CN112573516A - Preparation method of graphite negative electrode material for energy storage lithium ion battery - Google Patents
Preparation method of graphite negative electrode material for energy storage lithium ion battery Download PDFInfo
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- CN112573516A CN112573516A CN202011427794.1A CN202011427794A CN112573516A CN 112573516 A CN112573516 A CN 112573516A CN 202011427794 A CN202011427794 A CN 202011427794A CN 112573516 A CN112573516 A CN 112573516A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000004146 energy storage Methods 0.000 title claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 23
- 239000010439 graphite Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 16
- 239000007773 negative electrode material Substances 0.000 title claims description 6
- 239000000571 coke Substances 0.000 claims abstract description 44
- 239000010426 asphalt Substances 0.000 claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000010406 cathode material Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000004132 cross linking Methods 0.000 claims abstract description 10
- 239000011294 coal tar pitch Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000007711 solidification Methods 0.000 claims abstract description 9
- 230000008023 solidification Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000002006 petroleum coke Substances 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000011331 needle coke Substances 0.000 claims description 6
- 239000006253 pitch coke Substances 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 239000010405 anode material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000005087 graphitization Methods 0.000 abstract description 2
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 2
- 239000004634 thermosetting polymer Substances 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003860 storage 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
-
- 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
-
- 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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a preparation method of a graphite cathode material for an energy storage lithium ion battery, which comprises the following preparation steps: crushing coke, namely crushing the coke into powder with the average particle size of 15-17 mu m; step (2), mixing, wherein the coke powder and the coal tar pitch powder with the average particle size of 6-10 mu m and the softening point of 100-150 ℃ are uniformly mixed according to the mass ratio of 100:6-100: 10; step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at the temperature of 250-350 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 0.5-1.5 m3And h, completing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt. The invention carries out the coke powder under the air atmosphereThe asphalt coating treatment is carried out, so that the asphalt on the surface of coke particles is changed into a thermosetting polymer structure with insoluble and infusible characteristics; in the graphitization process, the stability of the electrode structure is ensured, and in addition, the heating is only 250-350 ℃, so that the energy is saved, and the yield is higher.
Description
Technical Field
The invention relates to the technical field of electrode production, in particular to a preparation method of a graphite cathode material for an energy storage lithium ion battery.
Background
The energy storage lithium ion battery is mainly applied to the fields of base stations, household energy storage, commercial standby power supplies, wind power and light energy power generation and storage, power grid frequency modulation and peak shaving and the like, and has the basic characteristics of good cycle performance and low cost. Therefore, the energy storage type negative electrode material has the characteristics of low price, good cycle performance and the like. The energy storage type negative electrode material commonly used at present is artificial graphite with an isotropic structure prepared by grinding, granulating and graphitizing petroleum coke before calcination. The anode material has excellent cycle performance, but has the disadvantages of long production process, low yield of each process and high granulation temperature (550-.
Disclosure of Invention
The invention aims to provide a preparation method of a graphite cathode material for an energy storage lithium ion battery, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a graphite cathode material for an energy storage lithium ion battery comprises the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 15-17 mu m;
step (2), mixing, wherein the coke powder and the coal tar pitch powder with the average particle size of 6-10 mu m and the softening point of 100-150 ℃ are uniformly mixed according to the mass ratio of 100:6-100: 10;
step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at the temperature of 250-350 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 0.5-1.5 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
Preferably, the coke is one, two or three of petroleum coke, pitch coke and needle coke, and the volatile matter of the coke is 6-10%, the ash content is less than 1%, and the sulfur content is less than 0.5%.
Preferably, the preparation method of the graphite negative electrode material for the energy storage lithium ion battery comprises the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 16 mu m;
step (2), mixing, namely uniformly mixing coke powder and coal tar pitch powder with the average particle size of 6 mu m and the softening point of 120 ℃ in a mass ratio of 100: 7;
step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at 320 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 1 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
Compared with the prior art, the method has the beneficial effects that the coke powder is subjected to asphalt coating treatment in the air atmosphere, so that the asphalt is covered on the surfaces of coke particles, and the oxidative crosslinking and curing of coal asphalt are realized, so that the asphalt on the surfaces of the coke particles is changed into a thermosetting polymer structure with insoluble and infusible properties; in the subsequent graphitization process, the volume shrinkage of the cross-linked asphalt is obviously smaller than that of coke, so that a closed hole structure is formed, a space is reserved for the expansion of graphite formed by the coke during lithium insertion, the stability of an electrode structure is ensured, and the cycle performance of the lithium ion battery is improved; in addition, the heating is only 250-350 ℃ which is far lower than 550-650 ℃ of the granulation process, the heating time is only 2-4h which is far lower than 6-10h of the granulation process, and therefore, the method is more energy-saving and has higher yield.
Drawings
Fig. 1 is a schematic diagram of the technical solution of the present invention.
FIG. 2 is a SEM photograph of the product of the example.
Figure 3 charging and discharging curves for the second product of example two.
FIG. 4 shows cycle performance data for a full cell 1C cycle at room temperature assembled with the product of example two as the negative electrode and lithium cobaltate as the positive electrode.
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 graphite cathode material for an energy storage lithium ion battery comprises the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 15 mu m;
step (2), mixing, namely uniformly mixing coke powder and coal tar pitch powder with the average particle size of 6 mu m and the softening point of 100 ℃ in a mass ratio of 100: 7;
step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at 250 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 0.5m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
Preferably, the coke is one, two or three of petroleum coke, pitch coke and needle coke, and the volatile matter of the coke is 6%, the ash content is less than 1%, and the sulfur content is less than 0.5%.
Example two
A preparation method of a graphite cathode material for an energy storage lithium ion battery comprises the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 16 mu m;
step (2), mixing, namely uniformly mixing coke powder and coal tar pitch powder with the average particle size of 6 mu m and the softening point of 120 ℃ in a mass ratio of 100: 7;
step (3), coating with asphalt in air atmosphereHeating the mixed material in a roller furnace or a horizontal kettle at 320 ℃ while stirring, wherein the heating time is 2-4h, and the air flow is 1 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
Preferably, the coke is one, two or three of petroleum coke, pitch coke and needle coke, and the volatile matter of the coke is 7%, the ash content is less than 1%, and the sulfur content is less than 0.5%.
EXAMPLE III
A preparation method of a graphite cathode material for an energy storage lithium ion battery comprises the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 16.5 mu m;
step (2), mixing, namely uniformly mixing coke powder and coal tar pitch powder with the average particle size of 8 mu m and the softening point of 135 ℃ in a mass ratio of 100: 7;
step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at the temperature of 250-350 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 0.5-1.5 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
Preferably, the coke is one, two or three of petroleum coke, pitch coke and needle coke, and the volatile matter of the coke is 8%, the ash content is less than 1%, and the sulfur content is less than 0.5%.
Example four
A preparation method of a graphite cathode material for an energy storage lithium ion battery comprises the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 17 mu m;
step (2), mixing, namely uniformly mixing coke powder and coal tar pitch powder with the average particle size of 10 mu m and the softening point of 150 ℃ in a mass ratio of 100: 7;
step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at 330 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 1.5 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
Preferably, the coke is one, two or three of petroleum coke, pitch coke and needle coke, and the volatile matter of the coke is 9%, the ash content is less than 1%, and the sulfur content is less than 0.5%.
After the electrode prepared in the second embodiment is measured, the gram capacity of the electrode is 355.7 mAh/g, the first coulombic efficiency is 93.3%, the cycle performance data of the full-cell assembled by taking the electrode as the negative electrode and lithium cobaltate as the positive electrode under the normal temperature of 1C cycle is obtained, the capacity of the negative electrode of the electrode prepared in the second embodiment is 8% excessive, and the compaction density of the negative electrode is 1.58 g/cm3。
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 (3)
1. A preparation method of a graphite cathode material for an energy storage lithium ion battery is characterized by comprising the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 15-17 mu m;
step (2), mixing, wherein the coke powder and the coal tar pitch powder with the average particle size of 6-10 mu m and the softening point of 100-150 ℃ are uniformly mixed according to the mass ratio of 100:6-100: 10;
step (3), coating asphalt, mixing the materials in a roller furnace or a horizontal kettle at the temperature of 250-350 ℃ in the air atmosphereHeating under stirring for 2-4 hr with air flow rate of 0.5-1.5 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
2. The preparation method of the graphite negative electrode material for the energy storage lithium ion battery according to claim 1, wherein the coke is one, two or three of petroleum coke, pitch coke and needle coke, and the volatile matter of the coke is 6-10%, the ash content is less than 1%, and the sulfur content is less than 0.5%.
3. The preparation method of the graphite anode material for the energy storage lithium ion battery according to claim 1, characterized by comprising the following preparation steps:
crushing coke, namely crushing the coke into powder with the average particle size of 16 mu m;
step (2), mixing, namely uniformly mixing coke powder and coal tar pitch powder with the average particle size of 6 mu m and the softening point of 120 ℃ in a mass ratio of 100: 7;
step (3), coating asphalt, heating the mixed material in a roller furnace or a horizontal kettle at 320 ℃ under the air atmosphere while stirring, wherein the heating time is 2-4h, and the air flow is 1 m3Finishing the coating of the asphalt on the coke and the crosslinking and solidification of the asphalt;
and (4) graphitizing, namely graphitizing the coke powder coated with the asphalt in an Acheson graphitizing furnace at 3000 ℃ to obtain the energy storage graphite cathode material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113526500A (en) * | 2021-07-20 | 2021-10-22 | 安徽科达新材料有限公司 | Preparation method of high-performance artificial graphite negative electrode material |
| CN114538423A (en) * | 2022-03-15 | 2022-05-27 | 上海杉杉科技有限公司 | Artificial graphite material and preparation method and application thereof |
| CN114715887A (en) * | 2022-03-14 | 2022-07-08 | 铜仁学院 | Preparation method of artificial graphite cathode material of lithium ion battery |
| CN115036558A (en) * | 2022-07-04 | 2022-09-09 | 北京大学 | Molten salt electrolyte, preparation method thereof, aluminum-sulfur battery capable of being charged quickly and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113526500A (en) * | 2021-07-20 | 2021-10-22 | 安徽科达新材料有限公司 | Preparation method of high-performance artificial graphite negative electrode material |
| CN114715887A (en) * | 2022-03-14 | 2022-07-08 | 铜仁学院 | Preparation method of artificial graphite cathode material of lithium ion battery |
| CN114538423A (en) * | 2022-03-15 | 2022-05-27 | 上海杉杉科技有限公司 | Artificial graphite material and preparation method and application thereof |
| CN115036558A (en) * | 2022-07-04 | 2022-09-09 | 北京大学 | Molten salt electrolyte, preparation method thereof, aluminum-sulfur battery capable of being charged quickly and application thereof |
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Application publication date: 20210330 |