CN105347333A - Preparation method of low-cost negative electrode material of power lithium ion battery - Google Patents

Preparation method of low-cost negative electrode material of power lithium ion battery Download PDF

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Publication number
CN105347333A
CN105347333A CN201510851428.1A CN201510851428A CN105347333A CN 105347333 A CN105347333 A CN 105347333A CN 201510851428 A CN201510851428 A CN 201510851428A CN 105347333 A CN105347333 A CN 105347333A
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preparation
lithium ion
ion battery
low cost
battery cathode
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CN201510851428.1A
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晏荦
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Guangdong Kaijin New Energy Technology Co Ltd
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Guangdong Kaijin New Energy Technology Co Ltd
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Priority to CN201510851428.1A priority Critical patent/CN105347333A/en
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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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/11—Powder tap density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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 provides a preparation method of a low-cost negative electrode material of a power lithium ion battery. The preparation method comprises the steps that graphitization treatment is conducted on a raw material, crushing processing and shaping are conducted, and a finished product is obtained. The graphitization treatment of the raw material is conducted in a graphitization furnace which is of a vertical enclosed structure, and the graphitization furnace of the vertical enclosed structure comprises a feeding opening, a graphitization high-temperature zone, a high temperature buffer zone and an automatic discharging system which are arranged from bottom to top. By means of the graphitization furnace of the vertical enclosed structure, heat energy utilization is greatly improved, and the energy consumption is reduced by 70 percent or above; flue gas is guided and treated in a concentrated mode, and the environment protection is increased by 95 percent or above; circulating water is adopted for cooling, and the water resource is saved by 80 percent or above; the temperatures in the furnace are consistent so that the quality of the product can be greatly improved.

Description

A kind of preparation method of lithium ion battery cathode material of low cost
Technical field
The invention belongs to lithium cell cathode material preparation field, particularly a kind of preparation method of lithium ion battery cathode material of low cost.
Background technology
Current electromobile particularly pure electric automobile receives the concern of people especially, wherein lithium ion battery is optimal electrical source of power, it is one of key part affecting vehicle performance, cost and user's experience, also be the component that in integral vehicle cost, accounting is maximum, its cost accounts for the half of integral vehicle cost, and the cost of the large critical material of the positive electrode material in lithium ion battery, negative material, barrier film and electrolytic solution four accounts for more than eighty per cant of battery cost.And negative pole aspect, graphite as current business-like lithium ion battery negative material, low price, Heat stability is good, environmental friendliness.
The first quarter in 2015 China's lithium cell negative pole material output 1.22 ten thousand tons, increases by 27.75% on a year-on-year basis; Negative material is domestic main based on synthetic graphite, and the first quarter, output 7200 tons, increased by 41% on a year-on-year basis; China's lithium cell cathode material output about 5.3 ten thousand tons in 2014,3.5 ten thousand tons of 2013 increase 51.43% on year-on-year basis, and negative material is main primarily of carbon materials, comprises natural graphite, synthetic graphite, greying mesocarbon microbeads.2014, lithium cell cathode material sales volume was about 4.82 ten thousand tons, increased by 30%. shipment 5.16 ten thousand tons on a year-on-year basis, increased by 31.9%. on a year-on-year basis and expected Chinese negative pole all materials industrial scale in 2015 and will reach 9.4 ten thousand tons.
Within 2014, the domestic negative material output value is 28.7 hundred million yuan, within 2013, increase 17.1%. negative material on year-on-year basis and still keep prices situation, synthetic graphite average price drop 13.8%, natural graphite average price drop 9.2%. is main because the negative material of current domestic volume production mainly contains synthetic graphite, natural graphite, carbonaceous mesophase spherules, lithium titanate etc., wherein graphite negative electrodes accounting is more than 90%. domestic graphite negative electrodes material production capacity surpluses, and supply exceed demand.
Insider points out, power cell is the principal element affecting new-energy automobile cost, its cost has been dropped to the 2.5 yuan/wh of 2014 by 3.5 yuan/about the wh of 2012, the price of battery core maintains 2 yuan/about wh substantially, more there is Some Enterprises by the price maintenance of its power brick below 2 yuan, can can resist with lead-acid cell completely at life cycle management internally-powered battery cost; In negative material field, the negative material of current mass application comprises carbon-based negative electrode material, lithium titanate anode material and alloy system negative material.Wherein carbon-based negative electrode material mainly comprises synthetic graphite, natural graphite, MCMB and Graphene.
2013, significantly gliding appearred in the overall price of Chinese lithium ion battery negative material, and rate of gross profit dropped to present about 15% from about 30% of last year, and the competition between domestic negative material enterprise is fiercer.
A kind of cathode material for lithium-ion power battery of CNIO2148355A disclosure of the invention and preparation method thereof, this negative material graphite matrix used is spherical, long-width ratio is the class spherical artificial graphite of 1.0 ~ 3.0, granularity D50 before body material is coated is 9 ~ 11 μm, matrix surface is coated with one deck non-graphite carbon material, and form " core one shell " structure, its covering amount is 2 ~ 8% of substrate quality, coated rear negative material grain graininess D50 is 10 ~ 12 μm, and specific surface area is 2 ~ 4m 2/ g, powder tapping density is 0.9 ~ 1.1g/cm3, and carbon content is more than 99.95%.Technique effect of the present invention is: cathode material for lithium-ion power battery has heavy body, high rate performance is excellent, absorbent is superior feature, and preparation method is simple simultaneously, and easily control, production cost is low, is applicable to suitability for industrialized production.
CN101798079A the present invention relates to negative material of a kind of lithium-ion-power cell and preparation method thereof, this graphite material is raw material by refinery coke, through greying, pulverize, nodularization, classification, after pitch or polymer wrapped, greying again, obtained globular graphite material, add additive synthetic graphite fine powder again, make the power battery cathode material of good rate capability.Starting material selected by this material are refinery coke, with low cost, manufacture craft simplify, product performance are superior, D50 at 7-15 μm, compacted density>=1.40, specific surface area≤2.5m 2/ g, first loading capacity>=330mAh/g, first discharging efficiency>=92%, high rate capability is excellent.This material can be used as the negative material of power cell well.
Summary of the invention
The object of this invention is to provide a kind of preparation method of lithium ion battery cathode material of low cost, after-smithing petroleum coke or pitch coke or coal tar are by adopting unique graphitization technique and equipment and studying its preparation technology and improve, simple with technique, cost is low, obtain the negative material product being applicable to lithium cell with being convenient to quality control, and obtained lithium ion battery negative material possesses features such as cost is low, good cycle.
For realizing above object, technical scheme of the present invention is:
A kind of preparation method of lithium ion battery cathode material of low cost, comprise raw material through graphitization processing, again through grinding and processing, shaping, obtain finished product, the graphitization processing of raw material is carried out in the graphitizing furnace of vertical enclosed construction, and the graphitizing furnace of described vertical enclosed construction comprises opening for feed from bottom to top, graphitizable high temperature district, high-temperature buffer district and automatic material discharge system.
Described raw material is that diameter is greater than 1cm and puts into block stock.
Described raw material be after-smithing petroleum coke, pitch coke and coal tar any one and more than.
Described refinery coke, pitch coke and coal tar are fugitive constituent <3%, ash <0.3%, the raw material of sulfur <0.5%.
The temperature in the graphitizable high temperature district of the graphitizing furnace of described vertical enclosed construction is 2400-3000 DEG C.
The granularity of material after greying after grinding and processing is 15-20 micron, powder pressing Mi Du≤0.5g/cm 3, Bi Biao Mian Ji≤5m 2/ g.
Described graphitizable high temperature district is outwards connected with smoke and waste steam boiler dust-removal system and Pneumatic floating desulphurization system in turn, and smoke and waste steam boiler also connects cogeneration group.
Circulating water cooling system is provided with around described automatic material discharge system.
The invention has the beneficial effects as follows:
Adopt the graphitizing furnace of vertical enclosed construction significantly to improve heat energy utilization, energy consumption reduces by more than 70%; Concentrated vectoring administers flue gas, and environment protection improves more than 95%; Adopt circulating water, water resources saves more than 80%; In-furnace temperature one causes product quality significantly to improve; Automatic continuous production, significantly reduces labour intensity, enhances productivity, and improves greying output; Waste heat, tailings are recycled, and experiment clean energy is produced.Target material cost ineffective benefit is high, and the market competitiveness is strong.
Accompanying drawing explanation
Fig. 1 is the graphitizing furnace schematic diagram of vertical enclosed construction;
In figure: 1, automatical feeding system; 2, opening for feed; 3, graphitizable high temperature district; 4, high-temperature buffer district; 5, automatic material discharge system; 6, circulating water cooling system; 7, smoke and waste steam boiler; 8, cogeneration unit; 9, dust-removal system; 10, Pneumatic floating desulphurization system; 11, vapor pipe; 12, extraction fan.
Embodiment
Further illustrate one embodiment of the present invention with reference to the accompanying drawings.
Embodiment one:
The after-smithing petroleum coke getting the block stock of 1000KG particle size diameter Φ >=1CM is raw material, through vertical continuous graphitizing furnace pyroprocessing, and graphitization temperature 2400-3000 DEG C, processing speed 300KG/ hour, after graphitizable high temperature process, through grinding and processing, shaping, is machined to 15-20 μm; Obtain a kind of artificial graphite material of low cost, D50 is 18.5 μm, powder pressing density: 1.92g/cm3, specific surface area: 3.2m2/g, first loading capacity: 345mAh/g, first discharging efficiency: 91.1%.
Embodiment two:
The after-smithing petroleum coke getting the block stock of 1000KG particle size diameter Φ >=1CM is raw material, through vertical continuous graphitizing furnace pyroprocessing, and graphitization temperature 2400-3000 DEG C, processing speed 300KG/ hour, after graphitizable high temperature process, through grinding and processing, shaping, is machined to 15-20 μm; Obtain a kind of artificial graphite material of low cost, D50 is 15.5 μm, powder pressing density: 1.80g/cm3, specific surface area: 6.3m2/g, first loading capacity: 342mAh/g, first discharging efficiency: 90.3%.
Embodiment three:
The after-smithing petroleum coke getting the block stock of 1000KG particle size diameter Φ >=1CM is raw material, through vertical continuous graphitizing furnace pyroprocessing, and graphitization temperature 2400-3000 DEG C, processing speed 500KG/ hour, after graphitizable high temperature process, through grinding and processing, shaping, is machined to 15-20 μm; Obtain a kind of artificial graphite material of low cost, D50 is 18.8 μm, powder pressing density: 2.02g/cm3, specific surface area: 3.2m2/g, first loading capacity: 345mAh/g, first discharging efficiency: 91.1%.
Embodiment four:
The pitch coke getting the block stock of 1000KG particle size diameter Φ >=1CM is raw material, through vertical continuous graphitizing furnace pyroprocessing, and graphitization temperature 2400-3000 DEG C, processing speed 200KG-500KG/ hour, after graphitizable high temperature process, through grinding and processing, shaping, is machined to 15-20 μm; Obtain a kind of artificial graphite material of low cost, D50 is 16.3 μm, powder pressing density: 1.86g/cm3, specific surface area: 5.6m2/g, first loading capacity: 340mAh/g, first discharging efficiency: 90.8%.
Embodiment five:
The coal tar getting the block stock of 1000KG particle size diameter Φ >=1CM is raw material, through vertical continuous graphitizing furnace pyroprocessing, and graphitization temperature 2400-3000 DEG C, processing speed 200KG-500KG/ hour, after graphitizable high temperature process, through grinding and processing, shaping, is machined to 15-20 μm; Obtain a kind of artificial graphite material of low cost, D50 is 17.4 μm, powder pressing density: 1.95g/cm3, specific surface area: 4.5m2/g, first loading capacity: 338mAh/g, first discharging efficiency: 90.2%.
Electrochemical property test:
The performance of the coated lithium ion battery negative material of hard carbon is contained for detecting the present invention, test by half-cell testing method, negative material with above embodiment and comparative example: SBR(solid content 50%): CMC=96.5:1.8:1.7(weight ratio), add appropriate amount of deionized water and reconcile into pulpous state, to coat on Copper Foil and within 12 hours, to make negative plate in vacuum drying oven inner drying; Use LiCoO2 is positive electrode active materials, with binding agent PVDF according to 94:3(weight ratio) mix, add appropriate NMP as dispersion agent furnishing slurry, be coated on aluminium foil, and make positive plate in vacuum drying oven inner drying; Electrolytic solution is 1MLiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film, is assembled into battery.Cycle performance test uses having put of 300mA to carry out constant current charge-discharge experiment, and charging/discharging voltage is limited in 4.2-3.0V, and the discharge and recharge cabinet computerizedd control carries out collection and the control of data.
X-ray diffracting spectrum:
Carry out material phase analysis with BRUKE, D8FOCUS type X-ray diffractometer (Germany produces) to gained powdered sample, use Cu target, pipe pressure 40.0kV, tube current 40.0mA, scanning speed 6o/min, step-length is 0.02o, sweep limit 10o-90o.
The principle of work of the graphitizing furnace of vertical enclosed construction is: raw material enters opening for feed 2 by automatical feeding system 1, then enter graphitizable high temperature district 3 and carry out pyroprocessing, entering automatic material discharge system 5 by high-temperature buffer district 4 after pyroprocessing, being provided with circulating water cooling system 6 around automatic material discharge system 5 for lowering the temperature to discharge system.The gas in graphitizable high temperature district enters smoke and waste steam boiler, and flue gas boiler connects the utilization of cogeneration unit raising to waste heat.The gas of smoke and waste steam boiler enters dust-removal system and carries out dedusting, then enters Pneumatic floating desulphurization system and purifies, finally discharged by vapor pipe by gas under the effect of extraction fan.
The above not imposes any restrictions technical scope of the present invention, all above embodiment is done according to the technology of the present invention essence any amendment, equivalent variations and modification, all still belong in the scope of technical scheme of the present invention.

Claims (8)

1. the preparation method of the lithium ion battery cathode material of a low cost, comprise raw material through graphitization processing, again through grinding and processing, shaping, obtain finished product, it is characterized in that: the graphitization processing of raw material is carried out in the graphitizing furnace of vertical enclosed construction, the graphitizing furnace of described vertical enclosed construction comprises opening for feed from bottom to top, graphitizable high temperature district, high-temperature buffer district and automatic material discharge system.
2. the preparation method of the lithium ion battery cathode material of low cost according to claim 1, is characterized in that: described raw material is that diameter is greater than 1cm and puts into block stock.
3. the preparation method of the lithium ion battery cathode material of low cost according to claim 1, is characterized in that: described raw material be after-smithing petroleum coke, pitch coke and coal tar any one and more than.
4. the preparation method of the lithium ion battery cathode material of low cost according to claim 3, it is characterized in that: described refinery coke, pitch coke and coal tar are fugitive constituent <3%, ash <0.3%, the raw material of sulfur <0.5%.
5. the preparation method of the lithium ion battery cathode material of low cost according to claim 1, is characterized in that: the temperature in the graphitizable high temperature district of the graphitizing furnace of described vertical enclosed construction is 2400-3000 DEG C.
6. the preparation method of the lithium ion battery cathode material of low cost according to claim 1, is characterized in that: the granularity of the material after greying after grinding and processing is 15-20 micron, powder pressing Mi Du≤0.5g/cm 3, Bi Biao Mian Ji≤5m 2/ g.
7. the preparation method of the lithium ion battery cathode material of low cost according to claim 1, it is characterized in that: described graphitizable high temperature district is outwards connected with smoke and waste steam boiler dust-removal system and Pneumatic floating desulphurization system in turn, and smoke and waste steam boiler also connects cogeneration group.
8. the preparation method of the lithium ion battery cathode material of low cost according to claim 1, is characterized in that: be provided with circulating water cooling system around described automatic material discharge system.
CN201510851428.1A 2015-11-30 2015-11-30 Preparation method of low-cost negative electrode material of power lithium ion battery Pending CN105347333A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106058158A (en) * 2016-07-21 2016-10-26 青岛海达新能源材料有限公司 Full-automatic continuous production equipment for anode material of lithium ion battery and method
CN109248637A (en) * 2017-07-14 2019-01-22 上海杉杉科技有限公司 The Equipment for Heating Processing and application method of continous way lithium ion battery negative material
CN110723730A (en) * 2019-10-21 2020-01-24 广东羚光新材料股份有限公司 High-specific-volume high-cycle-performance artificial graphite material and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201581943U (en) * 2010-01-25 2010-09-15 新郑市东升炭素有限公司 Device for recycling and utilizing waste heat of carbon-graphitized high-temperature flue gas
CN201647998U (en) * 2010-02-10 2010-11-24 黎应和 Vertical, high-temperature and continuous graphitizing furnace and cooling system thereof
CN104477885A (en) * 2014-11-20 2015-04-01 中国电子科技集团公司第四十八研究所 Vertical continuous induction type high-temperature graphitization furnace
CN204490511U (en) * 2015-02-10 2015-07-22 新郑市东升炭素有限公司 The horizontal broken artificial graphite treatment facility of novel vertical electrode
JP2015189644A (en) * 2014-03-28 2015-11-02 Ｊｘ日鉱日石エネルギー株式会社 Vertical graphitization furnace and method for producing graphite

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201581943U (en) * 2010-01-25 2010-09-15 新郑市东升炭素有限公司 Device for recycling and utilizing waste heat of carbon-graphitized high-temperature flue gas
CN201647998U (en) * 2010-02-10 2010-11-24 黎应和 Vertical, high-temperature and continuous graphitizing furnace and cooling system thereof
JP2015189644A (en) * 2014-03-28 2015-11-02 Ｊｘ日鉱日石エネルギー株式会社 Vertical graphitization furnace and method for producing graphite
CN104477885A (en) * 2014-11-20 2015-04-01 中国电子科技集团公司第四十八研究所 Vertical continuous induction type high-temperature graphitization furnace
CN204490511U (en) * 2015-02-10 2015-07-22 新郑市东升炭素有限公司 The horizontal broken artificial graphite treatment facility of novel vertical electrode

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106058158A (en) * 2016-07-21 2016-10-26 青岛海达新能源材料有限公司 Full-automatic continuous production equipment for anode material of lithium ion battery and method
CN109248637A (en) * 2017-07-14 2019-01-22 上海杉杉科技有限公司 The Equipment for Heating Processing and application method of continous way lithium ion battery negative material
CN109248637B (en) * 2017-07-14 2023-04-11 上海杉杉科技有限公司 Heat treatment equipment for continuous lithium ion battery cathode material and use method
CN110723730A (en) * 2019-10-21 2020-01-24 广东羚光新材料股份有限公司 High-specific-volume high-cycle-performance artificial graphite material and preparation method and application thereof

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Application publication date: 20160224