CN115954572A - Regeneration method of graphite negative electrode of lithium battery - Google Patents
Regeneration method of graphite negative electrode of lithium battery Download PDFInfo
- Publication number
- CN115954572A CN115954572A CN202211708095.3A CN202211708095A CN115954572A CN 115954572 A CN115954572 A CN 115954572A CN 202211708095 A CN202211708095 A CN 202211708095A CN 115954572 A CN115954572 A CN 115954572A
- Authority
- CN
- China
- Prior art keywords
- graphite
- lithium battery
- negative electrode
- graphite negative
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The application relates to a lithium battery graphite negative electrode regeneration method, which comprises the following steps: s1: drying and screening the recovered waste graphite negative electrode powder of the lithium battery; s2: roasting graphite powder at 550 ℃ in the air atmosphere, and keeping the temperature for 3h for high-temperature oxidation; s3: mixing and reacting the oxidized graphite with inorganic acid according to a liquid-solid ratio (mass ratio) of 5-10; s4: dissolving a carbon source in an organic solvent, and controlling the liquid-solid ratio (mass ratio) of the organic solvent to the carbon source to be 5-10; s5: and carrying out liquid phase coating on the graphite powder, and graphitizing under an inert atmosphere to obtain the regenerated graphite cathode. The method has the effects of high efficiency, high cost performance, no pollution and environmental protection.
Description
Technical Field
The application relates to the technical field of waste lithium battery recovery, in particular to a regeneration method of a graphite cathode of a lithium battery.
Background
The lithium battery has the advantages of high energy density, high output voltage, good cycle performance and the like, is widely applied, can be seen in the body shadow of electric vehicles, portable electronic products, large power supplies and other fields, and generally consists of a shell, a positive electrode material, a negative electrode material, an Al/Cu current collector, a diaphragm, electrolyte and the like. At present, the treatment mode of the waste lithium battery is mainly focused on the positive electrode noble metal material, the negative electrode material as the battery constitutes four raw materials accounting for 30-40% of the weight of the battery, and the graphite is very suitable for the insertion and the extraction of lithium ions in the charging and discharging process due to the characteristics of good conductivity, high degree of crystallization, good layered structure and the like, so the graphite becomes the most widely applied negative electrode material at present.
At present, two types of lithium battery recovery processing methods mainly comprise a fire method processing technology and an alkaline-acid method processing technology. The fire method treatment process mainly comprises the following steps: (1) In the patent (CN 105642649), metal aluminum, iron, copper, nickel, manganese, cobalt and lithium are fully volatilized in the form of oxides by adopting ultrahigh-temperature (2600-2800 ℃) roasting to obtain graphitized materials, but the method has high energy consumption and has great requirements on equipment; (2) publication No. 107555425A; crushing and grinding the microcrystalline graphite ore to a granularity of 100 meshes to 200 meshes, and placing the crushed microcrystalline graphite ore under a muffle furnace at 500-1000 ℃ for heat treatment for a period of time; mixing the minerals after heat treatment with an alkali solution, carrying out pressurized alkali leaching under the conditions that the ore pulp liquid-solid ratio is 10-12, the temperature is 100-110 ℃ and the reaction time is 2-3 h, and washing and drying leached residues to obtain filter residues after alkali leaching; adding a certain amount of acid into the obtained alkaline leaching residue for mixing, carrying out normal pressure acid leaching under the conditions that the pulp liquid-solid ratio is 10-12, the temperature is 110-120 ℃, and the reaction time is 2-3 h, and washing and drying the leaching residue to obtain a graphite product with the fixed carbon content of more than 98%.
However, this method has many disadvantages, and the method is a means of wet leaching the anode scrap by high-pressure alkaline leaching and atmospheric-pressure acid leaching to increase the fixed carbon content to 98%. However, the method only treats the waste cathode carbon materials into harmless waste residues, and cannot really realize resource recycling, so that how to reasonably recycle the lithium battery is a problem to be solved urgently.
Disclosure of Invention
In order to realize high-value conversion of the retired lithium battery and avoid the influence of waste on the environment, the application provides a regeneration method of a graphite cathode of the lithium battery.
The regeneration method for the graphite cathode of the lithium battery adopts the following technical scheme:
a regeneration method of a graphite negative electrode of a lithium battery comprises the following steps:
s1: drying and screening the recovered waste graphite negative electrode powder of the lithium battery;
s2: roasting graphite powder at 550 ℃ in the air atmosphere, and keeping the temperature for 3h for high-temperature oxidation;
s3: mixing and reacting the oxidized graphite with inorganic acid according to a liquid-solid ratio (mass ratio) of 5-10;
s4: dissolving a carbon source in an organic solvent, and controlling the liquid-solid ratio (mass ratio) of the organic solvent to the carbon source to be 5-10;
s5: and carrying out liquid phase coating on the graphite powder, and graphitizing under an inert atmosphere to obtain the regenerated graphite cathode.
Preferably: in S1, the particle size of the screened graphite negative electrode powder is less than or equal to 75um.
Preferably: in the S2, the roasting temperature is 500-700 ℃, and the roasting time is 2-4h.
Preferably: in S3, the inorganic acid includes any one or a combination of sulfuric acid, nitric acid, hydrofluoric acid, and hydrochloric acid.
Preferably: in S4, the carbon source includes any one or a combination of asphalt, glucose, polytetrafluoroethylene, or polyacrylonitrile.
Preferably: in S4, the organic solvent includes any one or a combination of chloroform, dichloromethane, toluene, carbon disulfide, tetrahydrofuran, tetrachloromethane, and petroleum ether.
Preferably: in S4, the ratio of the carbon source to the graphite powder is 3% -7% during coating modification of the carbon source.
Preferably: in S4, the inert atmosphere includes any one or a combination of helium, argon, and nitrogen.
Preferably: in the S5, the graphitization temperature is 2500-3000 ℃, and the heat preservation time is 2-5h.
In summary, the present application includes the following beneficial technical effects of at least one method for regenerating a graphite negative electrode of a lithium battery:
1. the method adopts air to carry out high-temperature oxidation on the waste graphite, has low cost and good effect, and solves the problem of environmental pollution caused by waste lithium batteries;
2. the organic acid adopted by the invention can effectively remove the metal impurities in the waste graphite powder of the lithium battery, and completely reaches the content standard of the metal impurities in the regenerated graphite;
3. according to the invention, the high solubility of asphalt in organic solvent tetrahydrofuran is utilized, the asphalt can be more uniformly coated on the surface of graphite through liquid phase coating, and then high-temperature graphitization is carried out to make up for the defects of large specific surface area, low first charge-discharge efficiency and low first coulombic efficiency that the surface of the recovered waste graphite is bare;
4. the regenerated graphite electrode material prepared by the method disclosed by the invention has the advantages of good rate capability, low first charge-discharge efficiency, low first coulombic efficiency and the like, and realizes high-value conversion of the retired lithium battery cathode material.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. It should be apparent that the described embodiments are only some of the 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 described embodiments of the application without any inventive step, are within the scope of protection of the application.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this application belongs. The use of the terms "a" or "an" and the like in the description and in the claims of the present application do not denote a limitation of quantity, but rather denote the presence of at least one.
The embodiment of the application discloses a regeneration method of a graphite negative electrode of a lithium battery.
Specifically, the regeneration method of the graphite negative electrode of the lithium battery comprises the following steps:
s1: and drying the recovered waste graphite cathode powder of the lithium battery for 2 hours in a drying oven at 90 ℃, and screening by using a 200-mesh screen. Drying, sieving, and sieving to obtain graphite negative electrode powder with particle size less than or equal to 75um;
s2: roasting graphite powder at 550 ℃ in the air atmosphere, and keeping the temperature for 3h for high-temperature oxidation, wherein the roasting temperature is 500-700 ℃, and the roasting time is 2-4h;
s3: mixing the oxidized graphite and inorganic acid according to a liquid-solid ratio (mass ratio) of 5-10;
s4: dissolving a carbon source in an organic solvent, and controlling the liquid-solid ratio (mass ratio) of the organic solvent to the carbon source to be 5-10, wherein the carbon source comprises any one or combination of asphalt, glucose, polytetrafluoroethylene or polyacrylonitrile; the organic solvent comprises any one or combination of trichloromethane, dichloromethane, toluene, carbon disulfide, tetrahydrofuran, tetrachloromethane and petroleum ether; the ratio of the carbon source to the graphite powder is 3-7% during carbon source coating modification; the inert atmosphere comprises any one or combination of helium, argon and nitrogen;
s5: carrying out liquid phase coating on graphite powder, and graphitizing under an inert atmosphere to obtain a regenerated graphite cathode; wherein the graphitization temperature is 2500-3000 ℃, and the heat preservation time is 2-5h.
Example 1:
s1: and drying the recovered waste graphite cathode powder of the lithium battery in a drying oven at 90 ℃ for 2h, and screening by using a 200-mesh screen. The granularity of the screened graphite cathode powder is less than or equal to 75um;
s2: carrying out high-temperature oxidation on graphite powder at 550 ℃ in the air atmosphere and keeping the temperature for 3h, wherein the roasting temperature is 500-700 ℃, the roasting time is 2-4h, and the loss on ignition of the graphite powder is 10% so as to remove the conductive agent, the binder and the thickening agent and form a uniform oxide layer on the surface of carbon;
s3: mixing the oxidized graphite and hydrofluoric acid according to a liquid-solid ratio (mass ratio) of 5 for reaction for 2h, filtering, washing twice according to the liquid-solid ratio (mass ratio) of 5: fe is less than or equal to 30ppm, zn is less than or equal to 5ppm, cr is less than or equal to 5ppm, ni is less than or equal to 5ppm, cu is less than or equal to 5ppm, al is less than or equal to 5ppm;
s4: dissolving asphalt in a tetrahydrofuran organic solvent according to a liquid-solid ratio of 5;
s5: the method comprises the following steps of performing 5% asphalt liquid phase coating on graphite powder, performing heat preservation for 4 hours at 2800 ℃ under the inert atmosphere of argon to graphitize the graphite powder to obtain regenerated graphite, and detecting that the tap density of the graphitized graphite is 1.04g/ml, the first discharge specific capacity is 353.08 mA.h.g < -1 >, and the first coulombic efficiency is 93.5%, so that the method meets the product standard of GB/T24332019 graphite cathode materials of lithium ion batteries, and achieves the aim of repairing and regenerating the waste graphite of lithium batteries.
Example 2:
s1: and drying the recovered waste graphite cathode powder of the lithium battery in a drying oven at 90 ℃ for 2h, and screening by using a 200-mesh screen. The granularity of the screened graphite cathode powder is less than or equal to 75um;
s2: carrying out high-temperature oxidation on graphite powder at 600 ℃ for 3h in an air atmosphere, wherein the roasting temperature is 500-700 ℃, the roasting time is 2-4h, and the loss on ignition of the graphite powder is 17% so as to remove the conductive agent, the binder and the thickening agent and form a uniform oxide layer on the surface of carbon;
s3: mixing the oxidized graphite and hydrofluoric acid according to a liquid-solid ratio (mass ratio) of 5 for reaction for 2h, filtering, washing twice according to the liquid-solid ratio (mass ratio) of 5: fe is less than or equal to 30ppm, zn is less than or equal to 5ppm, cr is less than or equal to 5ppm, ni is less than or equal to 5ppm, cu is less than or equal to 5ppm, al is less than or equal to 5ppm;
s4: dissolving asphalt in a tetrahydrofuran organic solvent according to a liquid-solid ratio of 5;
s5: the method comprises the steps of performing 5% asphalt liquid phase coating on graphite powder, performing heat preservation for 4 hours at 2800 ℃ under argon inert atmosphere to graphitize the graphite powder to obtain regenerated graphite, wherein detection shows that the tap density of the graphitized graphite is 1.02g/ml, the first discharge specific capacity is 355.60 mA.h.g < -1 >, and the first coulombic efficiency is 94.6%, so that the product standard of GB/T243333-2019 graphite cathode materials of lithium ion batteries is met, and the aim of repairing and regenerating the waste graphite of lithium batteries is fulfilled.
Example 3:
s1: and drying the recovered waste graphite cathode powder of the lithium battery for 2 hours in a drying oven at 90 ℃, and screening by using a 200-mesh screen. The granularity of the screened graphite cathode powder is less than or equal to 75um;
s2: carrying out 550 ℃ heat preservation on graphite powder for 3h at the air atmosphere for high-temperature oxidation, wherein the roasting temperature is 500-700 ℃, the roasting time is 2-4h, and the loss on ignition of the graphite powder is 10% so as to remove the conductive agent, the binder and the thickening agent and form a uniform oxide layer on the surface of carbon;
s3: mixing the oxidized graphite and hydrofluoric acid according to a liquid-solid ratio (mass ratio) of 5 for reaction for 2h, filtering, washing twice according to the liquid-solid ratio (mass ratio) of 5: fe is less than or equal to 30ppm, zn is less than or equal to 5ppm, cr is less than or equal to 5ppm, ni is less than or equal to 5ppm, cu is less than or equal to 5ppm, al is less than or equal to 5ppm;
s4: dissolving asphalt in a tetrahydrofuran organic solvent according to a liquid-solid ratio of 10;
s5: the method comprises the following steps of performing 5% asphalt liquid phase coating on graphite powder, performing heat preservation for 4 hours at 2800 ℃ under the inert atmosphere of argon to graphitize the graphite powder to obtain regenerated graphite, and detecting that the tap density of the graphitized graphite is 1.03g/ml, the first discharge specific capacity is 355.87 mA.h.g < -1 >, and the first coulombic efficiency is 95.1%, so that the method meets the product standard of GB/T24332019 graphite cathode materials of lithium ion batteries, and achieves the aim of repairing and regenerating the waste graphite of lithium batteries.
Example 4:
s1: and drying the recovered waste graphite cathode powder of the lithium battery for 2 hours in a drying oven at 90 ℃, and screening by using a 200-mesh screen. The granularity of the screened graphite cathode powder is less than or equal to 75um;
s2: carrying out high-temperature oxidation on graphite powder at 600 ℃ for 3h in an air atmosphere, wherein the roasting temperature is 500-700 ℃, the roasting time is 2-4h, and the loss on ignition of the graphite powder is 17% so as to remove the conductive agent, the binder and the thickening agent and form a uniform oxide layer on the surface of carbon;
s3: mixing the oxidized graphite and hydrofluoric acid according to a liquid-solid ratio (mass ratio) of 5 for reaction for 2h, filtering, washing twice according to the liquid-solid ratio (mass ratio) of 5: fe is less than or equal to 30ppm, zn is less than or equal to 5ppm, cr is less than or equal to 5ppm, ni is less than or equal to 5ppm, cu is less than or equal to 5ppm, al is less than or equal to 5ppm;
s4: dissolving asphalt in a tetrahydrofuran organic solvent according to a liquid-solid ratio of 5;
s5: the method comprises the steps of carrying out 7% asphalt liquid phase coating on graphite powder, carrying out heat preservation for 4 hours at 2800 ℃ under argon inert atmosphere to graphitize to obtain regenerated graphite, and detecting that the tap density of the graphitized regenerated graphite is 1.01g/ml, the first discharge specific capacity is 356.1 mA.h.g < -1 >, and the first coulombic efficiency is 95.42%, so that the product standard of GB/T243333-2019 graphite cathode materials of lithium ion batteries is met, and the aim of repairing and regenerating the waste graphite of lithium batteries is fulfilled.
Example 5:
s1: and drying the recovered waste graphite cathode powder of the lithium battery in a drying oven at 90 ℃ for 2h, and screening by using a 200-mesh screen. The granularity of the screened graphite cathode powder is less than or equal to 75um;
s2: carrying out high-temperature oxidation on graphite powder at 600 ℃ for 3h in an air atmosphere, wherein the roasting temperature is 500-700 ℃, the roasting time is 2-4h, and the loss on ignition of the graphite powder is 17% so as to remove the conductive agent, the binder and the thickening agent and form a uniform oxide layer on the surface of carbon;
s3: mixing the oxidized graphite and hydrofluoric acid according to a liquid-solid ratio (mass ratio) of 10 for reaction for 2h, filtering, washing twice according to a liquid-solid ratio (mass ratio) of 5: fe is less than or equal to 30ppm, zn is less than or equal to 5ppm, cr is less than or equal to 5ppm, ni is less than or equal to 5ppm, cu is less than or equal to 5ppm, al is less than or equal to 5ppm;
s4: dissolving asphalt in a tetrahydrofuran organic solvent according to a liquid-solid ratio of 5;
s5: the method comprises the following steps of carrying out 7% asphalt liquid phase coating on graphite powder, carrying out heat preservation for 4 hours at 2800 ℃ under the inert atmosphere of argon to graphitize the graphite powder to obtain regenerated graphite, and detecting that the tap density of the graphitized graphite is 1.01g/ml, the first discharge specific capacity is 355.8 mA.h.g < -1 >, and the first coulombic efficiency is 94.36%, so that the product standard of GB/T243358-2019 graphite cathode materials of lithium ion batteries is met, and the aim of repairing and regenerating the waste graphite of lithium batteries is fulfilled.
The above are preferred embodiments of the present application, and the scope of protection of the present application is not limited thereto, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (9)
1. A lithium battery graphite negative electrode regeneration method is characterized in that: the method comprises the following steps:
s1: drying and screening the recovered waste graphite negative electrode powder of the lithium battery;
s2: roasting graphite powder at 550 ℃ in the air atmosphere, and keeping the temperature for 3h for high-temperature oxidation;
s3: mixing the oxidized graphite and inorganic acid according to a liquid-solid ratio (mass ratio) of 5-10;
s4: dissolving a carbon source in an organic solvent, and controlling the liquid-solid ratio (mass ratio) of the organic solvent to the carbon source to be 5-10;
s5: and carrying out liquid phase coating on the graphite powder, and graphitizing under an inert atmosphere to obtain the regenerated graphite cathode.
2. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in S1, the particle size of the screened graphite negative electrode powder is less than or equal to 75um.
3. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in the S2, the roasting temperature is 500-700 ℃, and the roasting time is 2-4h.
4. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in S3, the inorganic acid includes any one or a combination of sulfuric acid, nitric acid, hydrofluoric acid, and hydrochloric acid.
5. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in S4, the carbon source includes any one or a combination of asphalt, glucose, polytetrafluoroethylene, or polyacrylonitrile.
6. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in S4, the organic solvent includes any one or a combination of chloroform, dichloromethane, toluene, carbon disulfide, tetrahydrofuran, tetrachloromethane, and petroleum ether.
7. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in S4, the ratio of the carbon source to the graphite powder is 3% -7% during coating modification of the carbon source.
8. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in S4, the inert atmosphere includes any one or a combination of helium, argon, and nitrogen.
9. The method for regenerating a graphite negative electrode of a lithium battery as claimed in claim 1, wherein: in the S5, the graphitization temperature is 2500-3000 ℃, and the heat preservation time is 2-5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211708095.3A CN115954572A (en) | 2022-12-29 | 2022-12-29 | Regeneration method of graphite negative electrode of lithium battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211708095.3A CN115954572A (en) | 2022-12-29 | 2022-12-29 | Regeneration method of graphite negative electrode of lithium battery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115954572A true CN115954572A (en) | 2023-04-11 |
Family
ID=87296773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211708095.3A Pending CN115954572A (en) | 2022-12-29 | 2022-12-29 | Regeneration method of graphite negative electrode of lithium battery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115954572A (en) |
-
2022
- 2022-12-29 CN CN202211708095.3A patent/CN115954572A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111072023B (en) | Method for recycling graphite from scrapped lithium ion battery | |
| CN101710632B (en) | Method for recovering and restoring anode material graphite of waste lithium ion battery | |
| WO2022179292A1 (en) | Method for preparing silicon-carbon composite material using negative electrodes of waste lithium-ion batteries and application | |
| CN112028065B (en) | SiOx-SiC-C/G silicon-carbon composite material and preparation and application thereof | |
| CN112047335B (en) | Combined treatment method for black powder of waste lithium ion battery | |
| CN111430831B (en) | Method for recovering waste lithium ion battery negative electrode material | |
| CN110690519B (en) | Method for recycling lithium ion battery negative electrode material | |
| CN108963265B (en) | Negative current collector for lithium metal battery and preparation method thereof | |
| CN112510281B (en) | Method for recovering all components of waste lithium ion battery | |
| WO2020103140A1 (en) | Biomass-based hard carbon negative electrode material for sodium ion battery, preparation method therefor and use thereof | |
| WO2020103138A1 (en) | Biomass-based functional-group-modified sodium-ion battery anode material, preparing method therefor and use thereof | |
| CN113991082B (en) | Method for preparing silicon-carbon negative electrode material of lithium ion battery by using silica fume | |
| CN113594450B (en) | Preparation method of coal-based artificial graphite cathode material for lithium ion battery | |
| CN114583315A (en) | Method for recycling carbon negative electrode material from waste lithium ion battery | |
| CN114212786A (en) | Method for preparing high-capacity high-rate graphite by taking waste lithium ion battery cathode material as raw material | |
| CN106684367B (en) | Low-temperature petroleum coke negative electrode material coated with nitrogen-containing polymer pyrolytic carbon and preparation method thereof | |
| CN115954572A (en) | Regeneration method of graphite negative electrode of lithium battery | |
| CN114134382A (en) | Preparation method of porous copper-germanium-aluminum-lithium battery negative electrode material | |
| KR100463079B1 (en) | Method for preparation of cathode material of nickel-carbon nanofiber secondary battery using carbon nanofiber | |
| CN113488714B (en) | Method for repairing failed lithium ion battery positive electrode material, regenerated positive electrode material and application | |
| CN116404293B (en) | Waste lithium battery graphite negative electrode recycling method based on oil sludge microwave pyrolysis cladding | |
| CN113285066B (en) | Vanadium phosphate @ carbon/expanded microcrystalline graphite composite negative electrode active material for potassium ion battery and preparation and application thereof | |
| CN111416170B (en) | Method for recycling waste lithium ion battery negative electrode and co-producing conductive agent | |
| CN115602865A (en) | Method for recovering lithium and copper in waste graphite negative electrode and preparing regenerated graphite | |
| CN117623301A (en) | Method for recycling graphite negative electrode of waste lithium ion battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |