CN112794319A - Preparation method of coking coal-based high-rate graphite negative electrode material - Google Patents
Preparation method of coking coal-based high-rate graphite negative electrode material Download PDFInfo
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- CN112794319A CN112794319A CN202011428281.2A CN202011428281A CN112794319A CN 112794319 A CN112794319 A CN 112794319A CN 202011428281 A CN202011428281 A CN 202011428281A CN 112794319 A CN112794319 A CN 112794319A
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- coking coal
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- 239000003245 coal Substances 0.000 title claims abstract description 93
- 238000004939 coking Methods 0.000 title claims abstract description 93
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 31
- 239000010439 graphite Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000000465 moulding Methods 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000010406 cathode material Substances 0.000 claims abstract description 21
- 238000000748 compression moulding Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005087 graphitization Methods 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000011331 needle coke Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- 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 provides a preparation method of a coking coal-based high-rate graphite cathode material, which comprises the following steps: crushing coke powder, namely crushing the coke powder into powder with the average particle size of 4-8 mu m; step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa; roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃; step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 10-14 mu m; and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at the temperature of 3000 ℃. The method comprises the following steps of sequentially carrying out crushing, forming, roasting, secondary crushing, graphitization and the like on coking coal with a certain index to prepare a graphite negative electrode material applied to a high-rate lithium ion battery; compared with the existing preparation method of the high-rate cathode material in the market, the method disclosed by the invention is lower in production cost, higher in yield and better in battery processing performance.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a preparation method of a coking coal-based high-rate graphite negative electrode material.
Background
The high-rate lithium ion battery is mainly applied to the fields of electric tools, aerospace models, unmanned aerial vehicles and the like, and is basically characterized by having the capacity of large-current charging and discharging. In order to improve the rate capability of the material, the currently adopted scheme is to crush needle coke before calcination to a small particle size of 6-8 μm, and graphitize to obtain the high-rate graphite negative electrode material. The problems of this solution include: (1) the price of the needle coke is high, and the needle coke is crushed to a small particle size of 6-8 mu m, so that the yield is low, and the cost of the raw materials is too high; (2) the packing density of the needle-shaped coke powder with the particle size of 6-8 mu m is too small, so that the charging amount of the material is too small, and the graphitization cost is too high; (3) the particle size of the finished product is too small, resulting in poor processability of the battery.
Disclosure of Invention
The invention aims to provide a preparation method of a coking coal-based high-rate graphite negative electrode material. The invention takes cheap coking coal as raw material, adopts mature process in carbon industry to prepare the high-rate graphite cathode material with good battery processing performance.
The technical scheme of the invention is realized as follows: a preparation method of a coking coal-based high-rate graphite cathode material comprises the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 4-8 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 10-14 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Preferably, the volatile matter of the coking coal is 15-30% and the ash content is less than 8%.
Preferably, the volatile matter of the coking coal is 20% and the ash content is 5%.
Preferably, the preparation method of the coking coal-based high-rate graphite negative electrode material comprises the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 6 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 12 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Preferably, the preparation method of the coking coal-based high-rate graphite negative electrode material comprises the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 7 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 13 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Compared with the prior art, the method comprises the steps of sequentially carrying out crushing, forming, roasting, secondary crushing, graphitization and the like on the coking coal with a certain index to prepare the graphite cathode material applied to the high-rate lithium ion battery; compared with the existing preparation method of the high-rate cathode material in the market, the method disclosed by the invention is lower in production cost, higher in yield and better in battery processing performance.
Drawings
FIG. 1 is a SEM photograph of a product of example II.
FIG. 2 is a charging/discharging curve of the product of the second embodiment.
FIG. 3 is a discharge curve of a full cell assembled by using the product of example two as a negative electrode and lithium cobaltate as a positive electrode.
FIG. 4 is a summary of the rate performance data for the products of example two.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
The following description is made for different data:
example one
A preparation method of a coking coal-based high-rate graphite cathode material comprises the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 4 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 10 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Preferably, the volatile matter of the coking coal is 15% and the ash content is 3%.
Example two
A preparation method of a coking coal-based high-rate graphite cathode material comprises the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 6 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 12 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Preferably, the volatile matter of the coking coal is 20% and the ash content is 5%.
EXAMPLE III
A preparation method of a coking coal-based high-rate graphite cathode material comprises the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 7 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 13 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Preferably, the coking coal has 25% of volatile matter and 7% of ash.
Example four
A preparation method of a coking coal-based high-rate graphite cathode material comprises the following steps:
crushing coke powder, namely crushing the coke into powder with the average particle size of 8 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 14 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
Preferably, the coking coal has a volatile matter content of 30% and an ash content of 7.5%.
The electrode obtained in example two was measured to have a gram capacity of 339 mAh/g and a first coulombic efficiency of 92.3%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The preparation method of the coking coal-based high-rate graphite cathode material is characterized by comprising the following steps of:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 4-8 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 10-14 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
2. The preparation method of the coking coal-based high-rate graphite negative electrode material as claimed in claim 1, wherein the volatile content of the coking coal is 15-30%, and the ash content is less than 8%.
3. The method for preparing the coking coal-based high-rate graphite negative electrode material according to claim 2, wherein the coking coal has a volatile content of 20% and an ash content of 5%.
4. The preparation method of the coking coal-based high-rate graphite negative electrode material according to claim 1, which is characterized by comprising the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 6 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 12 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
5. The preparation method of the coking coal-based high-rate graphite negative electrode material according to claim 1, which is characterized by comprising the following steps:
crushing coke powder, namely crushing the coke powder into powder with the average particle size of 7 mu m;
step two, molding, namely, molding the coking coal powder into block coking coal by compression molding, wherein the molding pressure is 2 MPa;
roasting, namely roasting the blocky coking coal in a roasting furnace at the temperature of 1000 ℃;
step four, secondary crushing, wherein the roasted product is subjected to secondary crushing to obtain carbonized coking coal powder with the average particle size of 13 mu m;
and step five, graphitizing the carbonized coking coal powder in an Acheson graphitizing furnace at 3000 ℃ to prepare the coking coal-based high-rate graphite cathode material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022257372A1 (en) * | 2021-06-10 | 2022-12-15 | 国家能源投资集团有限责任公司 | Graphite negative electrode material, preparation method therefor and use thereof |
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| GB759182A (en) * | 1953-01-06 | 1956-10-17 | Kaiser Aluminium Chem Corp | Improvements in or relating to the production of carbon material |
| CN104085883A (en) * | 2014-07-09 | 2014-10-08 | 深圳市贝特瑞新能源材料股份有限公司 | Artificial graphite negative electrode material for lithium ion battery and preparation method thereof |
| CN104681786A (en) * | 2015-03-04 | 2015-06-03 | 深圳市贝特瑞新能源材料股份有限公司 | Coal-based anode material, preparation method and lithium-ion battery |
| JP2018006270A (en) * | 2016-07-07 | 2018-01-11 | 新日鉄住金化学株式会社 | Graphite carbon material for lithium ion secondary battery negative electrode, method for manufacturing the same, and negative electrode or battery arranged by use thereof |
| 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 |
| CN111710530A (en) * | 2020-05-18 | 2020-09-25 | 大唐可再生能源试验研究院有限公司 | Preparation method of low-order coal-based porous carbon and application of low-order coal-based porous carbon in supercapacitor |
-
2020
- 2020-12-07 CN CN202011428281.2A patent/CN112794319A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB759182A (en) * | 1953-01-06 | 1956-10-17 | Kaiser Aluminium Chem Corp | Improvements in or relating to the production of carbon material |
| CN104085883A (en) * | 2014-07-09 | 2014-10-08 | 深圳市贝特瑞新能源材料股份有限公司 | Artificial graphite negative electrode material for lithium ion battery and preparation method thereof |
| CN104681786A (en) * | 2015-03-04 | 2015-06-03 | 深圳市贝特瑞新能源材料股份有限公司 | Coal-based anode material, preparation method and lithium-ion battery |
| JP2018006270A (en) * | 2016-07-07 | 2018-01-11 | 新日鉄住金化学株式会社 | Graphite carbon material for lithium ion secondary battery negative electrode, method for manufacturing the same, and negative electrode or battery arranged by use thereof |
| 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 |
| CN111710530A (en) * | 2020-05-18 | 2020-09-25 | 大唐可再生能源试验研究院有限公司 | Preparation method of low-order coal-based porous carbon and application of low-order coal-based porous carbon in supercapacitor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022257372A1 (en) * | 2021-06-10 | 2022-12-15 | 国家能源投资集团有限责任公司 | Graphite negative electrode material, preparation method therefor and use thereof |
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Application publication date: 20210514 |