CN103337605A - Method for preparing natural graphite cathode material of lithium ion battery by wet ball milling - Google Patents
Method for preparing natural graphite cathode material of lithium ion battery by wet ball milling Download PDFInfo
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- CN103337605A CN103337605A CN2013103058692A CN201310305869A CN103337605A CN 103337605 A CN103337605 A CN 103337605A CN 2013103058692 A CN2013103058692 A CN 2013103058692A CN 201310305869 A CN201310305869 A CN 201310305869A CN 103337605 A CN103337605 A CN 103337605A
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- 229910021382 natural graphite Inorganic materials 0.000 title claims abstract description 18
- 238000000498 ball milling Methods 0.000 title claims abstract description 11
- 239000010406 cathode material Substances 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 24
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
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- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
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- 239000007772 electrode material Substances 0.000 claims description 2
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- GBCAVSYHPPARHX-UHFFFAOYSA-M n'-cyclohexyl-n-[2-(4-methylmorpholin-4-ium-4-yl)ethyl]methanediimine;4-methylbenzenesulfonate Chemical compound CC1=CC=C(S([O-])(=O)=O)C=C1.C1CCCCC1N=C=NCC[N+]1(C)CCOCC1 GBCAVSYHPPARHX-UHFFFAOYSA-M 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical class OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
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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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Abstract
The invention discloses a method for preparing the natural graphite cathode material of a lithium ion battery by wet ball milling. The method comprises the following steps of grinding natural graphite material to obtain an intermediate product; adding the intermediate product, water, dispersing agent and a grinding ball into a stirring ball mill for stirring and ball milling at a certain ratio; after the ball-milling slurry is subjected to centrifugation or filter pressing to obtain cathode active substance containing trace moisture; drying and carrying out cyclone separation to obtain tiny particles; according to the type of the raw material, and determining whether graphitization processing needs to be carried out to finally obtain the cathode material disclosed by the invention. Compared with the prior art, the method disclosed by the invention is characterized in that a liquid phase ball milling method is adopted, the material morphology can be greatly improved, the tap density of the material is improved, the processing performance in the electrode processing process is improved, the batch stability of the product is guaranteed, the material yield is improved, the production cost is lowered, the dust pollution on the environment is greatly reduced, and the method is simple to operate and has high production efficiency.
Description
Technical field
The present invention relates to the method that a kind of wet ball grinding prepares the lithium ion battery natural graphite negative electrode material, be specifically related to a kind of lithium ion battery natural graphite negative electrode material manufacture method.
Background technology
Lithium ion battery be at present ideal in the world also be the highest chargeable chemical cell of technology, compare with other batteries, the every performance of lithium ion battery is more outstanding, have that volume is little, capacitance is big, the voltage advantages of higher, the lithium ion pond is mainly used in aspects such as mobile phone, notebook computer, electric tool, electronic product at present, to apply to fields such as electric automobile, electric bicycle, space flight and aviation, military mobile communication facility and equipment future, its demand is increasing, and is expected to present explosive growth in the electric automobile field.
Lithium ion battery negative material is based on the raw material of wood-charcoal material, mainly contain two kinds of native graphite and Delaniums, native graphite and Delanium all need as the lithium cell cathode material time it is repeatedly pulverized with spheroidization to be handled, during but existing processing method is produced, raw material availability is lower, common product yield (stock utilization) only about 45%, and the product pattern is also general, product batches is difficult to guarantee stable, and the dust environmental pollution in the production process is also relatively more serious.Therefore improve pattern and the raw-material utilance of product, reduce and pollute and production cost, develop new preparation technology, can produce very big facilitation to the lithium battery industry.
Summary of the invention
Purpose of the present invention is exactly at the problem on the prior art, and a kind of preparation method of novel, natural graphite negative electrode material that quality is higher is provided.A kind of wet ball grinding prepares the method for lithium ion battery natural graphite negative electrode material, may further comprise the steps:
One, earlier the native graphite raw material are pulverized by one-time mechanical, and the particle diameter of control powder, the electrode material intermediate product obtained;
Two, intermediate product and water, dispersant and mill ball are added agitating ball mill by a certain percentage, carry out stirring ball-milling with the rotating speed of 200～360rpm, the ball milling time is 15～300 minutes,
Three, with the slurry liquid body portion behind the ball milling in the step 2, utilize the mode of centrifugal or press filtration, remove the most aqueous solution, obtain containing the negative electrode active material of micro-moisture;
Four, the above-mentioned negative electrode active material that contains micro-moisture is isolated wherein fine particle by cyclone separator after super-dry, obtain natural graphite negative electrode material.
Native graphite raw material described in the above-mentioned steps one refer to a kind of in natural flake graphite, the natural micro crystal graphite, fixed carbon content 〉=95%.
The particle diameter of the intermediate product after process is pulverized in the above-mentioned steps one: D10 is 5～15 μ m, and D99 is 30～50 μ m.
The ratio of the intermediate product described in the above-mentioned steps two and water, dispersant and mill ball is 1:(2～3): (1.5～3): (0.01～0.05).
Mill ball described in the above-mentioned steps two is zirconium oxide balls, steel ball, agate abrading-ball, aluminium oxide abrading-ball or silicon nitride abrading-ball.
Dispersant described in the above-mentioned steps two comprises any one or more than one the mixing in stearic acid, neopelex, lauryl sodium sulfate, polyvinyl alcohol, CMC, butadiene-styrene rubber Ruzhong.
Three kinds of described modes centrifugal or press filtration of above-mentioned steps refer to adopt one or more in the equipment such as horizontal type scraper centrifuger, suspended centrifuge, vertical type automatic unloading centrifugal machine or belt filter press, plate and frame type filter-press, membrane pressure filter.
Adopting centrifugal and mode press filtration can remove in the solution 90%～97 moisture, is a kind of economic environmental protection, easily and method of operating.But the mode of removing moisture is not limited thereto.
The particle diameter of the negative material in the above-mentioned steps four after the process sorting: D10 is 5～15 μ m, and D99 is 30～50 μ m
The present invention is the preparation method of carbon cathode material compared to existing technology, and following advantage is arranged:
1) preparation method of the present invention, raw material availability is higher, and product yield can reach 70～80%, and treatment process is simple, preparation method's environmental protection, cost is lower;
2) the negative material granule-morphology that makes is good, the tap density height, and in the lithium ion battery preparation process, the materials processing performance is good, high comprehensive performance.
Description of drawings
Fig. 1 is the sem photograph of the embodiment of the invention 1.
Fig. 2 is the sem photograph of the embodiment of the invention 2.
Embodiment
The invention will be further described below in conjunction with drawings and Examples, but the present invention is not so limited.
Embodiment 1
(granular size is about 3mm with the 100Kg natural flake graphite, fixed carbon content is 97%), obtaining granularity D10 by the pulverizer fragmentation is 10.56 μ m, D99 is the random negative material intermediate of 36.71 μ m shapes 94.3Kg, add 200 kg of water and 200 kilograms of mill balls at agitating ball mill (500L), open stirring at low speed, add each 1 kilogram of dispersant detergent alkylate sulphur sodium and polyvinyl alcohol again, at last the negative material intermediate product is poured in the mixer, open high-speed stirred, rotating speed is 240rpm, stop after 90 minutes stirring, it is centrifugal to utilize the scraper-type centrifuge to carry out in slurry, will be wherein after most water removes, obtain containing the negative electrode active material of micro-moisture, and then adopt the drying device that has cyclone separator to be dried and separate in tiny powder, namely get lithium cell cathode material finished product 75.2Kg, product yield reaches 75.2%.
Embodiment 2
With the natural scale micro crystal graphite of 100 Kg (about granular size 1.5cm, fixed carbon content is 95%), obtaining granularity D10 by the pulverizer fragmentation is 7.43 μ m, D99 is the random negative material intermediates of 26.37 μ m shapes, add 200 kg of water and 180 kilograms of mill balls at agitating ball mill (500L), open stirring at low speed, add 1.5 kilograms of dispersant sodium cellulose glycolates again, at last the negative material intermediate product is added in the mixer, open high-speed stirred, rotating speed is 280rpm, stop after 120 minutes stirring, utilizing plate and frame type filter-press to carry out press filtration in slurry handles, will be wherein after most water removes, obtain containing the negative electrode active material of micro-moisture, and then adopt the drying device that has cyclone separator to be dried and separate in tiny powder, namely get lithium cell cathode material finished product 71.4Kg, product yield reaches 71.4%.
Embodiment 3
With the natural micro crystal graphite of 100 kg (about granular size 1mm), obtaining granularity D10 by the pulverizer fragmentation is 11.96 μ m, D99 is the random negative material intermediates of 38.27 μ m shapes, add 210 kg of water and 200 kilograms of mill balls at agitating ball mill (500L), open stirring at low speed, add 1 kilogram of dispersant sodium cellulose glycolate again, at last the negative material intermediate product is added in the mixer, open high-speed stirred, rotating speed is 300rpm, stop after 120 minutes stirring, utilizing plate and frame type filter-press to carry out press filtration in slurry handles, and then adopt the drying device have cyclone separator to be dried and separate in tiny powder, namely get lithium cell cathode material finished product 72.1Kg, product yield reaches 72.1%.
Comparative Examples 1
Natural scale crystallite 100kg with same weight among the embodiment 1, adopt common production technology, by repeatedly pulverizing and nodularization and sorting operation, obtain the negative material that is more or less the same among particle diameter and the embodiment 1, obtain finished product 58.1 Kg altogether, product yield reaches 58.1%.
Comparative Examples 2
Natural scale crystallite 100kg with same weight among the embodiment 2, adopt common production technology, by repeatedly pulverizing and nodularization and sorting operation, obtain the negative material that is more or less the same among particle diameter and the embodiment 2, obtain finished product 50.8 Kg altogether, product yield reaches 50.8%.
Comparative Examples 3
Natural micro crystal graphite 100kg with same weight among the embodiment 3, adopt common production technology, by repeatedly pulverizing and nodularization and sorting operation, obtain the negative material that is more or less the same among particle diameter and the embodiment 3, obtain finished product 52.3 Kg altogether, product yield reaches 52.3%.
Physical property for the prepared negative material of check the present invention adopts following detecting instrument and detection method (table one), and detection architecture sees Table two:
Table one: physical property detecting instrument and detection method
Electrical property for the prepared negative material of check the present invention, test with the half-cell method of testing, negative material with above embodiment and comparative example: acetylene black: the PVDF(Kynoar)=93: 3: the 4(weight ratio), add an amount of NMP(N-methyl pyrrolidone) the furnishing pulpous state, coat on the Copper Foil, made negative plate in 8 hours through 110 ℃ of dryings of vacuum; Be to electrode with metal lithium sheet, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1: 1: 1, microporous polypropylene membrane was barrier film, is assembled into battery.Charging/discharging voltage is 0～2.0V, and charge-discharge velocity is 0.2C, and battery performance is carried out and can test.Detection architecture sees Table two.
Table two: physical property and electrical property testing result
Analysis by embodiment 1 and Comparative Examples 1, embodiment 2 and Comparative Examples 2, embodiment 3 and Comparative Examples 3 as can be known, the negative material that process the inventive method makes, the negative material that its performance and production technology commonly used are produced is not than big difference, even the part physical index is better than the negative material that production technology commonly used is produced, and adopts its rate of finished products of the prepared negative material of the method all than high many of production technology commonly used.
More than show and described basic principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (8)
1. a wet ball grinding prepares the method for lithium ion battery natural graphite negative electrode material, may further comprise the steps:
One, earlier the native graphite raw material are pulverized by one-time mechanical, and the particle diameter of control powder, the electrode material intermediate product obtained;
Two, intermediate product and water, dispersant and mill ball are added agitating ball mill by a certain percentage, carry out stirring ball-milling with the rotating speed of 200～300rpm, the ball milling time is 15～300 minutes,
Three, with the slurry liquid body portion behind the ball milling in the step, utilize the mode of centrifugal or press filtration, remove the most aqueous solution, obtain containing the negative electrode active material of micro-moisture;
Four, the above-mentioned negative electrode active material that contains micro-moisture is isolated wherein fine particle by cyclone separator after super-dry, obtain natural graphite negative electrode material.
2. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: the native graphite raw material described in the step 5 refer to a kind of in natural flake graphite, the natural micro crystal graphite, fixed carbon content 〉=95%.
3. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: the particle diameter of the intermediate product after process is pulverized in the step 1: D10 is 5～15 μ m, and D99 is 30～50 μ m.
4. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: the ratio of the intermediate product described in the step 2 and water, dispersant and mill ball is 1:(2～3): (1.5～3): (0.01～0.05).
5. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: the mill ball described in the step 2 is zirconium oxide balls, steel ball, agate abrading-ball, aluminium oxide abrading-ball or silicon nitride abrading-ball.
6. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: dispersant described in the step 2 comprises any one or more than one the mixing in stearic acid, neopelex, lauryl sodium sulfate, polyvinyl alcohol, CMC, butadiene-styrene rubber Ruzhong.
7. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: the described mode centrifugal or press filtration of step 3 kind refers to adopt one or more in the equipment such as horizontal type scraper centrifuger, suspended centrifuge, vertical type automatic unloading centrifugal machine or belt filter press, plate and frame type filter-press, membrane pressure filter.
8. a kind of wet ball grinding according to claim 1 prepares the method for lithium ion battery natural graphite negative electrode material, it is characterized in that: the particle diameter of the negative material in the step 4 after the process sorting: D10 is 5～15 μ m, and D99 is 30～50 μ m.
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| CN110061237A (en) * | 2019-04-25 | 2019-07-26 | 广东工业大学 | A kind of amorphous carbon cell negative electrode material and its preparation method and application |
| CN111874901A (en) * | 2020-07-31 | 2020-11-03 | 广东凯金新能源科技股份有限公司 | Method for manufacturing long-circulating graphite |
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| CN104022303A (en) * | 2014-05-08 | 2014-09-03 | 景德镇陶瓷学院 | Preparation method of 8YSZ electrolyte film of anode supporting intermediate temperature single SOFC (Solid Oxide Fuel Cell) |
| CN110061237A (en) * | 2019-04-25 | 2019-07-26 | 广东工业大学 | A kind of amorphous carbon cell negative electrode material and its preparation method and application |
| CN111874901A (en) * | 2020-07-31 | 2020-11-03 | 广东凯金新能源科技股份有限公司 | Method for manufacturing long-circulating graphite |
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