CN108963260A - A kind of preparation process of lithium battery hard carbon composite negative pole material - Google Patents

A kind of preparation process of lithium battery hard carbon composite negative pole material Download PDF

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Publication number
CN108963260A
CN108963260A CN201810782466.XA CN201810782466A CN108963260A CN 108963260 A CN108963260 A CN 108963260A CN 201810782466 A CN201810782466 A CN 201810782466A CN 108963260 A CN108963260 A CN 108963260A
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China
Prior art keywords
hard carbon
ball
preparation process
negative pole
ratio
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Pending
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CN201810782466.XA
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Chinese (zh)
Inventor
马兴华
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Datong Xincheng New Material Co Ltd
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Datong Xincheng New Material Co Ltd
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Priority to CN201810782466.XA priority Critical patent/CN108963260A/en
Publication of CN108963260A publication Critical patent/CN108963260A/en
Pending legal-status Critical Current

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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
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • 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 invention discloses a kind of preparation processes of lithium battery hard carbon composite negative pole material, include the following steps: S1, raw material;S2, by sucrose base hard carbon powder, carbon nanotube, graphite powder, the ratio than 10-12:2-3:3-4 is taken out according to parts by weight, and it is uniformly mixed, it is then placed in ball mill, using copper ball as abrasive body, and it is heated to 700-900 DEG C of progress ball milling, 30-40 times, Ball-milling Time 10-15h are recycled, mixing fines is obtained;S3, mixing fines, PVDF, acetylene black are taken out and is uniformly mixed than the ratio for 40-50:4-6:2-3 according to parts by weight, be then heated to 160-200 DEG C, and be put into blender and kept for 160-200 DEG C, stir 4-6h;Then methyl pyrrolidone is added to stir evenly, so that mixed material is in thick;S4, the material in a mold by S3 preparation are clipped in the middle by two layers of copper foil, are then placed in moulding press, and the pressure for passing through 60-80MPa is pressed and molded, and obtain green compact;S5, green compact are cut, is then placed in dryer, dried 10-12 hours by 120-150 DEG C of temperature.

Description

A kind of preparation process of lithium battery hard carbon composite negative pole material
Technical field
The present invention relates to a kind of cell negative electrode material manufacturing process, more particularly to a kind of lithium battery hard carbon composite negative pole material The preparation process of material.
Background technique
Cathode refers to current potential in power supply (potential) lower one end.In primary battery, the electrode of oxidation, battery are referred to The left side is write in reaction.It is the pole that electronics flows out in circuit from the point of view of physical angle.And negative electrode material, then refer in battery The raw material of cathode is constituted, negative electrode material common at present has carbon negative pole material, tin base cathode material, lithium-containing transition metal nitride Negative electrode material, alloy type negative material and nanoscale negative electrode material.
And it is most common using graphite prepare, still, the manufacturing process of current battery negative electrode material very it is mature and Diversification, end properties are also relatively high, but the manufacturing process of each producer belongs to confidential state or by patent protection, because This, need the manufacturing field into cell negative electrode material must just design it is a kind of it is completely new, with the distinguishing manufacture of the prior art Technique.
But it is low by the manufacturing process of designed, designed or complex process, yield rate, cost increase is caused, so that enterprise Industry loses competitiveness;Poor product quality, so that enterprise competitiveness is poor.
Therefore, applicant proposes a kind of preparation process of lithium battery hard carbon composite negative pole material, simple process, and cost It is relatively low, but end properties can satisfy current demand.
Summary of the invention
In view of the above drawbacks of the prior art, technical problem to be solved by the invention is to provide a kind of lithium battery hard carbons The preparation process of composite negative pole material.
To achieve the above object, the present invention provides a kind of preparation processes of lithium battery hard carbon composite negative pole material, including Following steps:
S1, raw material, Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black, PVDF, methyl pyrrolidone;
The Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black fineness be 90 mesh or more, purity 99.99%;
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%;
S2, by sucrose base hard carbon powder, carbon nanotube, graphite powder, the ratio than 10-12:2-3:3-4 is taken out according to parts by weight, and It being uniformly mixed, is then placed in ball mill, the copper ball for being 4 millimeters using diameter is then charged with nitrogen and is used as protection gas as abrasive body, And it is heated to 700-900 DEG C of progress ball milling, 30-40 times, Ball-milling Time 10-15h are recycled, mixing fines is obtained;
S3, mixing fines, PVDF, acetylene black are taken out than the ratio for 40-50:4-6:2-3 according to parts by weight and mixed It is even, it is then heated to 160-200 DEG C, and be put into blender and kept for 160-200 DEG C, stirs 4-6h;Then methylpyrrole is added Alkanone stirs evenly, so that mixed material is in thick, it is preferable that the methyl pyrrolidone of addition and the weight for mixing fines Portion rate is 10-12:3-4;
S4, it is laid with one layer of copper foil in a mold, then pours into the S3 material prepared in mold, and repaved at most upper one layer of mold If one layer of copper foil, that is, the S3 material prepared is clipped in the middle with two layers of copper foil, it is then placed in moulding press, passes through 60- The pressure of 80MPa is pressed and molded, and obtains green compact, and green compact thickness is not more than 20 ㎜, and compression ratio is not less than 70%;
S5, green compact are cut, is then placed in dryer, dried 10-12 hours by 120-150 DEG C of temperature, taken out Lithium battery hard carbon composite negative pole material is obtained after cooling.
The beneficial effects of the present invention are: present invention process is simple, and manufacturing cost is relatively low, and end properties are not weaker than in the market Mainstream finished product, even better than import finished product.Therefore, bigger profit margin can be brought for enterprise, improves the competition of enterprise Power.
Specific embodiment
Below with reference to embodiment, the invention will be further described:
Embodiment one
A kind of preparation process of lithium battery hard carbon composite negative pole material, includes the following steps:
S1, raw material, Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black, PVDF, methyl pyrrolidone;
The Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black fineness be 90 mesh or more, purity 99.99%;
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%;
S2, by sucrose base hard carbon powder, carbon nanotube, graphite powder, the ratio than 11:2.5:3.4 is taken out according to parts by weight, and is mixed It closing uniformly, is then placed in ball mill, the copper ball for being 4 millimeters using diameter is then charged with nitrogen as protection gas as abrasive body, and 800 DEG C of progress ball millings are heated to, 35 times, Ball-milling Time 12h are recycled, obtain mixing fines;
S3, mixing fines, PVDF, acetylene black are taken out and is uniformly mixed than the ratio for 45:5:2 according to parts by weight, then 200 DEG C are heated to, and is put into blender and is kept for 200 DEG C, stirs 5h;Then methyl pyrrolidone is added to stir evenly, so that Mixed material is in thick;
S4, it is laid with one layer of copper foil in a mold, then pours into the S3 material prepared in mold, and repaved at most upper one layer of mold If one layer of copper foil, is then placed in moulding press, it is pressed and molded by the pressure of 70MPa, obtains green compact, green compact thickness is not more than 20 ㎜, compression ratio are not less than 70%;
S5, green compact are cut, is then placed in dryer, dried 11 hours by 140 DEG C of temperature, be after taking out cooling Obtain lithium battery hard carbon composite negative pole material.
Embodiment two
A kind of preparation process of lithium battery hard carbon composite negative pole material, includes the following steps:
S1, raw material, Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black, PVDF, methyl pyrrolidone;
The Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black fineness be 90 mesh or more, purity 99.99%;
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%;
S2, by sucrose base hard carbon powder, carbon nanotube, graphite powder, the ratio than 12:2:4 is taken out according to parts by weight, and is mixed equal It is even, it is then placed in ball mill, the copper ball for being 4 millimeters using diameter is then charged with nitrogen as protection gas as abrasive body, and heats To 850 DEG C of progress ball millings, 40 times, Ball-milling Time 14h are recycled, obtains mixing fines;
S3, mixing fines, PVDF, acetylene black are taken out and are uniformly mixed than the ratio for 50:4.5:2.5 according to parts by weight, 180 DEG C are then heated to, and is put into blender and is kept for 180 DEG C, stirs 6h;Then methyl pyrrolidone is added to stir evenly, So that mixed material is in thick, it is preferable that the methyl pyrrolidone of addition is 11:3 with the weight fraction ratio for mixing fines;
S4, it is laid with one layer of copper foil in a mold, then pours into the S3 material prepared in mold, and repaved at most upper one layer of mold If one layer of copper foil, that is, the S3 material prepared is clipped in the middle with two layers of copper foil, it is then placed in moulding press, passes through 80MPa Pressure compression molding, obtain green compact, green compact thickness be not more than 20 ㎜, compression ratio be not less than 70%;
S5, green compact are cut, is then placed in dryer, dried 10 hours by 150 DEG C of temperature, be after taking out cooling Obtain lithium battery hard carbon composite negative pole material.
Place is not described in detail by the present invention, is the well-known technique of those skilled in the art.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that those skilled in the art without It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all technologies in the art Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea Technical solution, all should be within the scope of protection determined by the claims.

Claims (4)

1. a kind of preparation process of lithium battery hard carbon composite negative pole material, which comprises the steps of:
S1, raw material, Sodium Polyacrylate, sucrose base hard carbon powder, carbon nanotube, graphite powder, acetylene black, PVDF, methyl pyrrolidone;
S2, by sucrose base hard carbon powder, carbon nanotube, graphite powder, the ratio than 10-12:2-3:3-4 is taken out according to parts by weight, and It being uniformly mixed, is then placed in ball mill, the copper ball for being 4 millimeters using diameter is then charged with nitrogen and is used as protection gas as abrasive body, And it is heated to 700-900 DEG C of progress ball milling, 30-40 times, Ball-milling Time 10-15h are recycled, mixing fines is obtained;
S3, mixing fines, PVDF, acetylene black are taken out than the ratio for 40-50:4-6:2-3 according to parts by weight and mixed It is even, it is then heated to 160-200 DEG C, and be put into blender and kept for 160-200 DEG C, stirs 4-6h;Then methylpyrrole is added Alkanone stirs evenly, so that mixed material is in thick;
S4, it is laid with one layer of copper foil in a mold, then pours into the S3 material prepared in mold, and repaved at most upper one layer of mold If one layer of copper foil, is then placed in moulding press, it is pressed and molded by the pressure of 60-80MPa, obtains green compact;
S5, green compact are cut, is then placed in dryer, dried 10-12 hours by 120-150 DEG C of temperature, taken out Lithium battery hard carbon composite negative pole material is obtained after cooling.
2. preparation process as described in claim 1, which is characterized in that in S1, the Sodium Polyacrylate, sucrose base hard carbon Powder, carbon nanotube, graphite powder, acetylene black fineness be 90 mesh more than, purity 99.99%;
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%.
3. preparation process as described in claim 1, which is characterized in that in S4, green compact thickness is not more than 20 ㎜, and compression ratio is not low In 70%.
4. preparation process as described in claim 1, which is characterized in that in S3, the methyl pyrrolidone of addition with mix fines Weight fraction ratio be 10-12:3-4.
CN201810782466.XA 2018-07-17 2018-07-17 A kind of preparation process of lithium battery hard carbon composite negative pole material Pending CN108963260A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007126257A1 (en) * 2006-05-01 2007-11-08 Lg Chem, Ltd. Lithium secondary battery of improved low-temperature power property
CN101399368A (en) * 2007-09-24 2009-04-01 董兴国 Electric core used for secondary lithium battery and preparation
CN102593524A (en) * 2012-03-01 2012-07-18 广州市云通磁电有限公司 Manufacturing method of orthohexagonal lithium ion battery cell
CN103151494A (en) * 2012-07-09 2013-06-12 深圳市海太阳实业有限公司 Preparation method of battery pole piece, the battery pole piece and battery
CN105355867A (en) * 2015-10-21 2016-02-24 山东玉皇新能源科技有限公司 Hard carbon negative electrode material for high-performance lithium ion power battery, and preparation method and application of hard carbon negative electrode material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007126257A1 (en) * 2006-05-01 2007-11-08 Lg Chem, Ltd. Lithium secondary battery of improved low-temperature power property
CN101399368A (en) * 2007-09-24 2009-04-01 董兴国 Electric core used for secondary lithium battery and preparation
CN102593524A (en) * 2012-03-01 2012-07-18 广州市云通磁电有限公司 Manufacturing method of orthohexagonal lithium ion battery cell
CN103151494A (en) * 2012-07-09 2013-06-12 深圳市海太阳实业有限公司 Preparation method of battery pole piece, the battery pole piece and battery
CN105355867A (en) * 2015-10-21 2016-02-24 山东玉皇新能源科技有限公司 Hard carbon negative electrode material for high-performance lithium ion power battery, and preparation method and application of hard carbon negative electrode material

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Application publication date: 20181207