CN107039654A - A kind of preparation method of high power capacity long circulating artificial plumbago negative pole material - Google Patents
A kind of preparation method of high power capacity long circulating artificial plumbago negative pole material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000010439 graphite Substances 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 240000003936 Plumbago auriculata Species 0.000 title abstract 2
- 238000005087 graphitization Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000012937 correction Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims description 28
- 239000002006 petroleum coke Substances 0.000 claims description 19
- 241000209456 Plumbago Species 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 239000006253 pitch coke Substances 0.000 claims description 13
- 239000011280 coal tar Substances 0.000 claims description 12
- 239000010426 asphalt Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 239000011269 tar Substances 0.000 claims description 11
- 239000003208 petroleum Substances 0.000 claims description 10
- 239000011294 coal tar pitch Substances 0.000 claims description 7
- 238000005242 forging Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 2
- 239000011334 petroleum pitch coke Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 26
- 239000010406 cathode material Substances 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 15
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011295 pitch Substances 0.000 description 5
- 239000003610 charcoal Substances 0.000 description 4
- 238000005253 cladding Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000007770 graphite material Substances 0.000 description 3
- 230000002427 irreversible effect Effects 0.000 description 3
- 239000002931 mesocarbon microbead Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to graphite cathode material technical field, specifically a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material, it is characterised in that it includes following preparation process：(1) raw material Shape correction；(2) mix for the first time；(3) it is heat-treated；(4) graphitization；(5) second of mixing；(6) charing heat treatment.Compared with the existing technology, process is simple by the present invention, and preparation method yield is high, which employs methods such as shaping, liquid phase coating modification, graphitizations, and obtained product efficiency for charge-discharge and resistance to PC performances are high；The tap density of product is effectively improved, the high comprehensive performance for the button cell being made of the negative material.
Description
Technical field
The present invention relates to graphite cathode material technical field, specifically a kind of high power capacity long circulating artificial plumbago negative pole
The preparation method of material.
Background technology
Lithium ion battery negative material has two kinds of Delanium and native graphite based on Carbon Materials, mainly.Delanium
There are MCMB such as CMS and MCMB, also intermediate-phase carbon fiber MCF and graphous graphite powder.First two Delanium be by
Widely used negative material, has the advantages that particle shape is good, irreversible capacity loss is low, cycle life is stable, but also deposit
In the deficiency that production cost is high, discharge capacity is low, the discharge capacity of MCMB is general in 320mAh/g or so.Irregularly
Form graphous graphite powder is not suitable for using directly as negative material due to haveing the shortcomings that tap density is low, specific surface area is high.
Natural graphite starting material cost is low, and its higher degree of graphitization makes it have higher embedding lithium ability, but the native graphite of sheet
The shortcoming that tap density is low, specific surface area is high is equally existed, is not suitable for using directly as negative material.Not by modification
Irreversible capacity loss is very high first for natural graphite negative electrode material, can typically reach 10%, is total in circulation due to occurring solvent
It is embedded, cause the problems such as capacity attenuation is fast.Although the native graphite electrical property by roundingization and surface treatment has clear improvement,
But still have the shortcomings that capacitance fall-off is very fast and production cost is higher.
For a long time, the capacitance for improving Delanium, the irreversible capacity loss first for reducing native graphite improve it
Cycle performance is always the emphasis of research and development.Various producers have been developed for artificial plumbago negative pole material
Method, these methods are mostly that, from material asphalt, process route is longer, and production cost is higher.
Japan Patent JP10294111 is carried out being melted place after low temperature cladding, cladding with pitch to graphite Carbon Materials
Reason and Light comminution, this method, which is difficult to, is evenly coated and keeps shape.Japan Patent JP11246209 be by graphite and
Hard charcoal particle impregnates at a temperature of 10~300 DEG C in pitch or tar, then carries out solvent separation and heat treatment, this method
It is difficult to form the bitumen layer with certain thickness high polymeric in graphite and hard charcoal surface, for carrying for graphite-structure stability
Height is limited.Japan Patent JP2000357506, to charcoal or graphite powder cladding cracking graphite, cracking graphite come from hydrocarbon and
Its mixture.Japan Patent JP2000243398 is that the atmosphere produced using asphalt pyrolysis is surface-treated to graphite material,
This method is unlikely, and make the to be modified form of material is greatly improved, thus is restricted the raising of electrical property.Day
This patent JP2002042816 is coated with CVD using aromatic hydrocarbons as raw material or coated with pitch phenolic resin, this with
JP2000182617 and JP2000283398 have similarity in effect.Japan Patent JP2000182617 is to use natural stone
Ink etc. and pitch or resin or its mixture Co carbonization, this method can reduce graphite material specific surface area, but in cladding effect
It is difficult to reach preferable control on fruit.Japan Patent JP2003100292, graphite is mixed with pitch, at a temperature of 600~800 DEG C
It is heat-treated.And JP200397357 is to mix graphite with heavy oil, then carry out delayed coking and heat treatment.Both the above is done
Method will typically have a pulverising step, and covered effect can be influenceed to a certain extent.
The content of the invention
The invention aims to overcome, existing asphalt modification graphite cathode material volumetric efficiency is low, be electrolysed containing PC
The defect that liquid discharge process stability is poor, capacity attenuation is fast, is covered resistance to using charcoal bag after even in liquid phase coating modification, high temperature graphitization
There is provided a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material for the technique of PC performances.
To achieve the above object, a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material, its feature are designed
It is, it includes following preparation process：
(1) raw material Shape correction：By petroleum coke or pitch coke Shape correction into equal particle diameter D50 be 6~28 μm, tap density
For 1.10~1.30g/cm3Material powder；
(2) mix for the first time：Material powder is mixed into obtain compound with coal tar or petroleum tar in machine is merged；It is described
The mass ratio of material powder and the coal tar or petroleum tar is 50: 50~90: 10；
(3) it is heat-treated：Compound carries out being heat-treated 12~24 hours under inert gas shielding with 300~700 DEG C；
(4) graphitization：Compound after heat treatment is with 2800~3200 DEG C, graphitization 20~60 hours；
(5) second of mixing：Compound after graphitization again with asphalt or coal tar pitch in mass ratio 80: 20~99: 1
Mixed；
(6) charing heat treatment：Under inert gas shielding, charing heat treatment 10~50 hours is carried out with 800~2000 DEG C,
D50 particle diameters are made at 8~30 μm, tap density is in 1.20g/cm3High power capacity long circulating artificial plumbago negative pole material above.
Petroleum coke described in step (1) or pitch coke are pitch coke before petroleum coke before forging or forging.
The mass ratio of described material powder and coal tar or petroleum tar is 80: 20~90: 10.
The temperature of described heat treatment is 400~600 DEG C.
The performance parameter of high power capacity long circulating artificial plumbago negative pole material obtained by preparation is：D50 particle diameters are 8~30 μm,
Tap density >=1.20g/cm3, discharge capacity >=365mAh/g of the button cell being made, the button cell being made puts first
Electrical efficiency >=95%, the discharge capacity (50%PC) >=80% for the button cell being made.
Compared with the existing technology, process is simple by the present invention, and preparation method yield is high, changes which employs shaping, liquid phase coating
Property the method such as processing, graphitization, obtained product efficiency for charge-discharge and resistance to PC performances are high；It is effectively improved the vibration density of product
Degree, the high comprehensive performance for the button cell being made of the negative material.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of prepared artificial plumbago negative pole material in the embodiment of the present invention 2.
Embodiment
Below in conjunction with embodiment, the preparation process to the present invention is further described through.But not therefore by the present invention
It is limited among described scope of embodiments.
Petroleum coke produces for Fushun second branch factory of oil.
Pitch coke produces for Shanghai Baosteel Chemical Co., Ltd.
Asphalt is the MQ-260 asphalt of the bright reinforcing work Materials Co., Ltd production in Dalian.
Coal tar pitch is the modified coal tar pitch that Henan Bo Hai Chemical Co., Ltd.s produce.
Embodiment 1
1st, by petroleum coke Shape correction into D50 particle diameters be 17.0 μm of powder；
2nd, petroleum coke powder mixes to obtain compound, petroleum coke powder with coal tar in machine is merged：Quality is than coal tar
Mass ratio is 90: 10；
3rd, compound is under inert gas shielding, in rotary retort type electric resistance furnace, is heat-treated 18 hours with 500 DEG C；
4th, compound after being heat-treated was with 3000 DEG C of graphitizations 48 hours；
5th, the compound after graphitization is mixed with asphalt in mass ratio 90: 10；
6th, under inert gas shielding, in roller kilns, charing heat treatment 30 hours is carried out with 1400 DEG C, lithium ion is made
Battery graphite cathode material.The button cell capacity that the graphite cathode material is made is 365.9mAh/g, and efficiency is first
95.8%, discharge capacity (50%PC) is 82.8%.
Embodiment 2
1st, it is 17.0 μm of pitch coke powder by pitch coke Shape correction D50 particle diameters
2nd, pitch coke powder mixes to obtain compound, pitch coke powder with petroleum tar in machine is merged：The matter of petroleum tar
Measure ratio 90: 10；
3rd, compound is under inert gas shielding, in rotary retort type electric resistance furnace, is heat-treated 12 hours with 700 DEG C；
4th, compound after being heat-treated was with 2800 DEG C of graphitizations 48 hours；
5th, the compound after graphitization is mixed with asphalt in mass ratio 90: 10；
6th, under inert gas shielding, in roller kilns, charing heat treatment 30 hours, obtained conduct are carried out with 1400 DEG C
The high power capacity long circulating artificial plumbago negative pole material of lithium ion battery negative material, the pattern enlarged drawing ginseng of the graphite cathode material
See Fig. 1.The button cell capacity that the graphite cathode material is made is 366.7mAh/g, and efficiency is 95.8%, discharge capacity first
(50%PC) is 84.0%.
Embodiment 3
1st, it is 28.0 μm of pitch coke powder by pitch coke Shape correction D50 particle diameters；
2nd, pitch coke powder mixes to obtain compound, pitch coke powder with petroleum tar in machine is merged：The matter of petroleum tar
Measure ratio 70: 30；
3rd, compound is under inert gas shielding, in rotary retort type electric resistance furnace, is heat-treated 24 hours with 300 DEG C；
4th, compound after being heat-treated was with 3200 DEG C of graphitizations 60 hours；
5th, the compound after graphitization is mixed with coal tar pitch in mass ratio 99: 1；
6th, under inert gas shielding, in roller kilns, charing heat treatment 10 hours is carried out with 1400 DEG C, lithium ion is made
Battery graphite cathode material.The button cell capacity that the graphite cathode material is made is 365.2mAh/g, and efficiency is first
95.3%, discharge capacity (50%PC) is 82.1%.
Embodiment 4
1st, it is 6.0 μm of petroleum coke powder by petroleum coke Shape correction D50 particle diameters；
2nd, petroleum coke powder mixes to obtain compound, petroleum coke powder with coal tar in machine is merged：The mass ratio of coal tar
50∶50；
3rd, compound is under inert gas shielding, in rotary retort type electric resistance furnace, is heat-treated 18 hours with 400 DEG C；
4th, compound after being heat-treated was with 3000 DEG C of graphitizations 20 hours；
5th, the compound after graphitization is mixed with asphalt in mass ratio 80: 20；
6th, under inert gas shielding, in roller kilns, charing heat treatment 50 hours is carried out with 800 DEG C, lithium ion is made
Battery graphite cathode material.The button cell capacity that the graphite cathode material is made is 365.5mAh/g, and efficiency is first
95.2%, discharge capacity (50%PC) is 83.2%.
Embodiment 5
1st, it is 17.0 μm of petroleum coke powders by petroleum coke Shape correction D50 particle diameters
2nd, petroleum coke powder mixes to obtain compound, petroleum coke powder with coal tar in machine is merged：The mass ratio of coal tar
80: 20,
3rd, compound is under inert gas shielding, in rotary retort type electric resistance furnace, is heat-treated 18 hours with 600 DEG C；
4th, compound after being heat-treated was with 3000 DEG C of graphitizations 40 hours；
5th, the compound after graphitization is mixed with coal tar pitch in mass ratio 90: 10；
6th, under inert gas shielding, in roller kilns, charing heat treatment 30 hours is carried out with 1400 DEG C, lithium ion is made
Battery graphite cathode material.Its button cell capacity is 367.2mAh/g, and efficiency is 95.8%, discharge capacity (50%PC) first
For 83.0%.
The performance parameter of high power capacity long circulating artificial plumbago negative pole material prepared by the present invention, referring to table 1：
Table 1
Comparative example 1
1st, it is 17.0 μm of powder by petroleum coke Shape correction D50；
2nd, it is heat-treated 48 hours with 3000 DEG C of graphitizations；
3rd, mixed again with coal tar pitch in mass ratio 80: 20；
4th, under inert gas shielding, in roller kilns, charing heat treatment 30 hours is carried out with 1400 DEG C, lithium ion is made
Battery graphite cathode material.Its button cell capacity is 354.1mAh/g, and efficiency is 91.2%, discharge capacity (30%PC) first
For 70.8%.
Embodiment effect
(1) graphite cathode material in embodiment 1~5 and comparative example 1 is subjected to particle diameter, tap density etc. respectively
Item index test, as a result referring to table 2.Instrument title and model used in test：Particle diameter, laser fineness gage
MS2000；Tap density, tap density meter FZS4-4B.
(2) graphite cathode material in embodiment 1~5 and comparative example 1 is entered using button cell method of testing
The test of row discharge capacity and first efficiency, as a result referring to table 2.
The present invention use button cell method of testing for：Conductive black is added in the carboxyl methyl cellulose aqueous solution,
Then graphite cathode material is added, styrene butadiene rubber sbr is eventually adding, stirred, is uniformly coated in slurry on coating machine
Pole piece is made on copper foil.The pole piece coated is put into temperature to be dried in vacuo 4 hours in 110 DEG C of vacuum drying chambers, pole piece is taken out
Rolled on roll squeezer, it is standby.Simulated battery is assemblied in the German Braun glove box of applying argon gas and carried out, and electrolyte is
1MLiPF6EC: DEC: DMC=1: 1: 1 (volume ratio), metal lithium sheet is to electrode.Volume test is in U.S.'s ArbinBT2000 types
Carried out on cell tester, charging/discharging voltage scope is 0.005 to 2.0V, and charge-discharge velocity is 0.1C.
Table 2：The performance parameter of embodiment and comparative example
The discharge capacity and efficiency for charge-discharge that can be seen that from the data in table 2 in comparative example 1 are low, tap density
Only 0.98g/cm3, tap density is low, and discharge capacity (30%PC) only reaches 70.8%；The stone prepared using the inventive method
Black negative material：Tap density is more than 1.20g/cm3, discharge capacity is more than 365mAh/g, and efficiency for charge-discharge is more than 95%, electric discharge
Capacity (50%PC) has extended cycle life more than 80%, and 1C/1C discharge and recharges were up to more than 2000 weeks.
Claims (5)
1. a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material, it is characterised in that it includes following prepare and walked
Suddenly：
(1) raw material Shape correction：By petroleum coke or pitch coke Shape correction into equal particle diameter D50 be 6~28 μm, tap density be
1.10~1.30g/cm3Material powder；
(2) mix for the first time：Material powder is mixed into obtain compound with coal tar or petroleum tar in machine is merged；The raw material
The mass ratio of powder and the coal tar or petroleum tar is 50: 50~90: 10；
(3) it is heat-treated：Compound carries out being heat-treated 12~24 hours under inert gas shielding with 300~700 DEG C；
(4) graphitization：Compound after heat treatment is with 2800~3200 DEG C, graphitization 20~60 hours；
(5) second of mixing：Compound after graphitization is carried out with asphalt or coal tar pitch in mass ratio 80: 20~99: 1 again
Mixing；
(6) charing heat treatment：Under inert gas shielding, charing heat treatment 10~50 hours is carried out with 800~2000 DEG C, that is, is made
D50 particle diameters are obtained at 8~30 μm, tap density is in 1.20g/cm3High power capacity long circulating artificial plumbago negative pole material above.
2. a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material as claimed in claim 1, it is characterised in that
Petroleum coke described in step (1) or pitch coke are pitch coke before petroleum coke before forging or forging.
3. a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material as claimed in claim 1, it is characterised in that
The mass ratio of described material powder and coal tar or petroleum tar is 80: 20~90: 10.
4. a kind of preparation method of high power capacity long circulating artificial plumbago negative pole material as claimed in claim 1, it is characterised in that
The temperature of described heat treatment is 400~600 DEG C.
5. a kind of such as preparation method of high power capacity long circulating artificial plumbago negative pole material according to any one of claims 1 to 4,
Characterized in that, the performance parameter of the high power capacity long circulating artificial plumbago negative pole material obtained by preparing is：D50 particle diameters are 8~30 μ
M, tap density >=1.20g/cm3, the discharge capacity >=365mAh/g for the button cell being made, the button cell being made is first
Discharging efficiency >=95%, the discharge capacity (50%PC) >=80% for the button cell being made.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109052390A (en) * | 2018-08-17 | 2018-12-21 | 东莞市凯金新能源科技股份有限公司 | A kind of fusion method and its material improving modified graphite presoma particle size range |
| CN110289417A (en) * | 2019-06-26 | 2019-09-27 | 鞍山赛欧新材料科技有限公司 | A kind of artificial graphite cathode material for lithium ion batteries preparation 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 |
| CN112289986A (en) * | 2020-09-28 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Preparation method of high-rate quick-charging graphite negative electrode material |
| CN112490443A (en) * | 2019-09-12 | 2021-03-12 | 宁波杉杉新材料科技有限公司 | Liquid-phase-coated graphite negative electrode material and preparation method thereof |
| CN112652746A (en) * | 2020-12-02 | 2021-04-13 | 上海杉杉科技有限公司 | Composite negative electrode material for lithium ion battery, preparation method and battery |
| CN112670503A (en) * | 2020-04-02 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Surface modified pyrolytic carbon material, battery and preparation method and application thereof |
| CN112670459A (en) * | 2019-12-09 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Graphite negative electrode material and preparation and application thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08339805A (en) * | 1995-06-13 | 1996-12-24 | Mitsubishi Chem Corp | Manufacture of nonaqueous solvent secondary battery electrode material |
| JP2004127913A (en) * | 2002-07-31 | 2004-04-22 | Matsushita Electric Ind Co Ltd | Lithium secondary battery |
| KR20090107740A (en) * | 2008-04-10 | 2009-10-14 | 엘에스엠트론 주식회사 | Negative active material used for secondary battery, electrode of secondary battery and secondary battery including the same |
| CN104659365A (en) * | 2014-12-30 | 2015-05-27 | 东莞市凯金新能源科技有限公司 | Preparation method of artificial graphite anode material for lithium ion battery |
| CN105428615A (en) * | 2015-11-09 | 2016-03-23 | 大连宏光锂业股份有限公司 | Production method for modified artificial graphite negative electrode material |
| CN106486669A (en) * | 2015-11-17 | 2017-03-08 | 上海杉杉科技有限公司 | A kind of high-discharge-rate lithium ion battery graphite cathode material and preparation method thereof |
| CN106495144A (en) * | 2015-11-17 | 2017-03-15 | 宁波杉杉新材料科技有限公司 | A kind of low bulk long circulating Delanium lithium ion battery negative material |
| CN106505198A (en) * | 2015-09-25 | 2017-03-15 | 宁波杉杉新材料科技有限公司 | A kind of graphite negative material of lithium ion battery and preparation method thereof |
| CN106532044A (en) * | 2015-09-13 | 2017-03-22 | 上海杉杉科技有限公司 | Lithium secondary battery composite graphite and preparation method thereof |
-
2017
- 2017-03-24 CN CN201710186177.9A patent/CN107039654A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08339805A (en) * | 1995-06-13 | 1996-12-24 | Mitsubishi Chem Corp | Manufacture of nonaqueous solvent secondary battery electrode material |
| JP2004127913A (en) * | 2002-07-31 | 2004-04-22 | Matsushita Electric Ind Co Ltd | Lithium secondary battery |
| KR20090107740A (en) * | 2008-04-10 | 2009-10-14 | 엘에스엠트론 주식회사 | Negative active material used for secondary battery, electrode of secondary battery and secondary battery including the same |
| CN104659365A (en) * | 2014-12-30 | 2015-05-27 | 东莞市凯金新能源科技有限公司 | Preparation method of artificial graphite anode material for lithium ion battery |
| CN106532044A (en) * | 2015-09-13 | 2017-03-22 | 上海杉杉科技有限公司 | Lithium secondary battery composite graphite and preparation method thereof |
| CN106505198A (en) * | 2015-09-25 | 2017-03-15 | 宁波杉杉新材料科技有限公司 | A kind of graphite negative material of lithium ion battery and preparation method thereof |
| CN105428615A (en) * | 2015-11-09 | 2016-03-23 | 大连宏光锂业股份有限公司 | Production method for modified artificial graphite negative electrode material |
| CN106486669A (en) * | 2015-11-17 | 2017-03-08 | 上海杉杉科技有限公司 | A kind of high-discharge-rate lithium ion battery graphite cathode material and preparation method thereof |
| CN106495144A (en) * | 2015-11-17 | 2017-03-15 | 宁波杉杉新材料科技有限公司 | A kind of low bulk long circulating Delanium lithium ion battery negative material |
Non-Patent Citations (1)
| Title |
|---|
| 甘雷等: ""沥青基人造石墨/天然石墨球复合炭负极材料的制备与性能"", 《中南大学学报（自然科学版）》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052390A (en) * | 2018-08-17 | 2018-12-21 | 东莞市凯金新能源科技股份有限公司 | A kind of fusion method and its material improving modified graphite presoma particle size range |
| CN110289417A (en) * | 2019-06-26 | 2019-09-27 | 鞍山赛欧新材料科技有限公司 | A kind of artificial graphite cathode material for lithium ion batteries preparation method |
| CN112490443A (en) * | 2019-09-12 | 2021-03-12 | 宁波杉杉新材料科技有限公司 | Liquid-phase-coated graphite negative electrode material and preparation method thereof |
| 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 |
| CN112670459A (en) * | 2019-12-09 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Graphite negative electrode material and preparation and application thereof |
| CN112670503A (en) * | 2020-04-02 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Surface modified pyrolytic carbon material, battery and preparation method and application thereof |
| CN112289986A (en) * | 2020-09-28 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Preparation method of high-rate quick-charging graphite negative electrode material |
| CN112652746A (en) * | 2020-12-02 | 2021-04-13 | 上海杉杉科技有限公司 | Composite negative electrode material for lithium ion battery, preparation method and battery |
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