CN115960468A - Preparation method of lithium ion negative electrode coating material - Google Patents
Preparation method of lithium ion negative electrode coating material Download PDFInfo
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- CN115960468A CN115960468A CN202310062475.2A CN202310062475A CN115960468A CN 115960468 A CN115960468 A CN 115960468A CN 202310062475 A CN202310062475 A CN 202310062475A CN 115960468 A CN115960468 A CN 115960468A
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- lithium ion
- reaction
- coating material
- negative electrode
- preparation
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- 239000011248 coating agent Substances 0.000 title claims abstract description 23
- 238000000576 coating method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 23
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 230000003197 catalytic effect Effects 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 19
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005977 Ethylene Substances 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004132 cross linking Methods 0.000 claims abstract description 6
- 230000009471 action Effects 0.000 claims abstract description 3
- 238000000605 extraction Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 claims description 3
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- JOXIMZWYDAKGHI-UHFFFAOYSA-N p-toluenesulfonic acid Substances CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 3
- 125000005489 p-toluenesulfonic acid group Chemical group 0.000 claims description 3
- 229920002866 paraformaldehyde Polymers 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 238000002407 reforming Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000012299 nitrogen atmosphere Substances 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 238000004939 coking Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 3
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 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
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to the field of coating materials, and discloses a preparation method of a lithium ion battery cathode coating material. The preparation method comprises the following steps: the ethylene tar and the effective components of the catalytic slurry oil are taken as raw materials, the crosslinking reaction is carried out under the combined action of a catalyst and a crosslinking agent, then oxygen is introduced for oxidation reaction, and the light components of the reaction product are removed to obtain the coating material. Wherein the proportion of ethylene tar in the raw material is 10-40%, and the proportion of catalytic slurry oil as an effective component for extraction is 60-90%. According to the invention, the preparation of the lithium ion negative electrode coating material with low ash content and high carbon residue is realized by optimizing the raw material mixing ratio and the reaction conditions.
Description
Technical Field
The invention relates to the field of coating materials, in particular to a lithium ion negative electrode coating material and other applications.
Background
Graphite materials are widely used as negative electrode materials of lithium ion batteries because of their characteristics of high specific capacity, long-life cycle, low lithium intercalation/deintercalation platform voltage, and the like. However, due to poor compatibility of the graphite electrode and the organic electrolyte, excessive SEI films are generated on the surface of the negative electrode, lithium ions in the electrolyte are consumed, interfacial impedance is greatly increased, electrochemical dynamic barrier is generated, even dissociation and stripping of a graphite layer of a motor occur, the cycle performance and energy density of the lithium ion battery are reduced, and the service life is shortened. In order to avoid the problem, researches are carried out on modification and modification of graphite, wherein the graphite surface is subjected to coating treatment, so that the extensive attention of putting up the shelf for simple and effective process is paid. In the aspect, a layer of amorphous carbon is coated on the surface of graphite, and due to the good compatibility of the amorphous carbon and an organic solvent, the low-voltage platform and the high capacity of a graphite electrode are reserved, the direct contact between the graphite electrode and an electrolyte is avoided, the electrochemical impedance is reduced, and the cycle performance and the rate performance of the lithium ion battery are further improved.
In this regard, the prior art has made many attempts to study a coating material for a lithium ion negative electrode. Patent CN112592734A continuously prepares lithium ion cathode coating material by removing light components from ethylene tar at high temperature and low pressure, but the method has single raw material and low yield. Patent CN109233305A carries out flash separation on the soft asphalt, and then coumarone resin is added to compound to obtain the coated asphalt with the content of quinoline insoluble substances, but the softening point of the coated asphalt prepared by the method is 110-140 ℃, and the reduced softening point can not meet the performance requirement of the high-softening-point coated material.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and improve the preparation method and application of broad-spectrum raw materials and product yield.
In order to achieve the purpose, the invention provides a preparation method, which takes effective components of ethylene tar and catalytic slurry oil as raw materials, carries out cross-linking reaction under the action of a catalyst and a cross-linking agent, and then removes light components to prepare a lithium ion negative electrode coating material; wherein the mass ratio of the ethylene tar in the raw material is 10-40%, and the mass ratio of the catalytic oil slurry as the extracted effective component is 60-90%.
The preparation method comprises the following steps:
(1) Mixing ethylene tar and effective components of catalytic slurry oil according to a proportion, adding a catalyst and a cross-linking agent into a reaction kettle, heating to 240-330 ℃, controlling the reaction pressure to 0.5-2.5MPa, the stirring speed of a reactor to 150-450r/min, and the reaction time to 1-8h;
(2) Then slowly removing the pressure to normal pressure, and selecting the air input quantity of air introduced into the bottom of the reaction kettle to be 0.5-2L/min, the reaction temperature is 240-300 ℃, and the reaction time is 2-6h;
(5) Stopping introducing air and stirring, and then removing light components to obtain the target product.
Preferably, the ethylene tar used has a sulfur content of less than 800ppm and a density of 1040g/ml.
Preferably, the preparation method of the effective components of the catalytic slurry oil comprises the following steps: removing catalyst powder from the catalytic slurry oil through multi-stage filtration, entering a hydro-reforming reactor to select a proper catalyst to remove partial sulfur, integrating partial characteristic components, entering a pressure reduction tower, removing partial light components, keeping substances between 400 and 520 ℃ in the actual flow, entering an extraction tower, removing asphaltene by using carbon five as a solvent, and remaining effective components.
Preferably, the catalyst is p-toluenesulfonic acid, and the crosslinking agent is trioxymethylene and paraformaldehyde according to a mass ratio of 2:3, and (3) preparing a mixture.
Preferably, the amount of the catalyst accounts for 0.5-8% of the total mass ratio of the raw materials, and the amount of the cross-linking agent accounts for 1-12% of the total mass ratio of the raw materials.
Preferably, the reaction kettle in the step (1) is in a nitrogen environment, the rotating speed of a stirring device is 150-450r/min, the reaction temperature is controlled to be 240-320 ℃, the reaction pressure is controlled to be 0.5-2.0MPa, the reaction time is 1-5h, the air input amount of air introduced in the step (2) is selected to be 0.5-2L/min, the stirring rotating speed of the reactor is 200-350r/min, the reaction temperature is 200-300 ℃, the reaction time is 2-6h, the air amount L/total raw material KG =20-100, and the light components are removed in the step (3) by adopting a reasonable method.
The softening point of the prepared lithium ion negative electrode coating material is 180-290 ℃, the toluene insoluble substance is more than 50 percent, the quinoline insoluble substance is less than 1 percent, and the ash content is less than 0.1 percent.
Has the advantages that:
1. the lithium ion negative electrode coating material prepared by the preparation method disclosed by the invention has a softening point of 180-290 ℃, and can meet the performance requirement of a high-softening-point coating material.
2. The invention improves the broad-spectrum property of raw materials and the yield of products.
3. The invention adopts the effective components of the catalytic slurry oil, can effectively improve the coking value and the yield of the lithium ion cathode coating material, can improve the coking value of the product by adding crosslinking, and reduces the oxidation reaction time under the same quality condition; the reaction temperature and the reaction time are controlled, and the quality and the yield of the product are improved.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The preparation method comprises the following steps:
example 1
In the embodiment, the proportion of ethylene tar in the raw material is 40 percent, and the effective component of the catalytic slurry oil is 60 percent; the dosage of the catalyst accounts for 6% of the total mass of the raw materials, and the dosage of the cross-linking agent accounts for 11% of the total mass of the raw materials. The catalyst is p-toluenesulfonic acid, and the cross-linking agent is trioxymethylene and paraformaldehyde according to a mass ratio of 2:3, and (b) preparing a mixture. The reaction kettle in the step (1) is in a nitrogen environment, the rotating speed of a stirring device is 350r/min, the reaction temperature is 320 ℃, the reaction pressure is controlled to be 1.5MPa, the reaction time is 3h, the air input amount of air introduced in the step (2) is selected to be 0.5-2L/min, the stirring rotating speed of a reactor is 350r/min, the reaction temperature is 240 ℃, the reaction time is 3h, the air amount L/total raw material KG =30, and the light components are removed in the step (3) by adopting a reasonable method.
Example 2
In the same way as in example 1, the percentage of ethylene tar in the raw material is 30%, and the effective component of the catalytic slurry oil is 70%.
Example 3
In the same way as in example 1, the raw material contains 20% of ethylene tar and 80% of the effective component of the catalytic slurry oil.
Example 4
In the same way as in example 1, the percentage of ethylene tar in the raw material is 10%, and the effective component of the catalytic slurry oil is 90%.
Example 5
The proportion of ethylene tar in the raw material is 40 percent, and the effective component of the catalytic slurry oil is 60 percent; adding 5% of catalyst and 7% of cross-linking agent, stirring at 280 deg.C for 420r/min, 2.0MPa for 4h; the reaction temperature of the step (2) is 200 ℃, and the reaction time is 2h; stirring device 400r/min, air volume L/raw material volume KG =50, and step (3) adopts reasonable method to remove light component.
Example 6
As in example 5, only the reaction temperature in step (1) was controlled to 240 ℃.
Example 7
As in example 5, only the reaction temperature in step (1) was controlled to 320 ℃.
Example 8
As in example 5, only the reaction pressure in step (1) was controlled to 2.5MPa.
Example 9
As in example 5, only the air amount L/raw material amount KG =80 in step (2) was controlled.
The data show that the coking value and the yield of the lithium ion negative electrode coating material can be effectively improved by the effective components of the catalytic slurry oil; the coking value of the product can be improved by adding crosslinking, and the oxidation reaction time can be reduced under the same quality condition; meanwhile, it can be seen that the higher the reaction temperature of the pre-crosslinking is, the more beneficial the reaction is, the reaction pressure only affects the quality and yield of the product within a certain range; the amount of oxygen introduced affects the yield and also the coking value, from which an equilibrium point has to be found.
In summary, the embodiment of the invention provides a preparation method of a lithium ion battery cathode coating material, which has relatively broad raw material spectrum and the product quality meeting the commercial application requirements.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can make various changes, substitutions and alterations herein without departing from the spirit and scope of the invention.
Claims (9)
1. A preparation method of a lithium ion negative electrode coating material is characterized in that ethylene tar and effective components of catalytic slurry oil are used as raw materials, a crosslinking reaction is carried out under the action of a catalyst and a crosslinking agent, and then light components are removed to prepare the lithium ion negative electrode coating material; wherein the mass ratio of the ethylene tar in the raw material is 10-40%, and the mass ratio of the catalytic oil slurry as the extracted effective component is 60-90%.
2. The method of claim 1, wherein the method of making comprises the steps of:
(1) Mixing ethylene tar and effective components of catalytic slurry oil in proportion, adding a catalyst and a cross-linking agent into a reaction kettle, heating to 240-330 ℃, controlling the reaction pressure to be 0.5-2.5MPa, the stirring speed of the reactor to be 150-450r/min, and the reaction time to be 1-8h.
(2) Slowly removing the pressure to normal pressure, introducing air into the bottom of the reaction kettle at an air inflow rate of 0.5-2L/min, stirring the reactor at a rotating speed of 200-350r/min, reacting at 240-300 ℃ for 2-6h;
(3) Stopping introducing air and stirring, and then removing light components to obtain the target product.
3. The method of claim 1, wherein the ethylene tar used has a sulfur content of less than 800ppm, a density of 1040g/ml and a feed ratio of 10-40%.
4. The method of claim 1, wherein the effective components of the catalytic slurry oil are prepared by: removing catalyst powder from the catalytic slurry oil through multi-stage filtration, entering a hydro-reforming reactor to select a proper catalyst to remove partial sulfur, integrating partial characteristic components, entering a pressure reduction tower, removing partial light components, keeping substances between 400 and 520 ℃ in the actual process, entering an extraction tower, removing asphaltene by using carbon five as a solvent, and taking the rest as effective components, wherein the raw material accounts for 60 to 90 percent.
5. The preparation method according to claim 1, wherein the catalyst is p-toluenesulfonic acid, and the crosslinking agent is trioxymethylene and paraformaldehyde in a mass ratio of 2:3, and (3) preparing a mixture.
6. The method according to claim 1, wherein the catalyst is used in an amount of 0.5 to 8% by mass based on the total mass of the raw materials, and the crosslinking agent is used in an amount of 1 to 12% by mass based on the total mass of the raw materials.
7. The preparation method according to claim 1, wherein nitrogen atmosphere is adopted in the reaction kettle in the step (1), the rotating speed of a stirring device is 150-450r/min, the reaction temperature is controlled between 240-320 ℃, the reaction pressure is controlled between 0.5-2.0MPa, the reaction time is 1-5h, the air input amount of the introduced air in the step (2) is selected from 0.5-2L/min, the stirring rotating speed of a reactor is 200-350r/min, the reaction temperature is 240-300 ℃, the reaction time is 2-6h, the air amount L/total raw material KG =20-100, and the light components are removed in the step (3) by adopting a reasonable method.
8. A lithium ion negative electrode coating material prepared according to the method of claims 1-7.
9. The lithium ion negative electrode coating material of claim 1, wherein the softening point of the lithium ion negative electrode coating material is 180-290 ℃, the toluene insoluble content is more than 50%, the quinoline insoluble content is less than 1%, and the ash content is less than 0.1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310062475.2A CN115960468A (en) | 2023-01-17 | 2023-01-17 | Preparation method of lithium ion negative electrode coating material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310062475.2A CN115960468A (en) | 2023-01-17 | 2023-01-17 | Preparation method of lithium ion negative electrode coating material |
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| CN115960468A true CN115960468A (en) | 2023-04-14 |
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| CN202310062475.2A Pending CN115960468A (en) | 2023-01-17 | 2023-01-17 | Preparation method of lithium ion negative electrode coating material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426852A (en) * | 2022-01-05 | 2022-05-03 | 中国石油化工股份有限公司 | High-softening-point asphalt and preparation method and application thereof |
| CN115093874A (en) * | 2022-07-31 | 2022-09-23 | 中国石油化工股份有限公司 | Preparation method and system of low-quinoline insoluble matter high-softening-point petroleum-based coated asphalt |
| CN115093872A (en) * | 2022-06-22 | 2022-09-23 | 中国石油大学(华东) | Coated asphalt and preparation method and application thereof |
-
2023
- 2023-01-17 CN CN202310062475.2A patent/CN115960468A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426852A (en) * | 2022-01-05 | 2022-05-03 | 中国石油化工股份有限公司 | High-softening-point asphalt and preparation method and application thereof |
| CN115093872A (en) * | 2022-06-22 | 2022-09-23 | 中国石油大学(华东) | Coated asphalt and preparation method and application thereof |
| CN115093874A (en) * | 2022-07-31 | 2022-09-23 | 中国石油化工股份有限公司 | Preparation method and system of low-quinoline insoluble matter high-softening-point petroleum-based coated asphalt |
Non-Patent Citations (1)
| Title |
|---|
| 赵晓隆等: ""催化油浆重质芳烃制备沥青树脂"", 《应用化工》, vol. 44, no. 9, pages 1677 - 1679 * |
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