CN105024074A - Preparation method of lithium ion battery cathode material adopting resin as raw material - Google Patents
Preparation method of lithium ion battery cathode material adopting resin as raw material Download PDFInfo
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- CN105024074A CN105024074A CN201410157586.2A CN201410157586A CN105024074A CN 105024074 A CN105024074 A CN 105024074A CN 201410157586 A CN201410157586 A CN 201410157586A CN 105024074 A CN105024074 A CN 105024074A
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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 preparation method of a lithium ion battery cathode material adopting resin as a raw material. The technical key point lies in taking resin as a basic material, performing polycondensation for the resin by insulating the air at the temperature of 350 to 500 DEG C, then carbonizing the polycondensed material at 800 to 1100 DEG C, crushing the carbonized material, mixing the crushed material and a bonding agent to obtain a mixture, kneading the mixture, water cooling a molded material, then baking the molded material, filling the baked material with a soaking agent, then performing the secondary baking, treating the baked material at a high temperature of 2300 to 3300 DEG C, sequentially crushing, grinding, screening and surface treating the high-temperature treated material, performing the surface modified reshaping for the surface-treated material, adding an additive into the reshaped material, then treating the material at a high temperature of 2100 to 2900 DEG C, and screening to obtain a finished product. By adopting the technical scheme, the self discharge is lower than 1 percent per month, the cycle life is long, the rate capacity is high, the capacity is high, the production efficiency is high, and the cost is low.
Description
Technical field
The present invention relates in technical field of lithium ion battery negative, particularly a kind of take resin as the lithium ion battery cathode material and its preparation method of raw material.
Background technology
Along with low-carbon (LC), green, recycling economy in the urgent need to, the research of new energy resource power battery is developed rapidly, lithium ion battery has that operating voltage is high, discharging voltage balance, cryogenic property are good, specific energy is high, self discharge is little, the advantage of memory-less effect, environmentally friendly and long service live, it is electrochemical educational circles study hotspot in recent years, wherein, ion cathode material lithium is the key factor determining performance of lithium ion battery.
In recent years, lithium ion battery negative material remains in actual applications occupies an leading position with charcoal graphite type material, but there is the certain defect that certain difference and charcoal graphite type material itself exist in the serviceability due to the different charcoal graphite cathode material of raw material sources, usually various physics is adopted in industry, chemical means improves the electrical property of charcoal graphite type material, wherein, a lot of by the practical approach of surface modification treatment, the surface treatment method of negative material is for raising capacity and improve cycle performance and have certain effect, no matter therefore for native graphite or artificial plumbago negative pole material, process for treating surface is all in very important status in process of production.
Phenolic resins is a kind of common macromolecular material, and phenolic resin starting material is inexpensive, abundance, high fixing carbon, hypotoxicity etc., and 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 1%/moon, cycle life is short, high rate performance is poor, and capacity is low, and production efficiency is low and cost is high.
Summary of the invention
In order to solve the problem, the invention provides a kind of take resin as the preparation method of the lithium ion battery negative material of raw material.
A kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: by material based on resin, by carrying out polycondensation reaction at 350-500 DEG C after isolated air, this reaction time is 3 hours, carries out carbonization again after the material isolates air after polycondensation reaction through 800-1100 DEG C, this time carbonization time is 2 to 4 hours, material after carbonization is carried out fragmentation, then prepares burden according to the requirement of average grain diameter, add kneading after bonding agent, cool material is shaping, forms resin glue;
Material after shaping is carried out roasting after water cooling, sintering temperature is 800-1100 DEG C, this roasting time is 3-4 hour, material after roasting carries out after baking after filling impregnating agent, after baking temperature is 750-900 DEG C, this time roasting time is 2-3 hour, material after roasting was littlely risen to 2300-3300 DEG C of high-temperature process up to 20 hours by room temperature 10, material after high-temperature process is carried out fragmentation successively, abrasive dust, screening and surface treatment, surface-treated material carried out successively surface modification reformation and add additive, again littlely 2100-2900 DEG C of high-temperature process was risen to up to 14 hours by room temperature by 8 by adding the material after additive, final sizing obtains finished product.
Described binding agent is polyimide binder.
Described impregnating agent is coal tar pitch, and the softening point of this coal tar pitch is 75 DEG C ~ 90 DEG C.
Described resin is phenolic resins.
The order number of described screening is 350 orders.
Maximum particle diameter after described fragmentation is 30 μm to 50 μm.
Described additive is phenolic resins.
The requirement of described average grain diameter is 8.0mm to 4mm.
Advantage of the present invention:
1,1%/moon of self discharge ﹤;
2, to 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 object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated; Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
A kind of take resin as the preparation method of the lithium ion battery negative material of raw material, by material based on resin, by carrying out polycondensation reaction at 350 DEG C after isolated air, this reaction time is 3 hours, carries out carbonization again after the material isolates air after polycondensation reaction through 800 DEG C, this time carbonization time is 2 hours, material after carbonization is carried out fragmentation, then prepares burden according to the requirement of average grain diameter, the requirement of this particle diameter, add kneading after bonding agent, cool material is shaping;
Material after shaping is carried out roasting after water cooling, sintering temperature is 800 DEG C, this roasting time is 3 hours, material after roasting carries out after baking after filling impregnating agent, after baking temperature is 750 DEG C, this time roasting time is 2 hours, material after roasting was risen to 2300 DEG C of high-temperature process at 10 hours by room temperature, this room temperature is 0 DEG C to 30 DEG C, material after high-temperature process is carried out fragmentation successively, abrasive dust, screening and surface treatment, surface-treated material carried out successively surface modification reformation and add additive, again 2100 DEG C of high-temperature process were risen to by 8 hours by room temperature by adding the material after additive, this room temperature is 0 DEG C to 30 DEG C, final sizing obtains finished product.
Described binding agent is polyimide binder.
Described impregnating agent is coal tar pitch, and the softening point of this coal tar pitch is 75 DEG C.
Described resin is phenolic resins.
The order number of described screening is 350 orders.
Maximum particle diameter after described fragmentation is 30 μm.
Described additive is phenolic resins.
The requirement of described average grain diameter is 8.0mm.
Embodiment 2
A kind of take resin as the preparation method of the lithium ion battery negative material of raw material, by material based on resin, by carrying out polycondensation reaction at 420 DEG C after isolated air, this reaction time is 3 hours, carries out carbonization again after the material isolates air after polycondensation reaction through 1000 DEG C, and this time carbonization time is 3 hours, material after carbonization is carried out fragmentation, prepare burden according to the requirement of average grain diameter, add kneading after bonding agent, cool material is shaping again;
Material after shaping is carried out roasting after water cooling, sintering temperature is 1000 DEG C, this roasting time is 3.5 hours, material after roasting carries out after baking after filling impregnating agent, after baking temperature is 800 DEG C, this time roasting time is 2.5 hours, material after roasting was risen to 2900 DEG C of high-temperature process at 15 hours by room temperature, this room temperature is 0 DEG C to 30 DEG C, material after high-temperature process is carried out fragmentation successively, abrasive dust, screening and surface treatment, surface-treated material carried out successively surface modification reformation and add additive, again 2600 DEG C of high-temperature process were risen to by 11 hours by room temperature by adding the material after additive, this room temperature is 0 DEG C to 30 DEG C, final sizing obtains finished product.
Described binding agent is polyimide binder.
Described impregnating agent is coal tar pitch, and the softening point of this coal tar pitch is 85 DEG C.
Described resin is phenolic resins.
The order number of described screening is 350 orders.
Maximum particle diameter after described fragmentation is 40 μm.
Described additive is phenolic resins.
The requirement of described average grain diameter is 6.0mm.
Embodiment 3
A kind of take resin as the preparation method of the lithium ion battery negative material of raw material, by material based on resin, by carrying out polycondensation reaction at 500 DEG C after isolated air, this reaction time is 3 hours, carries out carbonization again after the material isolates air after polycondensation reaction through 1100 DEG C, and this time carbonization time is 4 hours, material after carbonization is carried out fragmentation, prepare burden according to the requirement of average grain diameter, add kneading after bonding agent, cool material is shaping again;
Material after shaping is carried out roasting after water cooling, sintering temperature is 1100 DEG C, this roasting time is 4 hours, material after roasting carries out after baking after filling impregnating agent, after baking temperature is 900 DEG C, this time roasting time is 3 hours, material after roasting was risen to 3300 DEG C of high-temperature process at 20 hours by room temperature, this room temperature is 0 DEG C to 30 DEG C, material after high-temperature process is carried out fragmentation successively, abrasive dust, screening and surface treatment, surface-treated material carried out successively surface modification reformation and add additive, again 2900 DEG C of high-temperature process were risen to by 14 hours by room temperature by adding the material after additive, this room temperature is 0 DEG C to 30 DEG C, final sizing obtains finished product.
Described binding agent is polyimide binder.
Described impregnating agent is coal tar pitch, and the softening point of this coal tar pitch is 90 DEG C.
Described resin is phenolic resins.
The order number of described screening is 350 orders.
Maximum particle diameter after described fragmentation is 50 μm.
Described additive is phenolic resins.
The requirement of described average grain diameter is 4.0mm.
Embodiment result:
Negative material performance is:
Claims (8)
1. one kind take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: by material based on resin, by carrying out polycondensation reaction at 350-500 DEG C after isolated air, this reaction time is 3 hours, carries out carbonization again after the material isolates air after polycondensation reaction through 800-1100 DEG C, and this time carbonization time is 2 to 4 hours, material after carbonization is carried out fragmentation, prepare burden according to the requirement of average grain diameter, add kneading after bonding agent, cool material is shaping again;
Material after shaping is carried out roasting after water cooling, sintering temperature is 800-1100 DEG C, this roasting time is 3-4 hour, material after roasting carries out after baking after filling impregnating agent, after baking temperature is 750-900 DEG C, this time roasting time is 2-3 hour, material after roasting was littlely risen to 2300-3300 DEG C of high-temperature process up to 20 hours by room temperature 10, material after high-temperature process is carried out fragmentation successively, abrasive dust, screening and surface treatment, surface-treated material carried out successively surface modification reformation and add additive, again littlely 2100-2900 DEG C of high-temperature process was risen to up to 14 hours by room temperature by 8 by adding the material after additive, final sizing obtains finished product.
2. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: described binding agent is polyimide binder.
3. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: described impregnating agent is coal tar pitch, the softening point of this coal tar pitch is 75 DEG C ~ 90 DEG C.
4. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: described resin is phenolic resins.
5. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: the order number of described screening is 350 orders.
6. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: the maximum particle diameter after described fragmentation is 30 μm to 50 μm.
7. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: described additive is phenolic resins.
8. according to claim 1 a kind of take resin as the preparation method of the lithium ion battery negative material of raw material, it is characterized in that: the requirement of described average grain diameter is 8.0mm to 4mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410157586.2A CN105024074B (en) | 2014-04-18 | 2014-04-18 | A kind of preparation method using resin as the lithium ion battery negative material of raw material |
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| CN201410157586.2A CN105024074B (en) | 2014-04-18 | 2014-04-18 | A kind of preparation method using resin as the lithium ion battery negative material of raw material |
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| CN105024074A true CN105024074A (en) | 2015-11-04 |
| CN105024074B CN105024074B (en) | 2017-11-07 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004179015A (en) * | 2002-11-28 | 2004-06-24 | Nippon Carbon Co Ltd | Anode material for lithium-ion secondary battery, its manufacturing method and battery using this |
| 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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2014
- 2014-04-18 CN CN201410157586.2A patent/CN105024074B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004179015A (en) * | 2002-11-28 | 2004-06-24 | Nippon Carbon Co Ltd | Anode material for lithium-ion secondary battery, its manufacturing method and battery using this |
| 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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| CN105024074B (en) | 2017-11-07 |
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