CN108706582A - The preparation method of artificial plumbago negative pole material - Google Patents
The preparation method of artificial plumbago negative pole material Download PDFInfo
- Publication number
- CN108706582A CN108706582A CN201810679829.7A CN201810679829A CN108706582A CN 108706582 A CN108706582 A CN 108706582A CN 201810679829 A CN201810679829 A CN 201810679829A CN 108706582 A CN108706582 A CN 108706582A
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- Prior art keywords
- negative pole
- preparation
- plumbago negative
- artificial plumbago
- pole material
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
- H01M4/36—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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 discloses a kind of preparation methods of artificial plumbago negative pole material.Aim to solve the problem that natural graphite material is non-renewable, and quality and source is unstable, production cost is difficult to the technical problems such as controlled.The method of the present invention mainly includes the following steps that：I and II is broken, material size classification, rational gradation composition, except iron is modified, graphitization, and sieve pine etc..The present invention rationally plans as a whole the measures such as, classification broken using I and II and grading, so that coke grain size is met production needs, and pass through its particle size distribution of Gradation Optimization；The Ferromagnetic Impurities that may be introduced during recycling magnetic separation to remove production processing；Modifying agent, which is added, can improve the graphited production efficiency of product and ensure the quality of production of product；Higher charge/discharge capacity and efficiency for charge-discharge are made it have, the electric property of graphite cathode material is optimized；Sieve pine processing makes graphite cathode material be in loose condition (of surface), avoids the hardened reunion of powder granule.
Description
Technical field
The present invention relates to a kind of lithium battery graphite material preparing technical fields, and in particular to a kind of artificial plumbago negative pole material
The preparation method of material.
Background technology
Graphite is one of the mineral of elemental carbon crystallization, has light, high temperature resistant, heat conduction, conduction, lubrication, plasticity and change
It learns stability and waits excellent performances well, be widely used in aerospace, new energy, medicine, information technology, high-end equipment manufacturing, section
The new industries such as energy environmental protection, nuclear industry, new material, will be as the grand strategy resource of the following hi-tech development of support.
Lithium ion battery is widely used in laptop, mobile phone, new-energy automobile, electric vehicle, charge power supply, electronic work
In tool and each field such as digital communication equipment, and lithium ion battery is prepared in material, graphite cathode material be influence lithium from
The key material of sub- battery.Lithium ion battery mainly uses graphite microparticles as the negative material of its conductive cathode, grain at present
Degree is generally between 3 μm~30 μm.
Graphite includes natural graphite material and artificial graphite material, wherein natural graphite is primarily present in association graphite ore
In Tibetan, reserves are huge in earth mining deposits, although and occuping world head in China's natural graphite mineral reserve reserves and yield
Position, but natural graphite belongs to non-renewable mineral resources, and natural graphite is primarily present in association graphite mineral reserve, need through
It crosses exploitation and mine is selected and passed through purification and shaping classification etc. technique and is made, be affected by natural deposit, by cost
Control and product quality are affected.Thus low cost and high performance artificial graphite is then lithium battery graphite cathode material
New available sources.
Invention content
The technical problem to be solved in the present invention is to provide a kind of artificial plumbago negative pole material preparation method for lithium battery,
It is non-renewable to solve natural graphite material, and quality and source is unstable, production cost is difficult to the technical problems such as controlled.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
Using the coke product of petrochemical industry production as raw material, and it is made to occur to be graphitized lattice transformation at high temperature, to become
Artificial plumbago negative pole material, artificial plumbago negative pole material have extraordinary electric property, while have low cost, high magnification,
The characteristics of high capacity rate, long-life.Specific technical solution is as follows：
（1）Level-one is broken：Petroleum coke material coarse cutting is chosen to 0.5~1.5cm of granularity；
（2）Two-stage crushing：Petroleum coke after coarse crushing carries out two-stage crushing to granularity through flour mill and is less than 35 μm；
（3）Classification：Petroleum coke material after two-stage crushing is subjected to classification processing according to different grain size range, it is spare；
（4）Grading：Different grain size petroleum coke is matched according to certain particle size and carries out grading, and it is made to be uniformly mixed；Grading be with
It is classified tight association.Material varies through material particle size that is broken, being obtained after classification process, classification often by 5 μm of granularity <,
5 μm of < granularities <, 20 μm, 20 μm 35 μm of < granularities < are divided into three kinds of particulate, middle grain, coarse grain grain size categories（Meet normal distribution）.
Upon mixing, thin for improving density of material in material, coarse grain is then strong to improve material as skeleton for varigrained material
Degree.Present invention research finds to press above-mentioned three kinds of grain size category gradings, and makes its D50 particle size range（Meet normal distribution）At 7 μm
Between~20 μm, the graphite material after grading may make to all have preferable performance in terms of density and intensity.
（5）Except iron：Resulting material after grading mixing is delivered in magnetic separator progress magnetic separation processing, material removal itself and
The Ferromagnetic Impurities that may be introduced during production processing；
（6）It is modified：By step（5）Resulting material and modifying agent titanium dioxide carry out after mixing, pressure be 0.01~
0.1MPa, room temperature closed environment under be modified processing；
（7）Graphitization：By modified material under the atmospheric condition of inert gas shielding, stone at a temperature of 2000~3000 DEG C
Inkization is handled 2~10 hours；
（8）Sieve pine：By step（7）Material after graphitization processing carries out sieving loose processing in high frequency shale shaker so that after preparation
Graphite cathode material powder granule be in loose condition (of surface), avoid particle board conglomeration poly-.
In the step（1）In, preferably double-roll crusher is crushed.
In the step（2）In, preferably Raymond mill is crushed.
Preferably, in the step（3）In, sorting machine is frequency conversion pneumatic separator.
Preferably, in the step（5）In, the magnetic separator is permanent magnetic separator.
In the step（6）In, the dosage of the modifying agent titanium dioxide is 0.1 ‰~the 1 ‰ for the treatment of material quality.
（Titanium dioxide makes the artificial plumbago negative pole material prepared that certain meso-hole structure be presented, to have better particle absorption
Performance and electric property, while also improving graphited production efficiency）.
Preferably, in the step（8）In, the vibration frequency of the high frequency shale shaker is 5000~10000hz.
Compared with prior art, positive advantageous effects of the invention are：
1. of the invention rationally plan as a whole using level-one the process measure such as broken, two-stage crushing, classification and grading, by petroleum coke into
The processing of row granularity makes its granule size meet production needs, and passes through its particle size distribution of Gradation Optimization；Magnetic separation is recycled to remove
The Ferromagnetic Impurities that may be introduced during production processing are removed, avoid the presence of Ferromagnetic Impurities to the artificial plumbago negative pole of preparation
The electrical property of material has an impact；Modifying agent, which is added, can improve the graphited production efficiency of product and ensure the production matter of product
Amount；Higher charge/discharge capacity and efficiency for charge-discharge are made it have, the electric property of graphite cathode material is optimized；Sieve pine processing makes
It obtains graphite cathode material and is in loose condition (of surface), avoid the hardened reunion of powder granule.
2. synthesis crushes using two-stage and coordinate classification and powder grading to handle, it is same to ensure that granule size satisfaction production needs
When optimize powder granule particle size range distribution, make its granularity processing more rationally efficiently, improve working efficiency
3. modifying agent, which is added, can improve the graphited production efficiency of product and ensure the quality of production of product, its electrical property is improved
Energy.
4. artificial plumbago negative pole material prepared by the present invention is avoided that hardened reunion.
5. preparation method application of the present invention is strong, it is highly suitable for industrial application.
Specific implementation mode
Illustrate the specific implementation mode of the present invention with reference to embodiment, but following embodiment is used only to be described in detail
The present invention does not limit the scope of the invention in any way.
Involved equipment is conventional equipment unless otherwise instructed in the examples below；Involved raw material, such as
It is commercially available material without special instruction；Involved test, preparation method are unless otherwise instructed conventional method.
A kind of 1 artificial plumbago negative pole material preparation method of embodiment, mainly includes the following steps：
（1）Level-one is broken：Petroleum coke raw material is chosen by double-roll crusher coarse crushing to 0.5~1.5cm of granularity；
（2）Two-stage crushing：Petroleum coke after coarse crushing carries out two-stage crushing to granularity through Raymond mill and is less than 35 μm；
（3）Grading：It is different grain size range that petroleum coke material after two-stage crushing is sorted by frequency conversion pneumatic separator
Material, it is spare；
（4）Rational gradation composition：Grading treated material particle size is subjected to grading according to following grain size proportion and makes its mixing
Uniformly, wherein particulate（5 μm of granularity <）：Middle grain（5 μm of 20 μm of < granularities <）：Coarse grain（20 μm of 35 μm of < granularities <）Mass ratio
1:2:1.5, after evenly mixing, particle size range is（Meet normal distribution）D0 < 35 μm, 8.0 μm 18 μm of < D50 <, D94 >
3.0 。
（5）Except iron：Resulting material after grading mixing is delivered to progress magnetic separation processing in permanent magnetic separator, material removal is certainly
The Ferromagnetic Impurities that may be introduced during body and production processing；
（6）It is modified：By treating material quality 0.1 ‰~1 ‰ to step（5）Modifying agent titanium dioxide is added in resulting material
（Titanium dioxide makes the artificial plumbago negative pole material prepared that certain meso-hole structure be presented, to have better particle absorption
Performance and electric property, while also improving graphited production efficiency）After mixing, it is 0.06MPa, room temperature in pressure
Processing is modified under closed environment；
（7）Graphitization：By modified material under the atmospheric condition of inert gas shielding, at a temperature of 2500 DEG C at graphitization
Reason 6 hours；
（8）Sieve pine：By step（7）Material after graphitization processing is in high frequency shale shaker（Vibration frequency is 8000hz）In sieved
Pine processing so that the graphite cathode material powder granule after preparation is in loose condition (of surface), avoids particle board conglomeration poly-.It prepares
The main performance index of artificial plumbago negative pole material is as shown in table 1.
The main performance index of 1 artificial plumbago negative pole material of table
| Granularity | Purity | Resistivity |
| 8μm ~18μm | ≥99 | ≤3.2μΩ·m |
The present invention is described in detail above in conjunction with embodiment, still, person of ordinary skill in the field can
Understand, without departing from the purpose of the present invention, each design parameter in above-described embodiment can also be changed, shape
At multiple specific embodiments, it is the common variation range of the present invention, is no longer described in detail one by one herein.
Claims (9)
1. a kind of preparation method of artificial plumbago negative pole material, includes the following steps：
（1）Level-one is broken：Petroleum coke material coarse cutting is chosen to 0.5~1.5cm of granularity；
（2）Two-stage crushing：Petroleum coke after coarse crushing carries out two-stage crushing to granularity through flour mill and is less than 35 μm；
（3）Classification：Petroleum coke material after two-stage crushing is subjected to classification processing according to different grain size range, it is spare；
（4）Grading：Different grain size petroleum coke is subjected to grading by grain size proportion, and it is made to be uniformly mixed；
（5）Except iron：Resulting material after grading mixing is delivered to progress magnetic separation processing in magnetic separator, material removal itself and production
The Ferromagnetic Impurities that may be introduced in processing procedure；
（6）It is modified：By step（5）Resulting material and modifying agent titanium dioxide carry out after mixing, pressure be 0.01~
0.1MPa, room temperature closed environment under be modified processing；
（7）Graphitization：By modified material under the atmospheric condition of inert gas shielding, stone at a temperature of 2000~3000 DEG C
Inkization is handled 2~10 hours；
（8）Sieve pine：By step（7）Material after graphitization processing carries out sieving loose processing in high frequency shale shaker so that after preparation
Graphite cathode material powder granule be in loose condition (of surface), avoid particle board conglomeration poly-.
2. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（1）
In, preferably double-roll crusher is crushed.
3. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（2）
In, select Raymond mill to be crushed.
4. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（3）
In, classification processing is carried out using frequency conversion pneumatic separator.
5. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（3）
In, it is divided into three kinds of particulate, middle grain, coarse grain granularities etc. by 5 μm, 5 μm of granularity <, 20 μm, 20 μm of < granularities <, 35 μm of < granularities <
Grade.
6. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（4）
In, the principle of grading is typically to make its D50 particle size range between 7 μm~20 μm by after three kinds of grain size category gradings.
7. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（5）
In, the magnetic separator is permanent magnetic separator.
8. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（6）
In, the dosage of the modifying agent titanium dioxide is 0.1 ‰~the 1 ‰ for the treatment of material quality.
9. the preparation method of artificial plumbago negative pole material according to claim 1, which is characterized in that in the step（8）
In, the vibration frequency control of the high frequency shale shaker is 5000~10000hz.
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Cited By (4)
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| CN110127687A (en) * | 2019-05-24 | 2019-08-16 | 深圳鸿鹏新能源科技有限公司 | Artificial graphite and its preparation method and application |
| CN113823792A (en) * | 2021-01-05 | 2021-12-21 | 广东东岛新能源股份有限公司 | Preparation method for producing negative electrode material for lithium ion battery by using blocky graphite |
| CN114273025A (en) * | 2021-09-27 | 2022-04-05 | 济南宏腾信息科技有限公司 | Production method of artificial graphite negative electrode material |
| CN114585589A (en) * | 2020-01-10 | 2022-06-03 | 株式会社Lg新能源 | Artificial graphite, method for producing artificial graphite, negative electrode comprising artificial graphite, and lithium secondary battery |
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Application publication date: 20181026 |