CN105024074B - A kind of preparation method using resin as the lithium ion battery negative material of raw material - Google Patents
A kind of preparation method using resin as the lithium ion battery negative material of raw material Download PDFInfo
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- CN105024074B CN105024074B CN201410157586.2A CN201410157586A CN105024074B CN 105024074 B CN105024074 B CN 105024074B CN 201410157586 A CN201410157586 A CN 201410157586A CN 105024074 B CN105024074 B CN 105024074B
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
It is a kind of using resin as the preparation method of the lithium ion battery negative material of raw material, be characterized in that:By material based on resin, by completely cutting off after air in 350 500 DEG C of progress polycondensation reactions, material after polycondensation reaction is carbonized through 800 1100 DEG C again, material after carbonization is crushed, add kneading after bonding agent, it will be calcined after material water cooling after shaping, after roasting after baking is carried out after material filling impregnating agent, by the material after roasting by 2,300 3300 DEG C of high-temperature process, material after high-temperature process is crushed successively, milling, screening and surface treatment, surface-treated material is carried out to surface successively to be modified reformation and add additive, the material added after additive is subjected to screening after 2,100 2900 DEG C of high-temperature process again and obtains finished product;1%/moon is less than using the technical scheme self discharge, had extended cycle life, high rate performance is high, capacity is high, production efficiency is high and cost is low.
Description
Technical field
The present invention relates in technical field of lithium ion battery negative, more particularly to a kind of lithium using resin as raw material from
Sub- cell negative electrode material and preparation method thereof.
Background technology
With the urgent need for low-carbon, green and circular economy, the research of new energy resource power battery is developed rapidly,
Lithium ion battery has that operating voltage height, discharging voltage balance, low temperature performance well, specific energy are high, self discharge is small, memoryless effect
Should, environmentally friendly and long service live advantage, be electrochemical educational circles's study hotspot in recent years, wherein, ion cathode material lithium
It is the key factor for determining performance of lithium ion battery.
In recent years, lithium ion battery negative material is still to be occupied an leading position with charcoal graphite type material in actual applications,
But because there is certain difference and charcoal graphite type material sheet in the performance of the different charcoal graphite cathode material of raw material sources
Generally improve the electrical property of charcoal graphite type material using various physics, chemical means in the certain defect that body is present, industry, its
In, many by the practical approach of surface modification treatment, the surface treatment method of negative material is followed for improving capacity and improvement
Ring performance has certain effect, no matter therefore for native graphite or artificial plumbago negative pole material, process for treating surface is in life
All in very important status during production.
Phenolic resin is a kind of common high polymer material, and phenolic resin starting material is inexpensive, abundance, high fixing carbon, low
Toxicity etc., the synthesis cost of phenolic resin material is low in addition, technique is simple.
But the self discharge of existing lithium ion battery negative material is higher than for 1%/moon, and cycle life is short, high rate performance is poor,
Capacity is low, low production efficiency and cost height.
The content of the invention
In order to solve the above problems, the present invention provides a kind of preparation using resin as the lithium ion battery negative material of raw material
Method.
A kind of preparation method using resin as the lithium ion battery negative material of raw material, it is characterised in that:Using resin as
Basic material, by completely cutting off in 350-500 DEG C of progress polycondensation reaction after air, the reaction time is 3 hours, after polycondensation reaction
It is carbonized again through 800-1100 DEG C after material isolation air, this time carbonization time is 2 to 4 hours, and the material after carbonization is entered
Row is broken, and the requirement further according to average grain diameter carries out dispensing, adds kneading after bonding agent, and cool material shaping forms resin glue;
But it is calcined the material after shaping is water cooled afterwards, sintering temperature is 800-1100 DEG C, and this time roasting time is
3-4 hours, the material after roasting was filled and after baking is carried out after impregnating agent, and after baking temperature is 750-900 DEG C, is this time calcined
Time is 2-3 hours, and the material after roasting was risen into 2300-3300 DEG C of high-temperature process by room temperature at 10 hours to 20 hours, will
Material after high-temperature process is crushed successively, milling, screening and surface treatment, and surface-treated material is carried out into table successively
Face, which is modified, reforms and adds additive, and the material added after additive was risen into 2100- by room temperature to 14 hours by 8 hours again
2900 DEG C of high-temperature process, final sizing obtains finished product.
The binding agent is polyimide binder.
The impregnating agent is coal tar pitch, and the softening point of the coal tar pitch is 75 DEG C~90 DEG C.
The resin is phenolic resin.
The mesh number of the screening is 350 mesh.
It is described it is broken after maximum particle diameter be 30 μm to 50 μm.
The additive is phenolic resin.
The requirement of the average grain diameter is 8.0mm to 4mm.
Advantages of the present invention:
1, self discharge 1%/moons of ﹤;
2, have extended cycle life, good rate capability;
3, capacity is high;
4, technique is simple, and production efficiency is high;
5, cost is low, promotes economic benefit.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated;It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
A kind of preparation method using resin as the lithium ion battery negative material of raw material, material based on resin leads to
Cross and carry out polycondensation reaction after isolation air at 350 DEG C, the reaction time is 3 hours, after the material isolation air after polycondensation reaction
It is carbonized again through 800 DEG C, this time carbonization time is 2 hours, the material after carbonization is crushed, further according to average grain diameter
It is required that carrying out dispensing, the requirement of the particle diameter adds kneading after bonding agent, cool material shaping;
But it is calcined the material after shaping is water cooled afterwards, sintering temperature is 800 DEG C, the roasting time is 3 hours, roasting
After baking is carried out after material filling impregnating agent after burning, after baking temperature is 750 DEG C, and this time roasting time is 2 hours, will
Material after roasting rose to 2300 DEG C of high-temperature process at 10 hours by room temperature, and the room temperature is 0 DEG C to 30 DEG C, after high-temperature process
Material is crushed successively, milling, screening and be surface-treated, surface-treated material is carried out successively surface be modified reform and
Additive is added, the material after additive will be added 2100 DEG C of high-temperature process are risen to by room temperature by 8 hours again, the room temperature is 0
DEG C to 30 DEG C, final sizing obtains finished product.
The binding agent is polyimide binder.
The impregnating agent is coal tar pitch, and the softening point of the coal tar pitch is 75 DEG C.
The resin is phenolic resin.
The mesh number of the screening is 350 mesh.
It is described it is broken after maximum particle diameter be 30 μm.
The additive is phenolic resin.
The requirement of the average grain diameter is 8.0mm.
Embodiment 2
A kind of preparation method using resin as the lithium ion battery negative material of raw material, material based on resin leads to
Cross and carry out polycondensation reaction after isolation air at 420 DEG C, the reaction time is 3 hours, after the material isolation air after polycondensation reaction
It is carbonized again through 1000 DEG C, this time carbonization time is 3 hours, the material after carbonization is crushed, further according to average grain diameter
Requirement carry out dispensing, add kneading after bonding agent, the shaping of cool material;
But it is calcined the material after shaping is water cooled afterwards, sintering temperature is 1000 DEG C, the roasting time is 3.5 small
When, the material after roasting is filled and after baking is carried out after impregnating agent, and after baking temperature is 800 DEG C, and this time roasting time is 2.5
Hour, the material after roasting was risen into 2900 DEG C of high-temperature process at 15 hours by room temperature, the room temperature is 0 DEG C to 30 DEG C, by high temperature
Material after processing is crushed successively, milling, screening and surface treatment, and surface-treated material is carried out to surface successively and changed
Property reform and add additive, by add additive after material 2600 DEG C of high-temperature process are risen to by room temperature by 11 hours again,
The room temperature is 0 DEG C to 30 DEG C, and final sizing obtains finished product.
The binding agent is polyimide binder.
The impregnating agent is coal tar pitch, and the softening point of the coal tar pitch is 85 DEG C.
The resin is phenolic resin.
The mesh number of the screening is 350 mesh.
It is described it is broken after maximum particle diameter be 40 μm.
The additive is phenolic resin.
The requirement of the average grain diameter is 6.0mm.
Embodiment 3
A kind of preparation method using resin as the lithium ion battery negative material of raw material, material based on resin leads to
Cross and carry out polycondensation reaction after isolation air at 500 DEG C, the reaction time is 3 hours, after the material isolation air after polycondensation reaction
It is carbonized again through 1100 DEG C, this time carbonization time is 4 hours, the material after carbonization is crushed, further according to average grain diameter
Requirement carry out dispensing, add kneading after bonding agent, the shaping of cool material;
But it is calcined the material after shaping is water cooled afterwards, sintering temperature is 1100 DEG C, the roasting time is 4 hours,
After baking is carried out after material filling impregnating agent after roasting, after baking temperature is 900 DEG C, and this time roasting time is 3 hours,
Material after roasting was risen into 3300 DEG C of high-temperature process at 20 hours by room temperature, the room temperature is 0 DEG C to 30 DEG C, after high-temperature process
Material crushed successively, be milled, screening and be surface-treated, surface-treated material is carried out successively surface be modified reformation
With addition additive, the material added after additive was risen into 2900 DEG C of high-temperature process, the room temperature by 14 hours by room temperature again
For 0 DEG C to 30 DEG C, final sizing obtains finished product.
The binding agent is polyimide binder.
The impregnating agent is coal tar pitch, and the softening point of the coal tar pitch is 90 DEG C.
The resin is phenolic resin.
The mesh number of the screening is 350 mesh.
It is described it is broken after maximum particle diameter be 50 μm.
The additive is phenolic resin.
The requirement of the average grain diameter is 4.0mm.
Embodiment result:
Negative material performance is:
Claims (5)
1. a kind of preparation method using resin as the lithium ion battery negative material of raw material, it is characterised in that:It regard resin as base
Plinth material, polycondensation reaction is carried out by completely cutting off at 350-500 DEG C after air, the reaction time is 3 hours, the material after polycondensation reaction
It is carbonized again through 800-1100 DEG C after material isolation air, this carbonization time is 2 to 4 hours, and the material after carbonization is carried out
Broken, the requirement further according to average grain diameter carries out dispensing, adds kneading after binding agent, cool material shaping;
But it is calcined the material after shaping is water cooled afterwards, sintering temperature is 800-1100 DEG C, and this roasting time is 3-4
Hour, after baking is carried out after the material filling impregnating agent after roasting, after baking temperature is 750-900 DEG C, when being this time calcined
Between be 2-3 hours, the material after roasting was risen into 2300-3300 DEG C of high-temperature process to 20 hours at 10 hours by room temperature, by height
Material after temperature processing is crushed successively, is milled, screening and surface treatment, and surface-treated material is carried out into surface successively
It is modified to reform and add additive, the material added after additive was risen into 2100- to 14 hours by 8 hours by room temperature again
2900 DEG C of high-temperature process, final sizing obtains finished product, and the impregnating agent is coal tar pitch, and the softening point of the coal tar pitch is 75 DEG C~90
DEG C, the resin is phenolic resin, and the additive is phenolic resin.
2. a kind of preparation method using resin as the lithium ion battery negative material of raw material according to claim 1, it is special
Levy and be:The binding agent is polyimide binder.
3. a kind of preparation method using resin as the lithium ion battery negative material of raw material according to claim 1, it is special
Levy and be:The mesh number of the screening is 350 mesh.
4. a kind of preparation method using resin as the lithium ion battery negative material of raw material according to claim 1, it is special
Levy and be:It is described it is broken after maximum particle diameter be 30 μm to 50 μm.
5. a kind of preparation method using resin as the lithium ion battery negative material of raw material according to claim 1, it is special
Levy and be:The requirement of the average grain diameter is 8.0mm to 4mm.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102479943A (en) * | 2010-11-30 | 2012-05-30 | 上海杉杉科技有限公司 | Hard carbon cathode material, preparation method and use thereof |
CN102502594A (en) * | 2011-10-14 | 2012-06-20 | 上海理工大学 | Method for preparing isotropic graphite containing coal-based needle coke as aggregate |
CN102881869A (en) * | 2012-09-26 | 2013-01-16 | 东莞市翔丰华电池材料有限公司 | Modified hard carbon negative electrode material for lithium ion battery and preparation method for modified hard carbon negative electrode material |
Family Cites Families (1)
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JP3716830B2 (en) * | 2002-11-28 | 2005-11-16 | 日本カーボン株式会社 | Method for producing negative electrode material for lithium ion secondary battery |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102479943A (en) * | 2010-11-30 | 2012-05-30 | 上海杉杉科技有限公司 | Hard carbon cathode material, preparation method and use thereof |
CN102502594A (en) * | 2011-10-14 | 2012-06-20 | 上海理工大学 | Method for preparing isotropic graphite containing coal-based needle coke as aggregate |
CN102881869A (en) * | 2012-09-26 | 2013-01-16 | 东莞市翔丰华电池材料有限公司 | Modified hard carbon negative electrode material for lithium ion battery and preparation method for modified hard carbon negative electrode material |
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