CN104600297B - 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
- Publication number
- CN104600297B CN104600297B CN201510000779.1A CN201510000779A CN104600297B CN 104600297 B CN104600297 B CN 104600297B CN 201510000779 A CN201510000779 A CN 201510000779A CN 104600297 B CN104600297 B CN 104600297B
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- Prior art keywords
- phosphate precursor
- lithium phosphate
- source
- ferric lithium
- 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
-
- 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
-
- 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
-
- 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 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 synthesize the preparation technology of 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 storage
The aspects such as energy equipment, electric tool, vapour Vehicular dynamic battery, portable power source.LiFePO4 is various at present
All there is the situation of lot stability difference and exist in synthesis technique, mainly shows as precursor pulp granularity batch
Difference, the batch difference of slurry solid content, the presoma dried feed batch difference of pH value etc..
Current domestic LiFePO 4 material has defined large-scale production ability, but in actual production process
Existing between the physical and chemical indexes batch of sintetics variant, general performance is that the batch of LiFePO 4 material is stable
Property is poor.The main cause of this batches of materials less stable is synthesis presoma lot stability difference and system
During journey, equipment stablizes poor cause.
The present invention is for the lot stability difference solving to exist in above-mentioned ferric lithium phosphate precursor physical and chemical indexes
Problem, by carrying out precursor pulp batch mixing, adding a certain amount of dispersant and to presoma
Dried feed carries out the methods such as mixing, effectively solves 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 improving lot stability
Preparation method.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: improve the phosphorus of lot stability
Acid ferrum lithium presoma preparation method, comprises the following steps:
(1) the lithium source after continuously grinding, phosphorus source and source of iron mixture ground slurry are transferred to circulation
In agitator, after adding dispersant, carry out circulation stirring, the slurry in circulation stirring barrel is transferred to dry setting
Process it is dried, it is thus achieved that dry ferric lithium phosphate precursor in Bei；Lithium source, phosphorus source and source of iron mixture
Continuously grinding batch number is no less than 5 times；
(2) dried ferric lithium phosphate precursor powder is carried out powder body mixing in mixing apparatus, finally
Obtain the ferric lithium phosphate precursor that lot stability is high.
As preferably, dispersant is polyethylene glycols；The interpolation quality of dispersant is raw material gross mass
0.001%～0.5%.
As preferably, the ground slurry circulation stirring time is 1～5h.
As preferably, it is a batch that dried ferric lithium phosphate precursor powder is no less than 1000Kg by weight
Mixing, incorporation time is 1～2h.
The invention has the beneficial effects as follows:
By precursor pulp being carried out to batch mixing, adding a certain amount of dispersant and to forerunner's soma
Dry material carries out the methods such as mixing, effectively solves the physical and chemical indexes difference between ferric lithium phosphate precursor batch.
Detailed description of the invention
Embodiment 1:
Take 5 batches mixture of raw material slurry through agitation grinding, be transferred in circulation stirring barrel.By mixed
0.001% weighing PEG 20000 of raw material gross weight in compound slurry, be dissolved in going on a small quantity from
Sub-water is configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, open stirring and follow
Loop device 2h, make the slurry in circulation barrel mix, be uniformly dispersed after transfer them to drying equipment is carried out
It is dried.It is a batch by the presoma dried powder obtained in drying equipment by 1000Kg to mix at bipyramid
Equipment carries out 1h mixing, i.e. prepares the ferric lithium phosphate precursor that lot stability is high.
Embodiment 2:
Take 10 batches mixture of raw material slurry through agitation grinding, be transferred in circulation stirring barrel.Press
In mixture paste, 0.005% weighing Macrogol 4000 of raw material gross weight, is dissolved in going on a small quantity
Ionized water is configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, open stirring and
Circulating device 2h, make the slurry in circulation barrel mix, be uniformly dispersed after transfer them to drying equipment enters
Row is dried.It is that a batch is mixed at bipyramid by the presoma dried powder obtained in drying equipment by 4000Kg
Conjunction equipment carries out 2h mixing, i.e. prepares the ferric lithium phosphate precursor that lot stability is high.
Embodiment 3:
Take 10 batches mixture of raw material slurry through agitation grinding, be transferred in circulation stirring barrel.Press
In mixture paste, 0.01% weighing PEG400 of raw material gross weight, joins dispersant solution
In circulation stirring barrel, open stirring and circulating device 3h, make the slurry in circulation barrel mix, be uniformly dispersed
After transfer them to drying equipment is dried.By the presoma dried powder that obtains in drying equipment by
2000Kg is that a batch carries out 2h mixing in bipyramid mixing apparatus, i.e. prepares lot stability high
Ferric lithium phosphate precursor.
Embodiment 4:
Take 5 batches mixture of raw material slurry through agitation grinding, be transferred in circulation stirring barrel.By mixed
In compound slurry, 0.5% weighing PEG 20000 of raw material gross weight, is dissolved in a small amount of deionization
Water is configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, open stirring and circulation
Device 1h, make the slurry in circulation barrel mix, be uniformly dispersed after transfer them to drying equipment is done
Dry.It is a batch by the presoma dried powder obtained in drying equipment by 1000Kg to set in bipyramid mixing
Carry out 1h mixing in Bei, i.e. prepare the ferric lithium phosphate precursor that lot stability is high.
Embodiment 5:
Take 5 batches mixture of raw material slurry through agitation grinding, be transferred in circulation stirring barrel.By mixed
0.001% weighing PEG 20000 of raw material gross weight in compound slurry, be dissolved in going on a small quantity from
Sub-water is configured to dispersant solution.Dispersant solution is joined in circulation stirring barrel, open stirring and follow
Loop device 5h, make the slurry in circulation barrel mix, be uniformly dispersed after transfer them to drying equipment is carried out
It is dried.It is a batch by the presoma dried powder obtained in drying equipment by 1000Kg to mix at bipyramid
Equipment carries out 1h mixing, i.e. prepares the ferric lithium phosphate precursor that lot stability is high.
Invention described above embodiment, is not intended that limiting the scope of the present invention.Any
Amendment, equivalent and the improvement etc. made within the spirit and principles in the present invention, should be included in the present invention
Claims within.
Claims (4)
1. improve the ferric lithium phosphate precursor preparation method of lot stability, it is characterised in that include following
Step:
(1) the lithium source after continuously grinding, phosphorus source and source of iron mixture ground slurry are transferred to circulation
In agitator, after adding dispersant, carry out circulation stirring, the slurry in circulation stirring barrel is transferred to dry setting
Process it is dried, it is thus achieved that dry ferric lithium phosphate precursor in Bei；Described lithium source, phosphorus source and source of iron mixing
The continuously grinding batch number of thing is no less than 5 times；
(2) dried ferric lithium phosphate precursor powder is carried out powder body mixing in mixing apparatus, finally
Obtain the ferric lithium phosphate precursor that lot stability is high.
Ferric lithium phosphate precursor preparation method the most according to claim 1, it is characterised in that described point
Powder is polyethylene glycols；Interpolation quality is raw material gross mass 0.001%～the 0.5% of dispersant.
Ferric lithium phosphate precursor preparation method the most according to claim 1, it is characterised in that described in grind
The defibrination material circulation stirring time is 1～5h.
Ferric lithium phosphate precursor preparation method the most according to claim 1, it is characterised in that dried
Ferric lithium phosphate precursor powder by weight no less than 1000 this be that a batch mixes, incorporation time is
1～2h.
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| Application Number | Priority Date | Filing Date | Title |
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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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| Application Number | Priority Date | Filing Date | Title |
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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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| CN104600297A CN104600297A (en) | 2015-05-06 |
| CN104600297B true CN104600297B (en) | 2017-01-11 |
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| 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002175808A (en) * | 2000-12-08 | 2002-06-21 | Toyota Central Res & Dev Lab Inc | Lithium/transition metal compound oxide for cathode active material of lithium secondary battery, and its manufacturing method |
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- 2015-01-04 CN CN201510000779.1A patent/CN104600297B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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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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