CN101572302B - Method for preparing cathode materials of power lithium ion secondary batteries - Google Patents
Method for preparing cathode materials of power lithium ion secondary batteries Download PDFInfo
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- CN101572302B CN101572302B CN2009100196980A CN200910019698A CN101572302B CN 101572302 B CN101572302 B CN 101572302B CN 2009100196980 A CN2009100196980 A CN 2009100196980A CN 200910019698 A CN200910019698 A CN 200910019698A CN 101572302 B CN101572302 B CN 101572302B
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- ion secondary
- secondary batteries
- lithium ion
- power lithium
- cathode materials
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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
Abstract
The invention relates to a method for preparing cathode materials of power lithium ion secondary batteries, which is mainly used for preparing the cathode materials of the power lithium ion secondary batteries. The preparation method mainly comprises the following steps: adopting phenol-formaldehyde resin as a raw material, adding a certain proportion of additive, placing the mixture into a carbonization furnace for carbonization in the vacuum state at the temperature of between 600 and 800 DEG C, using a crushing and classifying machine to crush and classify the obtained pyrolytic carbon after carbonization, using a certain proportion of coating agent to coat the obtained materials with the particle diameter of between 5 and 30 mu m, crosslinking the coating agent on the surface of the pyrolytic carbon at the temperature of 300 DEG C to form a coated shell, and preparing the cathode materials of the power lithium ion secondary batteries after performing carbonization on the coated materials at the temperature of 700 DEG C and high-temperature graphitization on the coated materials at the temperature of 2,800 DEG C, wherein the reversible capacity of the cathode materials of the power lithium ion secondary batteries reaches 600 mAh/g, the cycle index reaches 600 times, and the cycle efficiency reaches 96 percent.
Description
One, technical field:
The invention belongs to a kind of preparation method of chemical field, be mainly used in a kind of preparation of cathode materials of power lithium ion secondary batteries.
Two, background technology:
Cathode materials of power lithium ion secondary batteries belongs to new high-tech product, and Main Function is to provide negative material for power lithium-ion rechargeable battery.The manufacturing process of at present traditional ion secondary battery cathode material lithium is complicated, environment there is certain pollution, the ion secondary battery cathode material lithium capacity of making is low, cycle-index is few, do not satisfy market to the instructions for use of cathode materials of power lithium ion secondary batteries, be badly in need of wanting a kind of better preparation technology to come out, to produce high-quality ion secondary battery cathode material lithium, meet the need of market.
Three, summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of cathode materials of power lithium ion secondary batteries produces the cathode materials of power lithium ion secondary batteries of function admirable, and the negative material of super quality and competitive price is provided for high-grade power lithium-ion rechargeable battery.
This preparation method mainly is that employing phenolic resins is raw material, add a certain proportion of additive, compound inserted under vacuum state, carry out charing in the retort, carbonization temperature is 600-800 ℃, behind the pyrolytic carbon process pulverizing grading machine crushing and classification of the good gained of charing, the material of gained 5-30um coats with a certain proportion of covering, adopt again 300 ℃ of temperature that covering is surface-crosslinked at pyrolytic carbon, form encasement, material after the coating is through 700 ℃ of charings, make reversible capacity behind 2800 ℃ of high temperature graphitizations and reach 600mAh/g, cycle-index 600 times, the cathode materials of power lithium ion secondary batteries of cycle efficieny 96%.
Described additive is one or more of 1-METHYLPYRROLIDONE, anhydrous stannous chloride, stannous chloride, butter of tin.
The proportioning of described additive and raw material is 1: 50.
Described covering is one or more of dimethyl ethyl carbonate, butyl lithium, n-hexane, naphthalene.
The proportioning of described covering and material is 1: 100.
The main beneficial effect of this method is owing to adopting additive so that phenolic resins pyrolysis in pyrolytic process is thorough, melt and state even, without shrinking pore.
Owing to adopting covering, the pyrolytic carbon and the covering that produce after the phenolic resins pyrolysis process are coated, after 300 ℃ of heating coverings are crosslinked, form encasement, further improved chemical property and the life cycle of pyrolytic carbon, make pyrolytic carbon state in encasement more stable.
Four, execution mode:
This preparation method is specific as follows: adopt the phenolic resins that meets the requirements through washing, 50 ℃ of oven dry, the raw material that obtains meeting the requirements, add in the retort at 50: 1 raw material and the additive handled well in proportion, vacuumize, be heated to 600-800 ℃ by 3-5 ℃/min, after constant temperature 3-5 hour, naturally be cooled to room temperature, the solids that obtains is crushed to 35um with thin section with pulverizer, and with grader will be wherein the 5-30um powder classification go out, this powder stirred 2-3 hour in stirred tank after adding covering by 1: 100, the still temperature control is at 90-100 ℃, afterwards, the gained compound inserted in the baking oven be heated to 300 ℃ by 5-10 ℃/min heating rate, constant temperature 2-3 hour, afterwards, material is heated to 700 ℃ by 10-15 ℃/min heating rate under vacuum state, constant temperature 2-3 hour, the material after the charing was heated to 2800 ℃ by 10-15 ℃/min heating rate under air-tight state, constant temperature 2-3 hour, the gained material again after the classified processing wherein the material classification of 5-30um go out, prepared pyrolytic carbon powder reversible capacity reaches 600mAh/g, cycle-index 600 times, cycle efficieny 96%, with the pyrolytic carbon powder-product that makes after testing after, with the vacuum-packed warehouse-in of fiber can.
The phenolic resins the key technical indexes that adopts sees Table one
| Model | Viscosity mPas (25 ℃) | Free phenol (%) | Free select | Moisture (%) | Solid content (%) | PH value |
| PF-1001 | 400-1000 | ＜13.0 | ＜3.0 | ＜14.0 | ≥75.0 | 6.8-7.2 |
Preparation method's main technologic parameters of a kind of cathode materials of power lithium ion secondary batteries of the present invention sees Table two
| Sequence number | Phenolic resins (kg) | Additive (kg) | Covering (kg) |
| 1 | 100 | One or more of 2 1-METHYLPYRROLIDONEs, anhydrous stannous chloride, stannous chloride, butter of tin. | One or more of 1 dimethyl ethyl carbonate, butyl lithium, n-hexane, naphthalene |
Cathode materials of power lithium ion secondary batteries of the present invention and common ion secondary battery cathode material lithium technical indicator contrast table see Table three
Claims (1)
1. the preparation method of a cathode materials of power lithium ion secondary batteries, mainly by the raw material proportioning, charing, crushing and classification, coat, crosslinked, charing, the pyrographite metallization processes forms, it is characterized in that: employing phenolic resins is raw material, add a certain proportion of additive, compound inserted under vacuum state, carry out charing in the retort, carbonization temperature is 600-800 ℃, behind the pyrolytic carbon process pulverizing grading machine crushing and classification of the good gained of charing, the material of gained 5-30um coats with a certain proportion of covering, adopt again 300 ℃ of temperature that covering is surface-crosslinked at pyrolytic carbon, form encasement, material after the coating is through 700 ℃ of charings, make reversible capacity behind 2800 ℃ of high temperature graphitizations and reach 600mAh/g, cycle-index 600 times, the cathode materials of power lithium ion secondary batteries of cycle efficieny 96%;
Wherein, additive is one or more of 1-METHYLPYRROLIDONE, anhydrous stannous chloride, stannous chloride, butter of tin, and the proportioning of described additive and raw material is 1: 50; Described covering is one or more of dimethyl ethyl carbonate, butyl lithium, n-hexane, naphthalene, and the proportioning of described covering and material is 1: 100.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100196980A CN101572302B (en) | 2009-03-07 | 2009-03-07 | Method for preparing cathode materials of power lithium ion secondary batteries |
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| CN2009100196980A CN101572302B (en) | 2009-03-07 | 2009-03-07 | Method for preparing cathode materials of power lithium ion secondary batteries |
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| CN101572302A CN101572302A (en) | 2009-11-04 |
| CN101572302B true CN101572302B (en) | 2013-01-09 |
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| CN2009100196980A Expired - Fee Related CN101572302B (en) | 2009-03-07 | 2009-03-07 | Method for preparing cathode materials of power lithium ion secondary batteries |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101916845B (en) * | 2010-08-05 | 2012-12-05 | 深圳市贝特瑞新能源材料股份有限公司 | Hard carbon material for power and energy-storage battery and preparation method thereof |
| CN101887966B (en) * | 2010-06-18 | 2012-12-05 | 深圳市贝特瑞新能源材料股份有限公司 | Preparation method of composite hard carbon cathode material of lithium ion battery |
| CN101894939B (en) * | 2010-07-02 | 2014-04-16 | 重庆大学 | Nano-Si or nano-Sn containing composite cathode material for lithium ion battery and preparation method thereof |
| CN101969122A (en) * | 2010-09-14 | 2011-02-09 | 东莞市迈科新能源有限公司 | Core-shell structured carbon for cathode material of lithium ion battery and preparation method thereof |
| CN105609761B (en) * | 2015-09-10 | 2018-05-11 | 昆明理工大学 | A kind of application of CuCl/Cu composite materials |
| CN106486652A (en) * | 2015-11-15 | 2017-03-08 | 上海杉杉科技有限公司 | A kind of graphite negative material of lithium ion battery and preparation method thereof |
| CN109873173A (en) * | 2019-02-28 | 2019-06-11 | 栗陶然 | A kind of preparation method of direct alcohol fuel cell cathode support body material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5595838A (en) * | 1992-02-04 | 1997-01-21 | Sharp Kabushiki Kaisha | Method for manufacturing carbon composite electrode material |
| CN1304187A (en) * | 1999-12-15 | 2001-07-18 | 北京有色金属研究总院 | Composite graphite negative electrode material for lithium cell and its preparation method |
| 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5595838A (en) * | 1992-02-04 | 1997-01-21 | Sharp Kabushiki Kaisha | Method for manufacturing carbon composite electrode material |
| CN1304187A (en) * | 1999-12-15 | 2001-07-18 | 北京有色金属研究总院 | Composite graphite negative electrode material for lithium cell and its preparation method |
| 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 |
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