CN104600297A - Lithium iron phosphate precursor preparation method capable of improving batch stability - Google Patents
Lithium iron phosphate precursor preparation method capable of improving batch stability Download PDFInfo
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- CN104600297A CN104600297A CN201510000779.1A CN201510000779A CN104600297A CN 104600297 A CN104600297 A CN 104600297A CN 201510000779 A CN201510000779 A CN 201510000779A CN 104600297 A CN104600297 A CN 104600297A
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- phosphate precursor
- lithium phosphate
- ferric lithium
- source
- iron phosphate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a lithium iron phosphate precursor preparation method capable of improving the batch stability. The lithium iron phosphate precursor preparation method comprises the following steps: (1) transferring the ground slurry of a mixture of a lithium source, a phosphorus source and an iron source after continuous grinding into a circular mixing barrel, adding a dispersing agent, circularly mixing, transferring the slurry in the circular mixing barrel into drying equipment and performing drying treatment to obtain a dried lithium iron phosphate precursor; and (2) performing powder mixing of the dried lithium iron phosphate precursor powder in mixing equipment to finally obtain a lithium iron phosphate precursor with high batch stability. The process disclosed by the invention is simple, has high operational feasibility, can be used for remarkably improving the batch stability of the lithium iron phosphate precursor and is suitable for industrial production.
Description
Technical field
The present invention relates to the preparation technology of synthesis lithium cell anode material of lithium iron phosphate presoma, refer more particularly to a kind of ferric lithium phosphate precursor preparation method improving lot stability.
Background technology
LiFePO 4 material is acknowledged as safest anode material for lithium-ion batteries, is widely used in the aspects such as energy storage device, electric tool, vapour Vehicular dynamic battery, portable power source.All there is the situation existence of lot stability difference in the various synthesis techniques of current LiFePO4, main manifestations is the batch difference of precursor pulp granularity, the batch difference of slurry solid content, the batch difference of presoma dried feed pH value etc.
Current domestic LiFePO 4 material has defined large-scale production ability, but variant between the physical and chemical indexes batch that there is sintetics in the production process of reality, and general performance is that the lot stability of LiFePO 4 material is poor.The main cause of this batches of materials less stable is synthesized equipment in presoma lot stability difference and processing procedure process and is stablized poor causing.
The problem of the lot stability difference of physical and chemical indexes is there is in above-mentioned ferric lithium phosphate precursor in the present invention for solving, by carrying out precursor pulp a batch mixing, adding a certain amount of dispersant and carry out the method such as mixing to presoma dried feed, effectively solve the physical and chemical indexes difference between ferric lithium phosphate precursor batch.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of ferric lithium phosphate precursor preparation method improving lot stability.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the ferric lithium phosphate precursor preparation method improving lot stability, comprises the following steps:
(1) the lithium source after continuously grinding, phosphorus source and source of iron mixture ground slurry are transferred in circulation stirring barrel, circulation stirring is carried out after adding dispersant, slurry in circulation stirring barrel is transferred in drying equipment and carries out drying process, obtain dry ferric lithium phosphate precursor;
(2) dried ferric lithium phosphate precursor powder is carried out powder mixing in mixing apparatus, the ferric lithium phosphate precursor that final acquisition lot stability is high.
As preferably, a continuously grinding batch number for lithium source, phosphorus source and source of iron mixture is no less than 5 times.
As preferably, dispersant is polyethylene glycols; The interpolation quality of dispersant is 0.001% ~ 0.5% of raw material gross mass.
As preferably, the ground slurry circulation stirring time is 1 ~ 5h.
As preferably, dried ferric lithium phosphate precursor powder is no less than 1000Kg by weight and is one batch and mixes, and incorporation time is 1 ~ 2h.
The invention has the beneficial effects as follows:
By carrying out precursor pulp a batch mixing, adding a certain amount of dispersant and carry out the method such as mixing to presoma dried feed, effectively solve the physical and chemical indexes difference between ferric lithium phosphate precursor batch.
Embodiment
Embodiment 1:
Get 5 batches through the mixture of raw material slurry of agitation grinding, be transferred in circulation stirring barrel.Weigh PEG 20000 by 0.001% of raw material total weight in mixture paste, be dissolved in a small amount of deionized water and be configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, opens and stir and circulating device 2h, the slurry in circulation barrel is mixed, be uniformly dispersed after transfer them in drying equipment and carry out drying.The presoma dried powder obtained in drying equipment is one batch by 1000Kg in bipyramid mixing apparatus, carries out 1h mixing, namely prepare the ferric lithium phosphate precursor that lot stability is high.
Embodiment 2:
Get 10 batches through the mixture of raw material slurry of agitation grinding, be transferred in circulation stirring barrel.Weigh Macrogol 4000 by 0.005% of raw material total weight in mixture paste, be dissolved in a small amount of deionized water and be configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, opens and stir and circulating device 2h, the slurry in circulation barrel is mixed, be uniformly dispersed after transfer them in drying equipment and carry out drying.The presoma dried powder obtained in drying equipment is one batch by 4000Kg in bipyramid mixing apparatus, carries out 2h mixing, namely prepare the ferric lithium phosphate precursor that lot stability is high.
Embodiment 3:
Get 10 batches through the mixture of raw material slurry of agitation grinding, be transferred in circulation stirring barrel.PEG400 is weighed by 0.01% of raw material total weight in mixture paste, dispersant solution is joined in circulation stirring barrel, open and stir and circulating device 3h, the slurry in circulation barrel is mixed, be uniformly dispersed after transfer them in drying equipment and carry out drying.The presoma dried powder obtained in drying equipment is one batch by 2000Kg in bipyramid mixing apparatus, carries out 2h mixing, namely prepare the ferric lithium phosphate precursor that lot stability is high.
Embodiment 4:
Get 5 batches through the mixture of raw material slurry of agitation grinding, be transferred in circulation stirring barrel.Weigh PEG 20000 by 0.5% of raw material total weight in mixture paste, be dissolved in a small amount of deionized water and be configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, opens and stir and circulating device 1h, the slurry in circulation barrel is mixed, be uniformly dispersed after transfer them in drying equipment and carry out drying.The presoma dried powder obtained in drying equipment is one batch by 1000Kg in bipyramid mixing apparatus, carries out 1h mixing, namely prepare the ferric lithium phosphate precursor that lot stability is high.
Embodiment 5:
Get 5 batches through the mixture of raw material slurry of agitation grinding, be transferred in circulation stirring barrel.Weigh PEG 20000 by 0.001% of raw material total weight in mixture paste, be dissolved in a small amount of deionized water and be configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, opens and stir and circulating device 5h, the slurry in circulation barrel is mixed, be uniformly dispersed after transfer them in drying equipment and carry out drying.The presoma dried powder obtained in drying equipment is one batch by 1000Kg in bipyramid mixing apparatus, carries out 1h mixing, namely prepare the ferric lithium phosphate precursor that lot stability is high.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any amendment done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within claims of the present invention.
Claims (5)
1. improve the ferric lithium phosphate precursor preparation method of lot stability, it is characterized in that, comprise the following steps:
(1) the lithium source after continuously grinding, phosphorus source and source of iron mixture ground slurry are transferred in circulation stirring barrel, circulation stirring is carried out after adding dispersant, slurry in circulation stirring barrel is transferred in drying equipment and carries out drying process, obtain dry ferric lithium phosphate precursor;
(2) dried ferric lithium phosphate precursor powder is carried out powder mixing in mixing apparatus, the ferric lithium phosphate precursor that final acquisition lot stability is high.
2. ferric lithium phosphate precursor preparation method according to claim 1, is characterized in that, a continuously grinding batch number for described lithium source, phosphorus source and source of iron mixture is no less than 5 times.
3. ferric lithium phosphate precursor preparation method according to claim 1, it is characterized in that, described dispersant is polyethylene glycols; The interpolation quality of dispersant is 0.001% ~ 0.5% of raw material gross mass.
4. ferric lithium phosphate precursor preparation method according to claim 1, it is characterized in that, the described ground slurry circulation stirring time is 1 ~ 5h.
5. ferric lithium phosphate precursor preparation method according to claim 1, is characterized in that, dried ferric lithium phosphate precursor powder is no less than 1000Kg by weight and is one batch and mixes, and incorporation time is 1 ~ 2h.
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| CN201510000779.1A CN104600297B (en) | 2015-01-04 | 2015-01-04 | Lithium iron phosphate precursor preparation method capable of improving batch stability |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111969178A (en) * | 2019-05-20 | 2020-11-20 | 贵州安达科技能源股份有限公司 | Lithium iron phosphate battery positive electrode slurry and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020110518A1 (en) * | 2000-12-08 | 2002-08-15 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Lithium transition metal composite oxide for use as positive active material of lithium secondary battery and method for producing the same |
| CN101913588A (en) * | 2010-07-08 | 2010-12-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing lithium iron phosphate nano material |
| CN102208625A (en) * | 2011-05-04 | 2011-10-05 | 合肥国轩高科动力能源有限公司 | Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery |
| JP2012204150A (en) * | 2011-03-25 | 2012-10-22 | Sumitomo Osaka Cement Co Ltd | Method of producing electrode active material and electrode active material, electrode, and battery |
| CN103258995A (en) * | 2013-06-06 | 2013-08-21 | 郑州瑞普生物工程有限公司 | Preparation method of lithium iron phosphate material |
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- 2015-01-04 CN CN201510000779.1A patent/CN104600297B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020110518A1 (en) * | 2000-12-08 | 2002-08-15 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Lithium transition metal composite oxide for use as positive active material of lithium secondary battery and method for producing the same |
| CN101913588A (en) * | 2010-07-08 | 2010-12-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing lithium iron phosphate nano material |
| JP2012204150A (en) * | 2011-03-25 | 2012-10-22 | Sumitomo Osaka Cement Co Ltd | Method of producing electrode active material and electrode active material, electrode, and battery |
| CN102208625A (en) * | 2011-05-04 | 2011-10-05 | 合肥国轩高科动力能源有限公司 | Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery |
| CN103258995A (en) * | 2013-06-06 | 2013-08-21 | 郑州瑞普生物工程有限公司 | Preparation method of lithium iron phosphate material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111969178A (en) * | 2019-05-20 | 2020-11-20 | 贵州安达科技能源股份有限公司 | Lithium iron phosphate battery positive electrode slurry and preparation method thereof |
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Address after: 230000 Yaohai Industrial Zone, Hefei New District, Anhui, No. D weft Road, No. 7 Applicant after: Hefei Guoxuan High-Tech Power Energy Co., Ltd. Address before: 230000 Yaohai Industrial Zone, Hefei New District, Anhui, No. D weft Road, No. 7 Applicant before: Hefei Guoxuan High-Tech Power Energy Co., Ltd. |
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Inventor after: Liu Dajun Inventor after: Li Chen Inventor after: Fang Jianhua Inventor before: Liu Dajun |
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