CN101552331A - Preparation technique of lithium-ion battery anode material lithium iron phosphate - Google Patents
Preparation technique of lithium-ion battery anode material lithium iron phosphate Download PDFInfo
- Publication number
- CN101552331A CN101552331A CNA200910026550XA CN200910026550A CN101552331A CN 101552331 A CN101552331 A CN 101552331A CN A200910026550X A CNA200910026550X A CN A200910026550XA CN 200910026550 A CN200910026550 A CN 200910026550A CN 101552331 A CN101552331 A CN 101552331A
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- Prior art keywords
- lithium
- lifepo
- phosphate
- preparation
- iron
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation technique of the lithium-ion battery anode material lithium iron phosphate, which belongs to the preparation method of the battery anode material. The lithium iron phosphate is prepared by taking iron powder Fe, lithium hydroxide LiOH or lithium carbonate LI2CO3 and phosphoric acid (H3PO4) as raw materials according to the following processing steps of preparation of acid phosphate ferrous, preparation of iron lithium phosphate, and sintering. The preparation technique has the advantages of simple production process, easy operation, safety and reliability, pure product, stable quality, low costs, and no pollution to the environment.
Description
Technical field
The present invention relates to the manufacture method of battery anode material, specifically is a kind of preparation technology of lithium-ion battery anode material lithium iron phosphate.
Background technology
Along with the minimizing day by day of fossil energy and the pay attention to day by day of human environmental pollution, seeking novel clean energy resource has become the task of top priority, so the utilization of electric energy is also more and more paid attention to by people.The battery that uses on mobile object at present generally is a lead acid accumulator.But traditional lead acid accumulator has the shortcoming that can't overcome, the one, and seriously polluted, wherein plumbous and acid all is the severe contamination source.The 2nd, from great, specific capacity is little.Three are to use the life-span short, dash, discharge time is few.Lithium ion battery development in recent years is very fast, and the research of ferric phosphate lithium cell at present is still in the starting stage, and existing Tianjin, Suzhou, the many families in Hunan produce.But in LiFePO 4 material production, application, there is following problem, the one, traditional production method is to the technological requirement height.The 2nd, unstable product quality, the technical indicator of each batch can not be consistent.The 3rd, cost is higher; All these problems all need to be resolved hurrily.
Summary of the invention
For addressing the above problem, the invention provides a kind of preparation technology of lithium-ion battery anode material lithium iron phosphate, for the production of China's ferrous phosphate lithium battery material provides a kind of new way.
The present invention realizes with following technical scheme: a kind of preparation technology of lithium-ion battery anode material lithium iron phosphate is characterized in that, with iron powder Fe, lithium hydroxide LiOH or lithium carbonate Li
2CO
3And phosphoric acid (H
3PO
4) be raw material, prepare by following processing step:
(1), preparation acid ferrous phosphate FeHPO
4
Iron powder Fe and phosphoric acid is mixed in 1: 1 ratio of molal quantity, stir, when being warmed up to 85-90 ℃, iron and phosphoric acid vigorous reaction; After the complete reaction hydrogen is discharged, obtain pale precipitation and be acid ferrous phosphate FeHPO
4
(2) produce LiFePO 4 LiFePO
4
With waiting lithium hydroxide LiOH solution of molal quantity, join in the above-mentioned white precipitate, fully mixed or with acid ferrous phosphate FeHPO
4Precipitation and lithium carbonate Li
2CO
3Fully mixed in 2: 1 ratio of molal quantity, promptly get LiFePO 4 LiFePO
4Presoma;
(3) presoma with LiFePO 4 places Shao Jie Kiln; add carbon encapsulated material, be warmed up to 150 ℃ water is evaporated fully, under the non-oxidized gas protection; be warmed up to again 700 ℃-800 ℃ sintering 16-20 hour, promptly obtain the LiFePO 4 LiFePO of olivine structural
4Crystal.
Principle and reaction equation are as follows:
1、Fe+H
3PO
4＝FeHPO
4++H
2↑
2, FeHPO
4+ LiOHH
2O=LiFePO
4+ 2H
2O or
2FeHPO
4+Li
2CO
3＝2LiFePO
4+CO
2↑+H
2O
Overall reaction can be expressed as (only will need in order to calculate):
(1)Fe+H
3PO
4+LiOH·H
2O＝LiFePO
4+2H
2O
++H
2↑
(2)2Fe+2H
3PO
4+LI
2CO
3＝2LiFePO
4+CO
2↑+H
2O+2H
2↑
Conventional method is compared, and the invention has the beneficial effects as follows:
1, because reaction is all carried out in solution, and each reaction all is a complete reaction, each reaction generates water, gas or precipitation respectively.Be convenient to the separation of product, produce simply, be convenient to operation, safe and reliable, product is pure, steady quality.
2, conventional method need be under the protection environment, 800-900 ℃ of sintering 24 hours, reaction condition is required comparatively strict, complex process.Each reaction of this method all is spontaneous carrying out in container, and reaction condition is lower, has avoided the difficulty of control reaction condition.
3, owing to there is not ammonia (NH
3), carbon monoxide (CO) gas generates, therefore to environment without any pollution.
4, owing to the raw material that use generally are easy to get, cheap.Each utilization rate of active components height.
5, produced in conventional processes LiFePO 4 (LiFePO
4) maximum difficulty is, the quality instability of product, every batch of technical indicator is difficult to consistent.LiFePO 4 (the LiFePO that this method is produced
4) the technical indicator consistency is higher, steady quality.
6, this method is saved the energy.
Embodiment
Further specify the inventive method and effect below in conjunction with embodiment.
Embodiment
Raw material: iron powder Fe, lithium hydroxide LiOH or lithium carbonate Li
2CO
3With phosphoric acid H
3PO
4
Production equipment: common reactor, revolution sintering oven.
Production technology: earlier handle waits the iron powder of molal quantity and 50% phosphoric acid to add in the reactor, is warmed up to 85-90 ℃, and stirring makes it complete reaction, and then in still the lithium hydroxide LiOH solution of molal quantity such as adding, or add the lithium carbonate Li of 1/2 molal quantity
2CO
3Solution stirs, and makes it complete reaction.Promptly make LiFePO 4 LiFePO
4The presoma suspension-turbid liquid.The lithium iron phosphate precursor suspension-turbid liquid is transferred among the Shao Jie Kiln; add carbon encapsulated material then, be warmed up to 150 ℃ water is evaporated fully, under the non-oxidized gas protection; be warmed up to 700 ℃ of sintering 20 hours again, can obtain the LiFePO 4 LiFePO of needed olivine structural
4Crystal.
Claims (1)
1, a kind of preparation technology of lithium-ion battery anode material lithium iron phosphate is characterized in that, with iron powder Fe, lithium hydroxide LiOH or lithium carbonate Li
2CO
3Calculating H3PO4 with phosphorus is raw material, prepares by following processing step:
(1), preparation acid ferrous phosphate FeHPO
4
Iron powder Fe and phosphoric acid is mixed in 1: 1 ratio of molal quantity, stir, when being warmed up to 85-90 ℃, iron and phosphoric acid vigorous reaction; After the complete reaction hydrogen is discharged, obtain pale precipitation and be acid ferrous phosphate FeHPO
4
(2) produce LiFePO 4 LiFePO
4
With waiting lithium hydroxide LiOH solution of molal quantity, join in the above-mentioned white precipitate, fully mixed or with acid ferrous phosphate FeHPO
4Precipitation and lithium carbonate LI
2CO
3Fully mixed in 2: 1 ratio of molal quantity, promptly get LiFePO 4 LiFePO
4Presoma;
(3) presoma with LiFePO 4 places sintering oven; add carbon encapsulated material, be warmed up to 150 ℃ water is evaporated fully, under the non-oxidized gas protection; be warmed up to again 700 ℃-800 ℃ sintering 16-20 hour, promptly obtain the LiFePO 4 LiFePO of olivine structural
4Crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910026550XA CN101552331A (en) | 2009-05-01 | 2009-05-01 | Preparation technique of lithium-ion battery anode material lithium iron phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910026550XA CN101552331A (en) | 2009-05-01 | 2009-05-01 | Preparation technique of lithium-ion battery anode material lithium iron phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101552331A true CN101552331A (en) | 2009-10-07 |
Family
ID=41156406
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200910026550XA Pending CN101552331A (en) | 2009-05-01 | 2009-05-01 | Preparation technique of lithium-ion battery anode material lithium iron phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101552331A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012045211A1 (en) * | 2010-10-09 | 2012-04-12 | 河南环宇集团有限公司 | Production method of lithium-ferrous phosphate double-salt positive-electrode material and positive-electrode material obtained |
| CN102447099A (en) * | 2010-10-09 | 2012-05-09 | 河南环宇集团有限公司 | New method for preparing lithium ferrous phosphate double-salt anode material by using iron chippings, phosphoric acid and lithium hydroxide |
| CN102800864A (en) * | 2012-08-23 | 2012-11-28 | 雅安世佳微尔科技有限公司 | Iron-lithium nanocomposite material synthesis technology |
| CN103035909A (en) * | 2011-09-29 | 2013-04-10 | 比亚迪股份有限公司 | Preparation methods of lithium iron phosphate precursor, lithium iron phosphate material and lithium iron phosphate/carbon composite material |
| CN103107333A (en) * | 2013-01-31 | 2013-05-15 | 贵州省开阳安达磷化工有限公司 | Lithium iron phosphate and preparation method thereof |
| CN114188508A (en) * | 2021-10-28 | 2022-03-15 | 厦门理工学院 | Lithium iron phosphate cathode material, preparation method and application |
-
2009
- 2009-05-01 CN CNA200910026550XA patent/CN101552331A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012045211A1 (en) * | 2010-10-09 | 2012-04-12 | 河南环宇集团有限公司 | Production method of lithium-ferrous phosphate double-salt positive-electrode material and positive-electrode material obtained |
| CN102447099A (en) * | 2010-10-09 | 2012-05-09 | 河南环宇集团有限公司 | New method for preparing lithium ferrous phosphate double-salt anode material by using iron chippings, phosphoric acid and lithium hydroxide |
| CN102447099B (en) * | 2010-10-09 | 2014-01-29 | 河南环宇集团有限公司 | New method for preparing lithium ferrous phosphate double-salt anode material by using iron chippings, phosphoric acid and lithium hydroxide |
| CN103035909A (en) * | 2011-09-29 | 2013-04-10 | 比亚迪股份有限公司 | Preparation methods of lithium iron phosphate precursor, lithium iron phosphate material and lithium iron phosphate/carbon composite material |
| CN103035909B (en) * | 2011-09-29 | 2015-07-22 | 比亚迪股份有限公司 | Preparation methods of lithium iron phosphate precursor, lithium iron phosphate material and lithium iron phosphate/carbon composite material |
| CN102800864A (en) * | 2012-08-23 | 2012-11-28 | 雅安世佳微尔科技有限公司 | Iron-lithium nanocomposite material synthesis technology |
| CN103107333A (en) * | 2013-01-31 | 2013-05-15 | 贵州省开阳安达磷化工有限公司 | Lithium iron phosphate and preparation method thereof |
| CN103107333B (en) * | 2013-01-31 | 2015-08-19 | 贵州安达科技能源股份有限公司 | A kind of preparation method of LiFePO4 and LiFePO4 |
| CN114188508A (en) * | 2021-10-28 | 2022-03-15 | 厦门理工学院 | Lithium iron phosphate cathode material, preparation method and application |
| CN114188508B (en) * | 2021-10-28 | 2023-02-14 | 厦门理工学院 | Lithium iron phosphate cathode material, preparation method and application |
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Open date: 20091007 |