CN106898772A - A kind of preparation method of high magnification high-pressure solid graphite cathode material - Google Patents

A kind of preparation method of high magnification high-pressure solid graphite cathode material Download PDF

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Publication number
CN106898772A
CN106898772A CN201710159125.2A CN201710159125A CN106898772A CN 106898772 A CN106898772 A CN 106898772A CN 201710159125 A CN201710159125 A CN 201710159125A CN 106898772 A CN106898772 A CN 106898772A
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China
Prior art keywords
graphite
graphite cathode
preparation
particle
carried out
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CN201710159125.2A
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Chinese (zh)
Inventor
陈锐
刘自乾
刘新耀
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Yaan Qianrun Lithium Battery Material Co Ltd
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Yaan Qianrun Lithium Battery Material Co Ltd
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Priority to CN201710159125.2A priority Critical patent/CN106898772A/en
Publication of CN106898772A publication Critical patent/CN106898772A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The present invention proposes a kind of preparation method of high magnification high-pressure solid graphite cathode material, it is raw material that this product uses high-quality Delanium, mix and load graphite crucible by coarse crushing, attritioning, classification fineness 10 13um, graphitization sintering is carried out at 3000 DEG C, obtain graphite cathode particle;Graphite cathode particle after sintering is carried out into coarse crushing sieving, you can obtain this product.Product processing technique of the invention is simple, and low cost, quality is easily controllable, and cost performance is high, it is adaptable to the preferable negative material that electrokinetic cell is used.The preparation method of high power capacity high-rate lithium battery negative material overcomes in the prior art the need for production graphite cathode material at ambient pressure that equipment is more, yield poorly, the shortcoming that energy consumption is big, with preferable prospects for commercial application.

Description

A kind of preparation method of high magnification high-pressure solid graphite cathode material
Technical field
The present invention relates to lithium ion battery manufacture field, a kind of system of high magnification high-pressure solid graphite cathode material is particularly related to Preparation Method.
Background technology
To be sold after broken artificial graphite nodularization shaping using nodularization system more than common artificial plumbago negative pole material.It is existing Automatic spheroidization system be primarily present problems with:Equipment is designed, the air-flow for using mainly for natural flake graphite nodularization Vortex Ultramicro-powder acc power is the same, when to artificial plumbago negative pole material nodularization shaping, the air-flow vortex Ultramicro-powder of equal-wattage The particle that chance causes nodularization good is crushed again, causes sphericity to be destroyed, yield reduction;In addition, in the nodularization later stage, existing portion Meticulous material is divided to be recovered, the material for participating in nodularization has been greatly decreased, and now still enters using high-power air-flow vortex Ultramicro-powder machine Row nodularization, can increase equipment energy consumption.
Still suffer from that specific surface area is big, gram specific capacity is low, compacted density is low by the artificial plumbago negative pole material of nodularization shaping The problems such as.It is the more preferable artificial plumbago negative pole material of processability, also needs to be modified it treatment.Patent CN101924209A By needle coke by modifications such as catalyzed graphitization, coatings, the artificial plumbago negative pole material of better performances is obtained;But it is prepared Raw material is complicated needle coke, price, and preparation technology.Patent CN1691374A is coated after covering material is dissolved with solvent In Delanium surface, obtained artificial plumbago negative pole material specific surface is low, and initial coulomb efficiency is high;But introduced in preparation process A large amount of solvents, complex process, effect on environment is big.Patent CN1649192A hard pitch is crushed to less than 2 μm after with it is natural Graphite is mixed, and obtained natural graphite negative electrode material initial coulomb efficiency reaches 92%;But it only will in preparation process Uniform mixing is asked, causes covered effect slightly worse compared to liquid phase coating effect, and require for pitch to be crushed to 2 μm in preparation process Hereinafter, existing micro mist equipment is extremely difficult reaches technological requirement.Therefore, how using more reasonably artificial plumbago negative pole material solid phase bag Coating technique, is one problem demanding prompt solution of current industry.
The content of the invention
The present invention proposes a kind of preparation method of high magnification high-pressure solid graphite cathode material, the technique of the method converted products Simply, low cost, quality is easily controllable.
The technical proposal of the invention is realized in this way:A kind of preparation method of high magnification high-pressure solid graphite cathode material, Comprise the following steps:
It is raw material that step a. chooses high-quality Delanium of the granularity less than 5mm, by its nodularization;
Graphite coarse crushing after above-mentioned nodularization is the graphite particle of 20-30um by step b.;
Above-mentioned graphite particle is carried out fine crushing by step c. with airslide disintegrating mill, is ground into the micro mist of 15-20 μm of particle diameter;
Then step d. mixes above-mentioned micro-powder graded fineness 10-13um with binding agent in homogenizer;
Powder after stirring is loaded graphite crucible by step e., and graphitization sintering is carried out at 2800 DEG C -3500 DEG C, obtains stone Black negative pole particle;
Graphite cathode particle after sintering is carried out coarse crushing sieving by step f., you can obtain this product.
Preferably, the graphite crucible temperature control of the graphitization sintering of the step e is advisable at 3000 DEG C.
Preferably, adding pitch micro mist during the attritioning of the step c in graphite, then mix.
Compared with prior art, the advantage of the invention is that:The product processing technique is simple, low cost, and quality is easy to control System, cost performance is high, it is adaptable to the preferable negative material that electrokinetic cell is used.The preparation of high power capacity high-rate lithium battery negative material Method overcomes in the prior art the need for production graphite cathode material at ambient pressure that equipment is more, yield poorly, the shortcoming that energy consumption is big, With preferable prospects for commercial application.
Specific embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation Example is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model of present invention protection Enclose.
Embodiment 1:
A kind of preparation method of high magnification high-pressure solid graphite cathode material, comprises the following steps:
The high-quality Delanium that step a. chooses granularity 5mm is raw material, by its nodularization;
Graphite coarse crushing after above-mentioned nodularization is the graphite particle of 20um by step b.;
Above-mentioned graphite particle is carried out fine crushing by step c. with airslide disintegrating mill, is ground into the micro mist of 15 μm of particle diameter, essence Pitch micro mist is added during broken in graphite, is then mixed;
Then step d. mixes above-mentioned micro-powder graded fineness 10um with binding agent in homogenizer;
Powder after stirring is loaded graphite crucible by step e., and graphitization sintering is carried out at 2800 DEG C, obtains graphite cathode Particle;
Graphite cathode particle after sintering is carried out coarse crushing sieving by step f., you can obtain this product.
Embodiment 2:
A kind of preparation method of high magnification high-pressure solid graphite cathode material, comprises the following steps:
The high-quality Delanium that step a. chooses granularity 3mm is raw material, by its nodularization;
Graphite coarse crushing after above-mentioned nodularization is the graphite particle of 25um by step b.;
Above-mentioned graphite particle is carried out fine crushing by step c. with airslide disintegrating mill, is ground into the micro mist of 18 μm of particle diameter, essence Pitch micro mist is added during broken in graphite, is then mixed;
Then step d. mixes above-mentioned micro-powder graded fineness 12um with binding agent in homogenizer;
Powder after stirring is loaded graphite crucible by step e., and graphitization sintering is carried out at 3000 DEG C, obtains graphite cathode Particle;
Graphite cathode particle after sintering is carried out coarse crushing sieving by step f., you can obtain this product.
Embodiment 3:
It is raw material that step a. chooses high-quality Delanium of the granularity less than 2mm, by its nodularization;
Graphite coarse crushing after above-mentioned nodularization is the graphite particle of 30um by step b.;
Above-mentioned graphite particle is carried out fine crushing by step c. with airslide disintegrating mill, is ground into the micro mist of 20 μm of particle diameter;
Then step d. mixes above-mentioned micro-powder graded fineness 13um with binding agent in homogenizer;
Powder after stirring is loaded graphite crucible by step e., and graphitization sintering is carried out at 3500 DEG C, obtains graphite cathode Particle;
Graphite cathode particle after sintering is carried out coarse crushing sieving by step f., you can obtain this product.
Compared with prior art, the advantage of the invention is that:The product processing technique is simple, low cost, and quality is easy to control System, cost performance is high, it is adaptable to the preferable negative material that electrokinetic cell is used.The preparation of high power capacity high-rate lithium battery negative material Method overcomes in the prior art the need for production graphite cathode material at ambient pressure that equipment is more, yield poorly, the shortcoming that energy consumption is big, With preferable prospects for commercial application.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.

Claims (3)

1. a kind of preparation method of high magnification high-pressure solid graphite cathode material, it is characterised in that:Comprise the following steps,
It is raw material that step a. chooses high-quality Delanium of the granularity less than 5mm, by its nodularization;
Graphite coarse crushing after above-mentioned nodularization is the graphite particle of 20-30um by step b.;
Above-mentioned graphite particle is carried out fine crushing by step c. with airslide disintegrating mill, is ground into the micro mist of 15-20 μm of particle diameter;
Then step d. mixes above-mentioned micro-powder graded fineness 10-13um with binding agent in homogenizer;
Powder after stirring is loaded graphite crucible by step e., and graphitization sintering is carried out at 2800 DEG C -3500 DEG C, is obtained graphite and is born Pole particle;
Graphite cathode particle after sintering is carried out coarse crushing sieving by step f., you can obtain this product.
2. the preparation method of a kind of high magnification high-pressure solid graphite cathode material according to claim 1, it is characterised in that:Institute The graphite crucible temperature control for stating the graphitization sintering of step e is advisable at 3000 DEG C.
3. a kind of preparation method of high magnification high-pressure solid graphite cathode material according to claim 1 and 2, its feature exists In:Pitch micro mist is added during the attritioning of the step c in graphite, is then mixed.
CN201710159125.2A 2017-03-17 2017-03-17 A kind of preparation method of high magnification high-pressure solid graphite cathode material Pending CN106898772A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108706582A (en) * 2018-06-27 2018-10-26 河南易成新能源股份有限公司 The preparation method of artificial plumbago negative pole material
CN112670504A (en) * 2020-12-25 2021-04-16 宁波杉杉新材料科技有限公司 Modified resistance material, graphite negative electrode material containing modified resistance material, and preparation method and application of graphite negative electrode material
CN113363466A (en) * 2021-06-16 2021-09-07 广东凯金新能源科技股份有限公司 Low-cost graphite negative electrode material based on crucible crushed aggregates and preparation method thereof
CN113800912A (en) * 2021-11-04 2021-12-17 大连宏光锂业股份有限公司 High compaction rate type lithium ion battery cathode material and preparation method thereof
CN113823792A (en) * 2021-01-05 2021-12-21 广东东岛新能源股份有限公司 Preparation method for producing negative electrode material for lithium ion battery by using blocky graphite

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1923681A (en) * 2006-08-14 2007-03-07 长沙市海容电子材料有限公司 Graphite material with shell-core structure and preparation method thereof
CN101087021A (en) * 2007-07-18 2007-12-12 深圳市贝特瑞新能源材料股份有限公司 Man-made graphite cathode material for lithium ion battery and its making method
CN101582503A (en) * 2008-05-14 2009-11-18 天津市铁诚电池材料有限公司 Negative electrode material of lithium ion battery with graphite covered by asphalt and preparation method thereof
CN103346294A (en) * 2013-06-24 2013-10-09 方大炭素新材料科技股份有限公司 Preparation method of artificial graphite cathode material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1923681A (en) * 2006-08-14 2007-03-07 长沙市海容电子材料有限公司 Graphite material with shell-core structure and preparation method thereof
CN101087021A (en) * 2007-07-18 2007-12-12 深圳市贝特瑞新能源材料股份有限公司 Man-made graphite cathode material for lithium ion battery and its making method
CN101582503A (en) * 2008-05-14 2009-11-18 天津市铁诚电池材料有限公司 Negative electrode material of lithium ion battery with graphite covered by asphalt and preparation method thereof
CN103346294A (en) * 2013-06-24 2013-10-09 方大炭素新材料科技股份有限公司 Preparation method of artificial graphite cathode material

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108706582A (en) * 2018-06-27 2018-10-26 河南易成新能源股份有限公司 The preparation method of artificial plumbago negative pole material
CN112670504A (en) * 2020-12-25 2021-04-16 宁波杉杉新材料科技有限公司 Modified resistance material, graphite negative electrode material containing modified resistance material, and preparation method and application of graphite negative electrode material
CN113823792A (en) * 2021-01-05 2021-12-21 广东东岛新能源股份有限公司 Preparation method for producing negative electrode material for lithium ion battery by using blocky graphite
CN113363466A (en) * 2021-06-16 2021-09-07 广东凯金新能源科技股份有限公司 Low-cost graphite negative electrode material based on crucible crushed aggregates and preparation method thereof
CN113800912A (en) * 2021-11-04 2021-12-17 大连宏光锂业股份有限公司 High compaction rate type lithium ion battery cathode material and preparation method thereof

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Application publication date: 20170627