CN115108551A - Method for manufacturing graphite negative electrode material - Google Patents
Method for manufacturing graphite negative electrode material Download PDFInfo
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- CN115108551A CN115108551A CN202210961290.0A CN202210961290A CN115108551A CN 115108551 A CN115108551 A CN 115108551A CN 202210961290 A CN202210961290 A CN 202210961290A CN 115108551 A CN115108551 A CN 115108551A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 103
- 239000010439 graphite Substances 0.000 title claims abstract description 103
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007773 negative electrode material Substances 0.000 title claims description 8
- 239000013078 crystal Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 24
- 239000010406 cathode material Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 12
- 238000010008 shearing Methods 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 229910021382 natural graphite Inorganic materials 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
-
- 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
- C01B32/21—After-treatment
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The application discloses a method for manufacturing a graphite cathode material, which comprises the following steps: and (3) carrying out microwave treatment on the crystalline graphite. Shearing and mixing the crystal graphite subjected to microwave treatment with water, and then carrying out ultrasonic treatment to obtain a crystal graphite solution. And centrifuging, washing, extracting, performing high-temperature treatment, crushing, selecting particles and performing electromagnetic iron removal on the crystalline graphite solution to obtain the graphite cathode material. The manufacturing method of the graphite cathode material has the advantages of environmental protection, low energy consumption, high yield, good energy density and long cycle life, and is an ideal manufacturing method of the graphite cathode material.
Description
Technical Field
The application relates to the field of chemical manufacturing, in particular to a manufacturing method of a graphite negative electrode material.
Background
At present, graphite materials are mainly used as the negative electrode materials of the lithium ion batteries and comprise natural graphite and artificial graphite. Compared with artificial graphite, natural graphite has high specific capacity, high compacted density, simple process and low production cost, but has great disadvantages in the aspects of cycle performance, quick charging and the like.
The main reasons for the poor performance of natural graphite in the aspects of circulation, quick charging and the like are as follows: 1. the distance between graphite layers is smaller than that of artificial graphite, the resistance of lithium ions in the embedding process is larger, and the lithium ions are easy to be separated out on the surface of the graphite under large current to cause capacity loss; natural graphite has more surface defects, an SEI film formed in the first charge and discharge has poor stability, and the cycle performance is reduced due to continuous damage and generation of SEI in the subsequent charge and discharge processes.
Disclosure of Invention
The application provides a manufacturing method of a graphite cathode material, which can realize environmental protection, low energy consumption, high yield and good energy density and cycle life.
The application provides a manufacturing method of a graphite negative electrode material, which comprises the following steps: and (3) carrying out microwave treatment on the crystalline graphite. Shearing and mixing the crystal graphite subjected to microwave treatment with water, and then carrying out ultrasonic treatment to obtain a crystal graphite solution. And centrifuging, washing, extracting, performing high-temperature treatment, crushing, selecting particles and performing electromagnetic iron removal on the crystalline graphite solution to obtain the graphite cathode material.
In some of these embodiments, the crystalline graphite has a particle size of 150-250 mesh.
In some of these embodiments, the conditions of the microwave treatment are: the time is 8-10 minutes, and the power is 600-700 watts.
In some of these embodiments, the mass of water is 10-12 times the mass of the crystalline graphite.
In some of these embodiments, the sonication conditions are: the time is 12-15 hours, and the power is 1200 and 1500 watts.
In some of these embodiments, the washing conditions are: adopting 10000-12000 ml of dilute hydrochloric acid with the mass concentration of 1-2% to carry out acid cleaning.
In some of these examples, the stirring time during the acid washing is 4 to 5 hours.
In some of these embodiments, the conditions for extraction are: the extraction is carried out by adopting at least one of glycol, N-methyl pyrrolidone and phenyl solvent.
In some of these embodiments, the conditions of the high temperature treatment are: the temperature is 400-500 ℃.
In some of these embodiments, the conditions for sizing are: the particle size is 21-30 microns when D50 is equal.
Compared with the prior art, the method has the following beneficial effects:
the manufacturing method enlarges the graphite interlayer spacing, reduces the surface defects, realizes environmental protection, low energy consumption and high yield, realizes good energy density and cycle life at the same time, and is an ideal manufacturing method of the graphite cathode material.
Detailed Description
The technical method in the embodiments of the present application will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The application provides a manufacturing method of a graphite negative electrode material, which comprises the following steps:
step one, carrying out microwave treatment on the crystalline graphite.
In the above steps, before microwave treatment of the crystalline graphite, the crystalline graphite with fully developed crystals is selected, then crushed to reach the required granularity, and then other impurities such as silicon oxide, aluminum oxide and the like are removed, and then the dried crystalline graphite is dried, and finally the dried crystalline graphite is subjected to microwave treatment. In the process, the defects and impurities in the material are fully exposed under the action of the rapid heat of the microwave, and the unqualified material outside the crystal nucleus can be effectively stripped to be reserved for next separation.
The granularity of the crystalline graphite is 150 meshes, 250 meshes, such as 150 meshes, 200 meshes and 250 meshes.
The conditions of the microwave treatment were: the time is 8-10 minutes, such as 8 minutes, 9 minutes and 10 minutes, and the power is 600-700 watts, such as 600 watts, 650 watts and 700 watts.
In the related technology, with the rapid development of the ion battery industry, the graphite cathode material which is an important component of the ion battery also has an explosive development, and people find that the traditional natural heat graphite additional material has a layered structure in application, and the layered structure gradually loses efficacy and disintegrates after repeated charge and discharge cycles in application, so that the service life of the cathode material is directly influenced. In order to solve the problem, a crystallization process is introduced in the preparation of the natural graphite cathode material, and a crystal graphite core is generated by re-melting in cathode graphite material particles at a high temperature so as to maintain the strength of the cathode material and ensure the service life. After the crystallization process is introduced, a large amount of energy is consumed and various toxic substances are discharged in order to form crystal nuclei in the graphite negative electrode material particles. The environment is seriously influenced, the manufacturing requirement of low energy consumption is not met, and the graphite cathode manufactured by using crystallization processes is limited in a plurality of places so far, so that the application requirement cannot be met. The method has the advantages that the natural crystalline graphite is adopted in the steps, the crystalline core of the graphite is effectively reserved, impurities which do not meet requirements are removed, the graphite cathode material with crystal nuclei can be realized without a crystallization process, the use requirements can be met, and the crystallization process with high energy consumption is not needed.
And step two, shearing and mixing the crystal graphite subjected to microwave treatment with water, and then carrying out ultrasonic treatment to obtain a crystal graphite solution.
In the above steps, the gaps are further deepened by the ultrasonic action, and the corners which do not meet the requirements in the graphite are eliminated.
Shear mixing may be carried out in a shearing apparatus such as a colloid mill. The shear mixing time is 1-3 hours, such as 1 hour, 2 hours, 3 hours.
The water may be deionized water. The mass of water is 10-12 times, such as 10 times, 11 times, 12 times of the mass of the crystalline graphite.
The ultrasonic treatment conditions were: the time is 12-15 hours, such as 12 hours, 13 hours and 15 hours, and the power is 1200-1500 watts, such as 1200 watts, 1300 watts and 1500 watts.
And step three, centrifuging, washing, extracting, performing high-temperature treatment, crushing, selecting particles and performing electromagnetic iron removal on the crystalline graphite solution to obtain the graphite cathode material.
In the above step, the washing conditions are as follows: the acid washing is carried out by using 10000-12000 ml (10000 ml, 11000 ml and 12000 ml) of diluted hydrochloric acid with the mass concentration of 1-2 percent (1 percent, 1.5 percent and 2 percent). In the acid washing process, the stirring time is 4-5 hours, such as 4 hours and 5 hours, and the stirring speed is 300-400 rpm, such as 300 rpm, 350 rpm and 400 rpm. In addition, instead of using dilute hydrochloric acid, oxalic acid may also be used. The above washing process eliminates organic impurities and impurities such as copper, iron, cobalt, etc.
The extraction conditions were: the extraction is carried out by adopting at least one of glycol, N-methyl pyrrolidone and phenyl solvent. The above extraction process effectively separates impurities below 5 microns.
The conditions of the high-temperature treatment are as follows: the temperature is 400-500 ℃, such as 400 ℃, 450 ℃ and 500 ℃, and the time is 2-3 hours, such as 2 hours and 3 hours. The high-temperature treatment may be performed in a chain type high-temperature furnace. The high temperature treatment process can eliminate organic impurities.
The particle selection conditions are as follows: the particle size is 21-30 microns (D50), such as 21 microns (D50), 26 microns (D50) and 30 microns (D50).
The following is a detailed description with reference to examples:
example 1
Selecting 150-mesh crystalline graphite with fully developed crystals, crushing to reach the required granularity, removing other impurities such as silicon oxide, aluminum oxide and the like, drying, and finally performing microwave treatment on the dried crystalline graphite, wherein the microwave treatment time is 10 minutes and the power is 600 watts. In the process, the graphite is rapidly heated by using microwaves, so that the original gap of the graphite is continuously enlarged and finally cracked, the original defective part of the graphite can be cracked, and at the moment, the size of the graphite is smaller than that of the original graphite, and the graphite is shown to be reduced to 38 micrometers by adopting a particle size test (D50).
Shearing and mixing the crystal graphite subjected to microwave treatment with deionized water, wherein the mass of the deionized water is 10 times that of the crystal graphite, the shearing and mixing time is 1 hour, then carrying out ultrasonic treatment, the ultrasonic treatment time is 15 hours, and the power is 1200 watts, so as to obtain a crystal graphite solution. The above process deepens the gap depth on the graphite surface and simultaneously removes the protruded edges and corners on the graphite surface, at this time, the particle size of the graphite is further reduced.
Centrifuging a crystalline graphite solution, then carrying out acid washing by adopting 10000 ml of dilute hydrochloric acid with the mass concentration of 1%, stirring for 4 hours at the stirring speed of 300 r/min in the acid washing process, then extracting by adopting ethylene glycol, then carrying out high-temperature treatment for 2 hours in a high-temperature furnace at 400 ℃, then crushing, selecting particles with the particle size of D50-30 microns, and carrying out electromagnetic iron removal to obtain the graphite cathode material.
The manufactured graphite cathode material is used as a cathode of a lithium ion battery for testing, the energy density is 340 milliampere hours and grams, the cycle life is 5000 times, and the use requirement of the battery cathode material is met.
Example 2
Selecting 250-mesh crystalline graphite with fully developed crystals, then carrying out crushing treatment to reach the required granularity, then removing other impurities such as silicon oxide, aluminum oxide and the like, then drying, and finally carrying out microwave treatment on the dried crystalline graphite, wherein the microwave treatment time is 8 minutes and the power is 700 watts. In the process, the graphite is rapidly heated by using microwaves, so that the original gap of the graphite is continuously enlarged and finally cracked, the original defective part of the graphite can be cracked, and at the moment, the size of the graphite is smaller than that of the original graphite, and the graphite is shown to be reduced to 26 microns by adopting a particle size test (D50).
Shearing and mixing the crystal graphite subjected to microwave treatment with deionized water, wherein the mass of the deionized water is 11 times that of the crystal graphite, the shearing and mixing time is 3 hours, then carrying out ultrasonic treatment, the ultrasonic treatment time is 13 hours, and the power is 1300 watts, so as to obtain a crystal graphite solution. The above process deepens the gap depth on the graphite surface and simultaneously removes the protruded edges and corners on the graphite surface, at this time, the particle size of the graphite is further reduced.
Centrifuging the crystalline graphite solution, then carrying out acid washing by using 12000 ml of dilute hydrochloric acid with the mass concentration of 2%, stirring for 5 hours at the stirring speed of 400 rpm, then extracting by using N-methyl pyrrolidone, then carrying out high-temperature treatment for 2 hours in a high-temperature furnace at 500 ℃, then crushing, selecting particles with the particle size of 21 microns (D50), and carrying out electromagnetic iron removal to obtain the graphite cathode material.
The manufactured graphite cathode material is used as the cathode of the lithium ion battery for testing, the energy density is 420 mAmp.g, the cycle life is 5000 times, and the use requirement of the battery cathode material is met.
Example 3
Selecting 200-mesh crystalline graphite with fully developed crystals, crushing to reach the required granularity, removing other impurities such as silicon oxide, aluminum oxide and the like, drying, and finally performing microwave treatment on the dried crystalline graphite, wherein the microwave treatment time is 9 minutes and the power is 650 watts. In the process, the graphite is rapidly heated by using microwaves, so that the original gap of the graphite is continuously enlarged and finally cracked, the original defective part of the graphite can be cracked, and at the moment, the size of the graphite is smaller than that of the original graphite, and the graphite is shown to be reduced to 30 micrometers by adopting a particle size test (D50).
Shearing and mixing the crystal graphite subjected to microwave treatment with deionized water, wherein the mass of the deionized water is 12 times that of the crystal graphite, the shearing and mixing time is 2 hours, then carrying out ultrasonic treatment, the ultrasonic treatment time is 15 hours, and the power is 1200 watts, so as to obtain a crystal graphite solution. The above process deepens the gap depth on the graphite surface and simultaneously removes the protruded edges and corners on the graphite surface, at this time, the particle size of the graphite is further reduced.
Centrifuging the crystalline graphite solution, then carrying out acid washing by using 11000 ml of diluted hydrochloric acid with the mass concentration of 1.5%, stirring for 4 hours in the acid washing process, at the stirring speed of 350 r/min, then extracting by using N-methyl pyrrolidone, then carrying out high-temperature treatment for 3 hours in a high-temperature furnace at 500 ℃, then crushing, selecting particles with the particle size of D50-26 microns, and carrying out electromagnetic iron removal to obtain the graphite cathode material.
The manufactured graphite cathode material is used as the cathode of the lithium ion battery for testing, the energy density is 390 milliampere hours and gram, the cycle life is 5000 times, and the use requirement of the battery cathode material is met.
The foregoing shows and describes the general principles, essential features, and advantages of the application. It will be understood by those skilled in the art that the present application is not limited to the embodiments described above, which are presented solely for purposes of illustrating the principles of the application, and that various changes and modifications may be made without departing from the spirit and scope of the application, which is defined by the appended claims, the specification, and equivalents thereof.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present application and not for limiting the protection scope of the present application, and although the present application is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present application without departing from the spirit and scope of the technical solutions of the present application.
Claims (10)
1. A method for manufacturing a graphite negative electrode material is characterized by comprising the following steps:
carrying out microwave treatment on the crystalline graphite;
shearing and mixing the crystal graphite subjected to microwave treatment with water, and then carrying out ultrasonic treatment to obtain a crystal graphite solution;
and centrifuging, washing, extracting, performing high-temperature treatment, crushing, selecting particles and performing electromagnetic iron removal on the crystalline graphite solution to obtain the graphite cathode material.
2. The manufacturing method according to claim 1,
the granularity of the crystalline graphite is 150-250 meshes.
3. The manufacturing method according to claim 1,
the microwave treatment conditions are as follows: the time is 8-10 minutes, and the power is 600-700 watts.
4. The manufacturing method according to claim 1,
the mass of the water is 10-12 times of that of the crystalline graphite.
5. The manufacturing method according to claim 1,
the ultrasonic treatment conditions are as follows: the time is 12-15 hours, and the power is 1200-1500 watts.
6. The manufacturing method according to claim 1,
the washing conditions are as follows: adopting 10000-12000 ml of dilute hydrochloric acid with the mass concentration of 1-2% to carry out acid cleaning.
7. The manufacturing method according to claim 6,
in the acid washing process, the stirring time is 4-5 hours.
8. The manufacturing method according to claim 1,
the extraction conditions are as follows: the extraction is carried out by adopting at least one of glycol, N-methyl pyrrolidone and phenyl solvent.
9. The manufacturing method according to claim 1,
the high-temperature treatment conditions are as follows: the temperature is 400-500 ℃.
10. The manufacturing method according to claim 1,
the particle selection conditions are as follows: the particle size is 21-30 microns when D50 is equal.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116239110A (en) * | 2023-01-09 | 2023-06-09 | 中山烯利来设备科技有限公司 | Shearing assembly line system |
CN117023575A (en) * | 2023-08-10 | 2023-11-10 | 深圳市华明胜科技有限公司 | Preparation process of high-capacity negative electrode material with gram capacity of 370mah/g |
CN117352711A (en) * | 2023-12-06 | 2024-01-05 | 上海巴库斯超导新材料有限公司 | Preparation process of novel carbon-coated silicon and graphite composite negative electrode material |
CN117550593A (en) * | 2024-01-11 | 2024-02-13 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
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CN103259018A (en) * | 2013-04-27 | 2013-08-21 | 黑龙江大学 | Preparation method of porous graphite flake applied to super-electric negative pole of lithium battery |
CN105375030A (en) * | 2015-10-30 | 2016-03-02 | 福建翔丰华新能源材料有限公司 | Preparation method of low-temperature and high-rate graphite anode material for power battery |
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2022
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103259018A (en) * | 2013-04-27 | 2013-08-21 | 黑龙江大学 | Preparation method of porous graphite flake applied to super-electric negative pole of lithium battery |
CN105375030A (en) * | 2015-10-30 | 2016-03-02 | 福建翔丰华新能源材料有限公司 | Preparation method of low-temperature and high-rate graphite anode material for power battery |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116239110A (en) * | 2023-01-09 | 2023-06-09 | 中山烯利来设备科技有限公司 | Shearing assembly line system |
CN117023575A (en) * | 2023-08-10 | 2023-11-10 | 深圳市华明胜科技有限公司 | Preparation process of high-capacity negative electrode material with gram capacity of 370mah/g |
CN117352711A (en) * | 2023-12-06 | 2024-01-05 | 上海巴库斯超导新材料有限公司 | Preparation process of novel carbon-coated silicon and graphite composite negative electrode material |
CN117352711B (en) * | 2023-12-06 | 2024-01-30 | 上海巴库斯超导新材料有限公司 | Preparation process of novel carbon-coated silicon and graphite composite negative electrode material |
CN117550593A (en) * | 2024-01-11 | 2024-02-13 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
CN117550593B (en) * | 2024-01-11 | 2024-04-26 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
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