CN107507979A - A kind of preparation method of high jolt ramming artificial plumbago negative pole material - Google Patents
A kind of preparation method of high jolt ramming artificial plumbago negative pole material Download PDFInfo
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- CN107507979A CN107507979A CN201610412498.1A CN201610412498A CN107507979A CN 107507979 A CN107507979 A CN 107507979A CN 201610412498 A CN201610412498 A CN 201610412498A CN 107507979 A CN107507979 A CN 107507979A
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- needle coke
- fine powder
- fusion
- jolt ramming
- negative pole
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- 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
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- 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
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The present invention relates to graphite material technical field, specifically a kind of preparation method of high jolt ramming artificial plumbago negative pole material, it is characterised in that use following preparation process：By needle coke through pulverization process into needle coke fine powder；Needle coke fine powder is obtained into needle coke fine powder shaping thing through spherical graphite trimmer Shape correction；By covering pulverization process to D50：0.1~100.0 μm obtains covering powder；Fusion treatment, obtain needle coke fusions；Graphitization processing；After reaction product after graphitization processing is cooled to room temperature, then screening process is carried out, obtain finished product.Compared with the existing technology, needle coke passes through shaping, fusion, graphitization and screening process to the present invention, and prepared Delanium has the characteristics that high jolt ramming, high discharge capacity, high efficiency first, low circulation expansion, long cycle life.
Description
Technical field
The present invention relates to graphite material technical field, specifically a kind of high jolt ramming artificial plumbago negative pole material
Preparation method.
Background technology
Into 21 century, petroleum reserves increasingly depleted on the earth, motor vehicle exhaust emission is to greenhouse caused by environment
Effect getting worse.In recent years, the electric automobile (EV) of motor driving, engine and motor combination
Hybrid electric automobile (HEV) due to can effectively utilize small volume, light weight lithium ion battery, form
To research and develop focus.Wherein, the characteristics of hybrid electric automobile is even more economical and low oil consumption.
Artificial plumbago negative pole material is due to its excellent dynamic performance, low expansion, the spy such as have extended cycle life
Point is always in lithium ion battery negative material in occupation of critical role, the especially electrokinetic cell in electric automobile
Upper extensive use.
However, capacity and degree of graphitization, the shape of particle, granular size, particle diameter due to Delanium
Be designed with much relations, and have that tap density is low to cause processing characteristics in lithium battery process always
The problem of poor.Therefore, a kind of regular particles are designed, granular size is moderate, particle diameter distribution reasonably high jolt ramming
Artificial plumbago negative pole material is always the emphasis studied.
Japan Patent JP2002-373656 will be 250 with height-oriented powdered graphite and softening point~
400 DEG C of mesophase pitch melting mixing, then crush, be classified, calcining, graphitization and compound is made,
This negative material combines the high power capacity of graphite and the excellent specific property of mesophase pitch, shows high efficiency
And tap density.
In addition, the poor processability of current many Delaniums, its main reason is exactly the jolt ramming of material
Density is low.Therefore the processing characteristics of material can also be improved by improving the tap density of Delanium, make lithium battery
Manufacturing process it is more convenient, reduce the requirement to equipment, reduce production cost.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of regular particles, granular size is moderate,
The rational high jolt ramming artificial plumbago negative pole material of particle diameter distribution.
To achieve the above object, a kind of preparation method of high jolt ramming artificial plumbago negative pole material, its feature are designed
It is to use following preparation process：
(1) by needle coke through pulverization process into D50 be 2~30 microns of needle coke fine powder；
(2) it is 25~45Hz in frequency through spherical graphite trimmer by needle coke fine powder, Shape correction 20~
Obtain needle coke fine powder shaping thing within 60 minutes；
(3) by covering pulverization process to D50：0.1~100.0 μm obtains covering powder；
(4) it is alternately added needle coke fine powder shaping thing in fusion machine while stirring and covering powder is carried out
Fusion treatment, obtains needle coke fusions, and fusion machine rotating speed is 20~350r/min, time of fusion
For 1~30min, the weight ratio of needle coke and covering is 1: 2~100；
(5) by needle coke fusions under a shielding gas, it is with 2000~3200 DEG C of temperature, heating rate
5 DEG C/min, 1~20h of graphitization processing；
(6) after the reaction product after graphitization processing is cooled to room temperature, then screening process is carried out, obtains finished product；
Described needle coke using coal-based needle coke green coke or coal-based needle coke be ripe burnt or oil system Raw needle coke or
At least one of ripe Jiao of oil system needle coke；
Described covering is using any of asphalt, coal tar pitch, phenolic resin or epoxy resin；
Described protective gas is using at least one of high pure nitrogen, high-purity argon gas.
The D50 particle diameters of described finished product are 16~16.5 microns, tap density is 1.02~1.12g/cm3、
Specific surface area is 1.2~1.7m2/ g, ash content≤0.03%, discharge capacity are up to 362mAh/g, efficiency reaches first
More than 92%.
One during described pulverization process is airslide disintegrating mill crushing, mechanical crusher crushes, roll mill crushes
Kind is a variety of.
Described fusion treatment merges for solid phase.
Compared with the existing technology, needle coke passes through shaping, fusion, graphitization and screening process, institute to the present invention
The Delanium of preparation has high jolt ramming, high discharge capacity, high efficiency first, low circulation expansion, long
The features such as cycle life.
Brief description of the drawings
Fig. 1 is that the material for preparing makes and helped after battery in 500 weeks capacity of 1C charge and discharges in the embodiment of the present invention 4
The chart of conservation rate.
Fig. 2 is the SEM stereoscan photographs of the material prepared in the embodiment of the present invention 4.
Embodiment
Below in conjunction with embodiment, technical scheme is further described through.
Phenolic resin, epoxy resin are not required specifically in the present invention, because in follow-up preparation process
In be all to become carbon.
Embodiment 1
It is that needle coke passes through air-flow crushing into the fine powder that D50 particle diameters are 16.0 μm by oil, by needle coke fine powder
By spherical trimmer, the frequency for adjusting spherical trimmer is 45Hz, and Shape correction obtains needle coke in 20 minutes
Fine powder shaping thing.
Asphalt as covering is crushed to the asphalt powder that D50 particle diameters are 4 μm.
Then needle coke fine powder shaping thing and asphalt powder are alternately added while stirring into fusion machine, are melted
Conjunction is handled, and needle coke is 1: 10 with asphalt powder weight ratio, and fusion machine rotating speed is 50r/min, and time of fusion is
4min。
After fusion terminates, under the protection of nitrogen, and graphitization processing 300 minutes at a temperature of 2700 DEG C,
The reaction product after graphitization processing is cooled to room temperature afterwards, and sieved, lithium ion battery stone is made
Black negative material.Half-cell capacity 362.5mAh/g, first efficiency 93.8%.
Embodiment 2
It is that needle coke passes through air-flow crushing into the fine powder that D50 is 13 μm by oil.
By needle coke fine powder by spherical trimmer, it is 45Hz to adjust spherical shaping unit frequency, Shape correction 30
Minute obtains needle coke fine powder shaping thing.
Asphalt as covering is crushed to D50 particle diameters up to 10 μm.
Then needle coke fine powder shaping thing and asphalt powder are alternately added while stirring into fusion machine, are melted
Conjunction is handled.Needle coke and asphalt powder weight ratio are 1: 20, and fusion machine rotating speed is 100r/min, time of fusion
For 15min.
After fusion terminates, under the protection of nitrogen, and graphitization processing 300 minutes at a temperature of 2800 DEG C,
Reaction product is cooled to room temperature afterwards, and sieved, graphite negative material of lithium ion battery is made.Half
Battery capacity 365.5mAh/g, first efficiency 92.5%.
Embodiment 3
Coal-based needle coke is passed through needle coke fine powder into the fine powder that D50 is 16.0 μm by air-flow crushing
Trimmer, adjustment main frame frequency are 45Hz, and Shape correction obtains shaping thing in 40 minutes.Phenolic resin is crushed to
100 μm, native graphite shaping thing and phenolic resin are alternately added under stirring into fusion machine, carries out fusion treatment.
Needle coke is 1: 20 with phenolic resin weight ratio, and fusion machine rotating speed is 200r/min, time of fusion 30min.
After fusion terminates, under the protection of nitrogen, and graphitization processing 300 minutes at a temperature of 2900 DEG C,
Reaction product is cooled to room temperature afterwards, and sieved, graphite negative material of lithium ion battery is made.Half
Battery capacity 366.1mAh/g, first efficiency 93.2%.
Embodiment 4
It is that needle coke passes through air-flow crushing into the fine powder that D50 is 16.0 μm by oil, needle coke fine powder is passed through
Trimmer, adjustment main frame frequency are 50Hz, and Shape correction obtains shaping thing in 60 minutes.Asphalt is crushed to
D50 particle diameters are 2 μm, and native graphite shaping thing and asphalt powder are alternately added under stirring into fusion machine, is entered
Row fusion treatment.Needle coke is 1: 20 with asphalt powder weight ratio, and fusion machine rotating speed is 200r/min, fusion
Time is 10min.
After fusion terminates, under the protection of nitrogen, and graphitization processing 300 minutes at a temperature of 3000 DEG C,
Reaction product is cooled to room temperature afterwards, and sieved, graphite negative material of lithium ion battery is made.Half
Battery capacity 364.9mAh/g, first efficiency 93.7%.
Embodiment 5
It is that needle coke passes through air-flow crushing into the fine powder that D50 is 16.0 μm by oil, needle coke fine powder is passed through
Trimmer, adjustment main frame frequency are 50Hz, and Shape correction obtains shaping thing in 60 minutes.Asphalt is crushed to
D50 particle diameters are 10 μm, and native graphite shaping thing and asphalt powder are alternately added under stirring into fusion machine, is entered
Row fusion treatment.Needle coke is 1: 50 with asphalt powder weight ratio, and fusion machine rotating speed is 200r/min, fusion
Time is 3min.
After fusion terminates, under the protection of nitrogen, and graphitization processing 300 minutes at a temperature of 3100 DEG C,
Reaction product is cooled to room temperature afterwards, and sieved, graphite negative material of lithium ion battery is made.Half
Battery capacity 366.2mAh/g, first efficiency 94.1%.
Embodiment 6
Coal-based needle coke is passed through needle coke fine powder into the fine powder that D50 is 16.0 μm by air-flow crushing
Trimmer, adjustment main frame frequency are 50Hz, and Shape correction obtains shaping thing in 60 minutes.Asphalt is crushed to
D50 particle diameters are 2 μm, and native graphite shaping thing and asphalt powder are alternately added under stirring into fusion machine, is entered
Row fusion treatment.Needle coke is 1: 20 with asphalt powder weight ratio, and fusion machine rotating speed is 200r/min, fusion
Time is 10min.
After fusion terminates, under the protection of nitrogen, and graphitization processing 300 minutes at a temperature of 3200 DEG C,
Reaction product is cooled to room temperature afterwards, and sieved, graphite negative material of lithium ion battery is made.Half
Battery capacity 365.8mAh/g, first efficiency 94.3%.
Embodiment 6
Coal-based needle coke is passed through needle coke fine powder into the fine powder that D50 is 30.0 μm by air-flow crushing
Trimmer, adjustment main frame frequency are 50Hz, and Shape correction obtains shaping thing in 60 minutes.Epoxy resin is crushed to
D50 particle diameters are 7 μm, and native graphite shaping thing and epoxy powder are alternately added under stirring into fusion machine,
Carry out fusion treatment.Needle coke is 1: 20 with epoxy powder weight ratio, and fusion machine rotating speed is 200r/min,
Time of fusion is 10min.
After fusion terminates, under the protection of argon gas, and graphitization processing 300 minutes at a temperature of 3200 DEG C,
Reaction product is cooled to room temperature afterwards, and sieved, graphite negative material of lithium ion battery is made.Half
Battery capacity 368.2mAh/g, first efficiency 94.9%.
It is referring to following table：Using the performance of the product that the present invention prepares and not shaped prepared product
Contrast table.It can be seen that Delanium prepared after raw material are shaped has high jolt ramming, high discharge capacity, height
First the features such as efficiency, low circulation expansion, long cycle life.
Full battery testing method is used in the present invention：It will be prepared in the graphite prepared in the embodiment of the present invention
Graphite make negative pole, positive pole, 1M-LiPF6EC: DMC: EMC=1: 1: 1 (volume ratio) are made with cobalt acid lithium
Solution makees electrolyte assembling and helps battery, and the graphite that testing example 4 is prepared fills after being applied to battery in 1C
500 weeks capability retentions are put, referring to Fig. 1 and Fig. 2, it is seen that there is the graphite that the present invention prepares high electric discharge to hold
Amount.
Claims (4)
1. a kind of preparation method of high jolt ramming artificial plumbago negative pole material, it is characterised in that walked using following prepare
Suddenly：
(1) by needle coke through pulverization process into D50 be 2~30 microns of needle coke fine powder；
(2) it is 25~45Hz in frequency through spherical graphite trimmer by needle coke fine powder, Shape correction 20~
Obtain needle coke fine powder shaping thing within 60 minutes；
(3) by covering pulverization process to D50：0.1~100.0 μm obtains covering powder；
(4) it is alternately added needle coke fine powder shaping thing in fusion machine while stirring and covering powder is carried out
Fusion treatment, obtains needle coke fusions, and fusion machine rotating speed is 20~350r/min, time of fusion
For 1~30min, the weight ratio of needle coke and covering is 1: 2~100；
(5) by needle coke fusions under a shielding gas, it is with 2000~3200 DEG C of temperature, heating rate
5 DEG C/min, 1~20h of graphitization processing；
(6) after the reaction product after graphitization processing is cooled to room temperature, then screening process is carried out, obtains finished product；
Described needle coke is using the ripe burnt or oil system needle coke of coal-based needle coke green coke or coal-based needle coke
At least one of green coke or ripe Jiao of oil system needle coke；
Described covering uses any in asphalt, coal tar pitch, phenolic resin or epoxy resin
Kind；
Described protective gas is using at least one of high pure nitrogen, high-purity argon gas.
2. a kind of preparation method of high jolt ramming artificial plumbago negative pole material as claimed in claim 1, it is special
Sign is：The D50 particle diameters of described finished product are 16~16.5 microns, tap density be 1.02~
1.12g/cm3, specific surface area be 1.2~1.7m2/ g, ash content≤0.03%, discharge capacity reach
362mAh/g, first efficiency are up to more than 92%.
3. a kind of preparation method of high jolt ramming artificial plumbago negative pole material as claimed in claim 1, it is special
Sign is：Described pulverization process is that airslide disintegrating mill crushes, mechanical crusher crushes, roll-in
Be milled it is broken in one or more.
4. a kind of preparation method of high jolt ramming artificial plumbago negative pole material as claimed in claim 1, it is special
Sign is：Described fusion treatment merges for solid phase.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328613A (en) * | 2017-12-15 | 2018-07-27 | 大同新成新材料股份有限公司 | A kind of method and negative material producing graphite cathode material using needle coke |
| CN108807995A (en) * | 2018-08-03 | 2018-11-13 | 安徽科达洁能新材料有限公司 | A kind of lithium ion battery graphite cathode material and preparation method thereof |
| CN109273713A (en) * | 2018-08-22 | 2019-01-25 | 广东东岛新能源股份有限公司 | A kind of power battery cathode shaping char particle and preparation method thereof |
| CN109473678A (en) * | 2018-12-18 | 2019-03-15 | 潍坊汇成新材料科技有限公司 | A kind of method of the secondary cladding process production lithium ion battery negative material of pitch |
| CN110156005A (en) * | 2019-06-13 | 2019-08-23 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of the graphite cathode material of fast charge lithium ion battery |
| CN110212186A (en) * | 2019-06-13 | 2019-09-06 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of high multiplying power lithium ion battery graphite cathode material |
| CN110718690A (en) * | 2018-07-12 | 2020-01-21 | 宝武炭材料科技有限公司 | Preparation method of battery negative electrode material based on needle coke green coke and calcined coke |
| CN111362259A (en) * | 2018-12-25 | 2020-07-03 | 中信国安盟固利动力科技有限公司 | Limit low specific surface area lithium ion battery negative electrode material and preparation method thereof |
| CN112018386A (en) * | 2019-05-31 | 2020-12-01 | 宁波杉杉新材料科技有限公司 | Artificial graphite material, composite material, preparation method of composite material and lithium ion secondary battery |
| CN114538434A (en) * | 2022-03-31 | 2022-05-27 | 中国神华煤制油化工有限公司 | Graphite negative electrode material and preparation method and application thereof |
| CN115036490A (en) * | 2022-07-01 | 2022-09-09 | 内蒙古三信科技发展有限公司 | Non-charring negative electrode material with low temperature resistance and preparation method thereof |
| CN115924905A (en) * | 2022-12-28 | 2023-04-07 | 广东众大智能科技有限公司 | Asphalt-coated needle coke granularity stabilizing method |
| CN116062744A (en) * | 2022-12-23 | 2023-05-05 | 合肥国轩新材料科技有限公司 | Method for preparing artificial graphite by utilizing tailing fine powder |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328613A (en) * | 2017-12-15 | 2018-07-27 | 大同新成新材料股份有限公司 | A kind of method and negative material producing graphite cathode material using needle coke |
| CN108328613B (en) * | 2017-12-15 | 2019-10-25 | 大同新成新材料股份有限公司 | A kind of method and negative electrode material using needle coke production graphite cathode material |
| CN110718690B (en) * | 2018-07-12 | 2022-07-12 | 宝武碳业科技股份有限公司 | Preparation method of battery negative electrode material based on needle coke green coke and calcined coke |
| CN110718690A (en) * | 2018-07-12 | 2020-01-21 | 宝武炭材料科技有限公司 | Preparation method of battery negative electrode material based on needle coke green coke and calcined coke |
| CN108807995A (en) * | 2018-08-03 | 2018-11-13 | 安徽科达洁能新材料有限公司 | A kind of lithium ion battery graphite cathode material and preparation method thereof |
| CN109273713A (en) * | 2018-08-22 | 2019-01-25 | 广东东岛新能源股份有限公司 | A kind of power battery cathode shaping char particle and preparation method thereof |
| CN109473678A (en) * | 2018-12-18 | 2019-03-15 | 潍坊汇成新材料科技有限公司 | A kind of method of the secondary cladding process production lithium ion battery negative material of pitch |
| CN109473678B (en) * | 2018-12-18 | 2022-01-28 | 潍坊汇成新材料科技有限公司 | Method for producing lithium ion battery cathode material by asphalt secondary coating process |
| CN111362259B (en) * | 2018-12-25 | 2021-12-24 | 荣盛盟固利新能源科技股份有限公司 | Limit low specific surface area lithium ion battery negative electrode material and preparation method thereof |
| CN111362259A (en) * | 2018-12-25 | 2020-07-03 | 中信国安盟固利动力科技有限公司 | Limit low specific surface area lithium ion battery negative electrode material and preparation method thereof |
| CN112018386B (en) * | 2019-05-31 | 2022-03-15 | 宁波杉杉新材料科技有限公司 | Artificial graphite material, composite material, preparation method of composite material and lithium ion secondary battery |
| CN112018386A (en) * | 2019-05-31 | 2020-12-01 | 宁波杉杉新材料科技有限公司 | Artificial graphite material, composite material, preparation method of composite material and lithium ion secondary battery |
| CN110212186A (en) * | 2019-06-13 | 2019-09-06 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of high multiplying power lithium ion battery graphite cathode material |
| CN110156005A (en) * | 2019-06-13 | 2019-08-23 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of the graphite cathode material of fast charge lithium ion battery |
| CN114538434A (en) * | 2022-03-31 | 2022-05-27 | 中国神华煤制油化工有限公司 | Graphite negative electrode material and preparation method and application thereof |
| CN114538434B (en) * | 2022-03-31 | 2023-09-22 | 中国神华煤制油化工有限公司 | Graphite anode material and preparation method and application thereof |
| CN115036490A (en) * | 2022-07-01 | 2022-09-09 | 内蒙古三信科技发展有限公司 | Non-charring negative electrode material with low temperature resistance and preparation method thereof |
| CN116062744A (en) * | 2022-12-23 | 2023-05-05 | 合肥国轩新材料科技有限公司 | Method for preparing artificial graphite by utilizing tailing fine powder |
| CN115924905A (en) * | 2022-12-28 | 2023-04-07 | 广东众大智能科技有限公司 | Asphalt-coated needle coke granularity stabilizing method |
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