solution is 12-15m3Ammonium dihydrogen phosphate solution/h with a flow rate of 1.0-1.5m3The volume of the hydrogen peroxide solution containing the base solution is 100m3Stirring in a reaction kettle for reaction, wherein the base solution is a ferrous sulfate solution, controlling the reaction temperature to be 50-60 ℃, the reaction time to be 1.5-2.0h, adding a phosphoric acid solution after the reaction is finished, controlling the pH of the reaction system to be 1.0-1.5, heating to 90-92 ℃, keeping the temperature for 2-3h, carrying out solid-liquid separation, washing, drying and calcining to obtain a lithium iron phosphate precursor (namely anhydrous iron phosphate), and carrying out air flow crushing and packaging to obtain a lithium iron phosphate precursor finished product.
Further, the adding amount of the base solution in the step (2) is 20-25% of the volume of the reaction kettle.
Further, the step (2) washing process comprises: washing for 5-6 times by deionized water at 90-92 ℃, wherein the solid-to-liquid ratio of each time is 1: 8-1:10.
Further, the step (2) is dried and calcined by a rotary kiln, the temperature is 600-650 ℃, and the calcination time is 4-6 hours.
The invention has the beneficial technical effects that the lithium iron phosphate precursor ferric phosphate is produced by controlling the process conditions, and the large-volume reaction kettle is adopted, so that the batch uniformity and the stability are good, and the single kettle yield is 3m higher than that of the single kettle3The reaction kettle is 30 times higher, and the energy consumption of each ton of iron phosphate is reduced by more than 50%. Finished product particle size D50: 1.0-3.2um, phosphorus-iron ratio: 1.01-1.03, morphology: spherical shape, S<0.02％。
Drawings
Figure 1 is an SEM image of iron phosphate prepared according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
A production method of a lithium iron phosphate precursor comprises the following steps:
(1) raw materials: the concentration of ferrous sulfate solution is 1.0mol/L, the concentration of ammonium dihydrogen phosphate solution is 1.1mol/L, hydrogen peroxide and 85% phosphoric acid solution;
(2) reaction: the flow rate is 12m3Per hour ferrous sulfate solution with flow rate of 15m3Ammonium dihydrogen phosphate solution/h, flow 1.0m3Hydrogen peroxide solution with the concentration of 20m is added at the same time3The volume of the base liquid is 100m3Stirring in a reaction kettle for reaction, wherein a base solution is a ferrous sulfate solution, the reaction temperature is controlled to be 50 ℃, the reaction time is 1.5h, after the reaction is finished, adding a phosphoric acid solution to control the pH of a reaction system to be 1.0-1.1, heating to 90 ℃, keeping the temperature for 2h, quickly performing solid-liquid separation, washing for 5 times by using 90 ℃ deionized water, and the solid-liquid ratio of each time is 1: and 9, drying and calcining in a rotary kiln at the temperature of 600 ℃ for 4 hours to obtain a lithium iron phosphate precursor (namely anhydrous iron phosphate), and performing jet milling and packaging to obtain a finished product of the lithium iron phosphate precursor. Finished product particle size D50: 1.0um, phosphorus-iron ratio: 1.01, morphology:spherical shape, S0.0098%.
Example 2
A production method of a lithium iron phosphate precursor comprises the following steps:
(1) raw materials: the concentration of ferrous sulfate solution is 1.2mol/L, the concentration of ammonium dihydrogen phosphate solution is 1.3mol/L, hydrogen peroxide and 85% phosphoric acid solution;
(2) reaction: the flow rate is 15m3Per hour of ferrous sulfate solution with flow rate of 12m3Ammonium dihydrogen phosphate solution/h, flow 1.5m3Hydrogen peroxide solution with the concentration of 25m is added at the same time3The volume of the base liquid is 100m3Stirring in a reaction kettle for reaction, wherein a base solution is a ferrous sulfate solution, the reaction temperature is controlled to be 60 ℃, the reaction time is 1.7h, after the reaction is finished, adding a phosphoric acid solution to control the pH of a reaction system to be 1.1-1.3, heating to 92 ℃, keeping the temperature for 2.5h, quickly performing solid-liquid separation, washing for 6 times by using deionized water at 92 ℃, and the solid-liquid ratio of each time is 1: and 10, drying and calcining the mixture in a rotary kiln at the temperature of 610 ℃ for 5.5 hours to obtain a lithium iron phosphate precursor (namely anhydrous iron phosphate), and performing jet milling and packaging to obtain a finished product of the lithium iron phosphate precursor. Finished product particle size D50: 2.0um, phosphorus to iron ratio: 1.02, morphology: spherical shape, S0.0082%.
Example 3
A production method of a lithium iron phosphate precursor comprises the following steps:
(1) raw materials: the concentration of ferrous sulfate solution is 1.5mol/L, the concentration of ammonium dihydrogen phosphate solution is 1.6mol/L, hydrogen peroxide and 85% phosphoric acid solution;
(2) reaction: the flow rate is 13m3Per hour of ferrous sulfate solution with a flow of 13m3Ammonium dihydrogen phosphate solution/h, flow 1.3m3Hydrogen peroxide solution with the concentration of 20m is added at the same time3The volume of the base liquid is 100m3Stirring in a reaction kettle for reaction, wherein the base solution is a ferrous sulfate solution, the reaction temperature is controlled to be 55 ℃, the reaction time is 2 hours, after the reaction is finished, adding a phosphoric acid solution to control the pH of a reaction system to be 1.3-1.5, heating to 91 ℃, keeping the temperature for 2.5 hours, rapidly performing solid-liquid separation, washing for 5 times by using deionized water at 91 ℃, and the solid-liquid ratio of each time is 1: and 8, drying and calcining in a rotary kiln at 650 ℃ for 4.And 5 hours, obtaining a lithium iron phosphate precursor (namely anhydrous iron phosphate), and performing jet milling and packaging to obtain a finished product of the lithium iron phosphate precursor. Finished product particle size D50: 3.1um, phosphorus to iron ratio: 1.03, morphology: spherical shape, S0.0102%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (4)
1. A method for producing a lithium iron phosphate precursor, characterized by comprising:
(1) raw materials: ferrous sulfate solution with concentration of 1.0-1.5mol/L, ammonium dihydrogen phosphate solution with concentration of 1.1-1.6mol/L, hydrogen peroxide and 85% phosphoric acid solution;
(2) reaction: the flow rate is 12-15m3The flow rate of the ferrous sulfate solution is 12-15m3Ammonium dihydrogen phosphate solution/h with a flow rate of 1.0-1.5m3The volume of the hydrogen peroxide solution containing the base solution is 100m3Stirring in a reaction kettle for reaction, wherein the base solution is a ferrous sulfate solution, controlling the reaction temperature to be 50-60 ℃, the reaction time to be 1.5-2.0h, adding a phosphoric acid solution after the reaction is finished, controlling the pH of the reaction system to be 1.0-1.5, heating to 90-92 ℃, keeping the temperature for 2-3h, carrying out solid-liquid separation, washing, drying and calcining to obtain a lithium iron phosphate precursor, and carrying out jet milling and packaging to obtain a finished product of the lithium iron phosphate precursor.
2. The method for producing the lithium iron phosphate precursor according to claim 1, wherein the amount of the base solution added in the step (2) is 20-25% of the volume of the reaction kettle.
3. The method for producing a lithium iron phosphate precursor according to claim 1, wherein the washing step (2) comprises: washing for 5-6 times by deionized water at 90-92 ℃, wherein the solid-to-liquid ratio of each time is 1: 8-1:10.
4. The method for producing the lithium iron phosphate precursor according to claim 1, wherein the step (2) is carried out by drying and calcining in a rotary kiln at a temperature of 600-650 ℃ for 4-6 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102422467A (en) * | 2009-05-04 | 2012-04-18 | 觅科科技公司 | Electrode active composite materials and methods of making thereof |
| CN102515129A (en) * | 2011-12-20 | 2012-06-27 | 江苏中电长迅能源材料有限公司 | Preparation method for submicron battery-grade ferric phosphate |
| CN106981656A (en) * | 2017-05-13 | 2017-07-25 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of LITHIUM BATTERY iron manganese phosphate |
| CN109205584A (en) * | 2018-10-09 | 2019-01-15 | 湖南雅城新材料有限公司 | A kind of preparation method of high-speed rail phosphorus than ferric phosphate |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
-
2021
- 2021-12-02 CN CN202111457200.6A patent/CN114229814A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102422467A (en) * | 2009-05-04 | 2012-04-18 | 觅科科技公司 | Electrode active composite materials and methods of making thereof |
| CN102515129A (en) * | 2011-12-20 | 2012-06-27 | 江苏中电长迅能源材料有限公司 | Preparation method for submicron battery-grade ferric phosphate |
| CN106981656A (en) * | 2017-05-13 | 2017-07-25 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of LITHIUM BATTERY iron manganese phosphate |
| CN109205584A (en) * | 2018-10-09 | 2019-01-15 | 湖南雅城新材料有限公司 | A kind of preparation method of high-speed rail phosphorus than ferric phosphate |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
Non-Patent Citations (2)
| Title |
|---|
| 戴志成: "《硅化合物的生产与应用》", 31 May 1994, 成都科技大学出版社, pages: 230 * |
| 文梓芸等著: "《中国混凝土工业可持续发展的战略研究》", 31 August 2013, 中国建材工业出版社, pages: 67 * |
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