CN115084695A - Recovery and regeneration process of graphite cathode of lithium ion battery - Google Patents
Recovery and regeneration process of graphite cathode of lithium ion battery Download PDFInfo
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- CN115084695A CN115084695A CN202110272840.3A CN202110272840A CN115084695A CN 115084695 A CN115084695 A CN 115084695A CN 202110272840 A CN202110272840 A CN 202110272840A CN 115084695 A CN115084695 A CN 115084695A
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- 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
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
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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
- 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
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Abstract
The invention relates to a battery material recovery process, in particular to a recovery and regeneration process of a graphite cathode of a lithium ion battery. The process firstly recovers and classifies the negative graphite powder of the scrapped lithium ion battery, and then sequentially performs screening copper removal, low-temperature heat treatment, pulping and kneading, carbonization treatment, screening and demagnetization to prepare the regenerated and repaired graphite material. The process can fully utilize the SEI film on the surface of the discarded graphite, carry out lithium salt repair on the surface of the regenerated graphite, and improve the cycle performance of the regenerated graphite, and the cycle performance of the obtained regenerated graphite is improved by more than 30 percent compared with that of the conventional regenerated graphite.
Description
Technical Field
The invention relates to a recovery process of a battery material, in particular to a recovery and regeneration process of a graphite cathode of a lithium ion battery.
Background
With the increasing use of lithium ion batteries year by year, the recycling of the key materials of the retired lithium ion batteries has quietly formed a new industry.
For the recovery of the graphite cathode of the retired lithium ion battery, the conventional process route comprises recovery, classification, acid liquor copper removal, drying, heat treatment and screening demagnetization. The process is an effective, simple and rough recovery process, copper foil scraps are washed away by liquid phase copper removal, organic matters such as SBR/CMC and the like are decomposed by heat treatment, and residual carbon obtained by pyrolysis and carbon black originally contained in a pole piece can be used as a conductive additive. The process route has the advantages of simple process and easy operation, but has the disadvantage that the process does not pay attention to the SEI film on the graphite surface of the retired and recovered lithium ion battery, which can cause the damage of the graphite surface in the regeneration process and the waste of lithium salt.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a new regeneration process route for the graphite cathode of a decommissioned and recycled lithium ion battery, which fully utilizes an SEI film on the graphite surface of the decommissioned and recycled lithium ion battery and repairs a lithium salt on the surface of the regenerated graphite, and the process route comprises the following steps: recovering, classifying, screening to remove copper, low-temperature heat treatment, pulping and kneading, carbonizing, screening and demagnetizing.
The invention is realized by the following technical scheme:
a recycling and regenerating process of a graphite cathode of a lithium ion battery comprises the following steps:
s1, recovery and classification: recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder;
s2, screening to remove copper: screening the classified graphite powder by using a swing screen, wherein the swing frequency is 200-;
s3, low-temperature heat treatment: carrying out low-temperature heat treatment on the graphite powder subjected to copper removal by screening in the step S2 while heating and stirring, wherein the heating temperature is 120-150 ℃, and the heat treatment time is 30-60 min;
s4, pulping and kneading: mixing the graphite powder subjected to the low-temperature heat treatment in the step S3 with distilled water, heating to 100-120 ℃ for kneading, wherein the kneading speed is 30-50rpm, and the kneading time is 5-8 h;
s5, carbonization: carbonizing the material kneaded in the step S4 in a protective atmosphere at the temperature of 700 ℃ and 900 ℃ for 0.5-2 h;
s6, screening and demagnetizing: and (5) screening and demagnetizing the material carbonized in the step (S5) to obtain the regenerated and repaired graphite material.
Preferably, in step S1, the classified graphite powder has a D50 range of 2 μm or less, ash content of 1% or less, and graphitization degree range of 5% or less.
Preferably, in the step S2, the swing sieve is a plane swing sieve, the screen is rectangular, and the swing amplitude is 5-8% of the length of the screen;
preferably, in step S2, the rocking sieve is divided into two layers, the first layer is 200 mesh sieve, and the second layer is 270 mesh sieve.
Preferably, in step S3, the heating temperature of the low-temperature heat treatment is 150 ℃, and the heat treatment time is 30 min.
Preferably, in the step S3, when the graphite powder from which copper has been removed in the step S2 is subjected to low-temperature heat treatment, the graphite powder is stirred while being heated, and the stirring speed is 10 to 30 rpm.
Preferably, in the step S4, the graphite powder after the low-temperature heat treatment in the step S3 is mixed with distilled water according to a mass ratio of 1 (0.6-2).
Preferably, in the step S4, the graphite powder after the low-temperature heat treatment in the step S3 is mixed with distilled water according to the mass ratio of 1:1, heated to 120 ℃ and kneaded, wherein the kneading speed is 50rpm, and the kneading time is 5 hours.
Preferably, in step S5, the temperature of the carbonization treatment is 700 ℃, and the time of the carbonization treatment is 2 h.
Preferably, in step S5, the protective atmosphere is carbon dioxide.
The invention has the following technical effects:
the conventional lithium ion battery graphite retirement recycling process route is as follows: recovering, classifying, removing copper by acid liquor, drying, heat treating, screening and removing magnetism. The new process route for recycling the lithium ion battery graphite in retired service adopted by the invention is as follows: recovering, classifying, screening to remove copper, low-temperature heat treatment, pulping and kneading, carbonizing, screening and demagnetizing. The innovation points of the novel process are as follows:
(1) the dry method swinging screening copper removal process is adopted, compared with the acid solution copper removal process, the process is simpler and more environment-friendly, and the obtained oversize products can further refine metal copper; in addition, compared with ultrasonic screening and suspension vibration screening, the screening efficiency of the swing screening mode is lower, but the mechanical force in the screening process is soft, the copper foil cannot be crushed into copper scraps, and the copper content can be ensured to be lower than 50ppm (the ash content does not contain lithium salt);
(2) the low-temperature heat treatment process is added, so that the components of the SEI film are complex and difficult to directly utilize, and the thickness of the formed SEI film is uneven due to different circulation times of waste graphite from different sources, so that the low-temperature heat treatment process is added, and the main purpose of the process is to thermally decompose the SEI film into uniform lithium carbonate so as to guarantee the uniformity of lithium salt repair in the later period;
(3) the pulping and kneading process includes dissolving lithium carbonate with distilled water under heating and stirring condition, heating and kneading, and separating lithium carbonate from graphite surface to repair lithium salt surface.
The new process can fully utilize the SEI film on the surface of the discarded graphite and carry out lithium salt repair on the surface of the regenerated graphite, so that the lithium salt in the discarded graphite can be fully utilized, the cycle performance of the regenerated graphite can be improved, and the cycle performance of the obtained regenerated graphite is improved by more than 30% compared with that of the conventional regenerated graphite.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
S1, recovery and classification: recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder; the D50 range of the classified graphite powder is less than or equal to 2 mu m, the ash content is less than or equal to 1 percent, and the graphitization degree range is less than or equal to 5 percent.
S2, screening to remove copper: and screening the classified graphite powder by using a swing screen, wherein the swing screen is a plane swing screen, the screen is rectangular, the swing screen is divided into two layers, the first layer screen is a 200-mesh screen, the second layer screen is a 270-mesh screen, the swing frequency is 200-fold and 500-fold/min, the swing amplitude is 5-8% of the length of the screen, and the copper content in the graphite is controlled within 50ppm by screening and copper removal.
S3, low-temperature heat treatment: and (4) carrying out low-temperature heat treatment on the graphite powder subjected to copper removal by screening in the step S2, heating and stirring at the stirring speed of 10rpm at the heating temperature of 120 ℃, and carrying out heat treatment for 60 min.
S4, pulping and kneading: and (4) mixing the graphite powder subjected to the low-temperature heat treatment in the step (S3) with distilled water according to the mass ratio of 1:1, heating to 120 ℃ for kneading, wherein the kneading speed is 50rpm, and the kneading time is 5 hours, so as to obtain a material subjected to pulping and kneading.
S5, carbonization: and (3) carbonizing the material which is prepared by pulping and kneading in the step (S4), wherein the carbonizing treatment is carried out in a carbon dioxide atmosphere, the temperature of the carbonizing treatment is 700 ℃, and the time of the carbonizing treatment is 0.5 h.
S6, screening and demagnetizing: and (5) screening and demagnetizing the material carbonized in the step (S5) to obtain a sample No. 1.
Example 2
S1, recovery and classification: recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder; the D50 range of the classified graphite powder is less than or equal to 2 mu m, the ash content is less than or equal to 1 percent, and the graphitization degree range is less than or equal to 5 percent.
S2, screening to remove copper: and (4) screening the classified graphite powder by using a swing screen, wherein the swing frequency is 300 times/min, and the copper content in the graphite is controlled within 50ppm by screening and copper removal.
S3, low-temperature heat treatment: and (4) carrying out low-temperature heat treatment on the graphite powder subjected to copper removal by screening in the step S2, heating and stirring at the stirring speed of 20rpm, the heating temperature of 130 ℃, and the heat treatment time of 50 min.
S4, pulping and kneading: mixing the graphite powder subjected to low-temperature heat treatment in the step S3 with distilled water according to the mass ratio of 1: 0.6, heating to 100 ℃ for kneading, wherein the kneading speed is 30rpm, and the kneading time is 8 hours;
s5, carbonization: and (3) carbonizing the material which is prepared by pulping and kneading in the step (S4), wherein the carbonizing treatment is carried out in a carbon dioxide atmosphere, the temperature of the carbonizing treatment is 800 ℃, and the time of the carbonizing treatment is 1.5 h.
S6, screening and demagnetizing: and (5) screening and demagnetizing the material carbonized in the step (S5) to obtain a sample No. 2.
Example 3
S1, recovery and classification: recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder; the D50 range of the classified graphite powder is less than or equal to 2 mu m, the ash content is less than or equal to 1 percent, and the graphitization degree range is less than or equal to 5 percent.
S2, screening to remove copper: and (4) screening the classified graphite powder by using a swing screen, wherein the swing frequency is 500 times/min, and the copper content in the graphite is controlled within 50ppm by screening and copper removal.
S3, low-temperature heat treatment: and (4) carrying out low-temperature heat treatment on the graphite powder subjected to copper removal by screening in the step S2, heating and stirring at the stirring speed of 30rpm at the heating temperature of 150 ℃, and carrying out heat treatment for 30 min.
S4, pulping and kneading: mixing the graphite powder subjected to low-temperature heat treatment in the step S3 with distilled water according to the mass ratio of 1:2, heating to 110 ℃ for kneading, wherein the kneading speed is 40rpm, and the kneading time is 5 hours;
s5, carbonization: carbonizing the material which is prepared by pulping and kneading in the step S4 in a protective atmosphere at 700 ℃ for 2 h; the protective atmosphere is carbon dioxide.
S6, screening and demagnetizing: and (5) screening and demagnetizing the material carbonized in the step (S5) to obtain a sample No. 3.
Example 4
S1, recovery and classification: recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder; the D50 range of the classified graphite powder is less than or equal to 2 mu m, the ash content is less than or equal to 1 percent, and the graphitization degree range is less than or equal to 5 percent.
S2, screening to remove copper: screening the classified graphite powder by using a swing screen, wherein the swing frequency is 400 times/min, and the copper content in the graphite is controlled within 50ppm by screening and copper removing;
s3, low-temperature heat treatment: and (4) carrying out low-temperature heat treatment on the graphite powder subjected to copper removal by screening in the step S2, heating and stirring at the stirring speed of 10rpm at the heating temperature of 150 ℃, and carrying out heat treatment for 30 min.
S4, pulping and kneading: and (3) mixing the graphite powder subjected to the low-temperature heat treatment in the step (S3) with distilled water according to the mass ratio of 1:1, heating to 120 ℃ and kneading, wherein the kneading speed is 50rpm, and the kneading time is 6 hours.
S5, carbonization: and carbonizing the material which is prepared by pulping and kneading in the step S4 in the protective atmosphere of carbon dioxide at 900 ℃ for 0.5 h.
S6, screening and demagnetizing: and (5) screening and demagnetizing the material carbonized in the step (S5) to obtain a sample No. 4.
Comparative example
Recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder; the D50 range of the classified graphite powder is less than or equal to 2 mu m, the ash content is less than or equal to 1 percent, and the graphitization degree range is less than or equal to 5 percent. And removing copper from the classified graphite powder by hydrochloric acid and nitric acid, washing and filtering for multiple times until the filtrate is neutral, drying the filter cake at 120 ℃ to obtain the copper-removed graphite powder, heating the copper-removed graphite powder to 800 ℃ in a nitrogen atmosphere, preserving heat for 1h, and screening and demagnetizing to obtain a comparative example.
The electrochemical performances of the above examples and comparative examples are as follows:
from the above table, it can be seen that: the SEI film of the lithium ion battery graphite is recovered by using retired service, lithium salt surface repair is carried out in the recovery and utilization process, the cycle performance of the obtained negative electrode is obviously superior to that of the conventional regenerated graphite, and the cycle frequency is improved by more than 30%.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that various improvements and modifications within the structure and principle of the present invention can be realized by those skilled in the art, and the protection scope of the present invention should be considered.
Claims (10)
1. A recycling and regenerating process of a graphite cathode of a lithium ion battery is characterized by comprising the following steps:
s1, recovery and classification: recovering negative graphite powder of the scrapped lithium ion battery, and classifying according to particle type, particle size and graphitization degree to obtain classified graphite powder;
s2, screening to remove copper: screening the classified graphite powder by using a swing screen, wherein the swing frequency is 200-;
s3, low-temperature heat treatment: carrying out low-temperature heat treatment on the graphite powder subjected to copper removal by screening in the step S2 while heating and stirring, wherein the heating temperature is 120-150 ℃, and the heat treatment time is 30-60 min;
s4, pulping and kneading: mixing the graphite powder subjected to the low-temperature heat treatment in the step S3 with distilled water, heating to 100-120 ℃ for kneading, wherein the kneading speed is 30-50rpm, and the kneading time is 5-8 h;
s5, carbonization: carbonizing the material kneaded in the step S4 in a protective atmosphere at the temperature of 700 ℃ and 900 ℃ for 0.5-2 h;
s6, screening and demagnetizing: and (5) screening and demagnetizing the material carbonized in the step (S5) to obtain the regenerated and repaired graphite material.
2. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in step S1, the classified graphite powder has a D50 range of not more than 2 μm, an ash content of not more than 1%, and a graphitization degree range of not more than 5%.
3. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in the step S2, the swing sieve is a planar swing sieve, the screen is rectangular, and the swing amplitude is 5-8% of the length of the screen.
4. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in the step S2, the swing sieve is divided into two layers, the first layer of sieve is 200 mesh sieve, and the second layer of sieve is 270 mesh sieve.
5. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in the step S3, the heating temperature of the low-temperature heat treatment is 150 ℃, and the heat treatment time is 30 min.
6. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in the step S3, when the graphite powder from which copper has been removed by the sieving in the step S2 is subjected to low-temperature heat treatment, the graphite powder is stirred while being heated, and the stirring speed is 10 to 30 rpm.
7. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in the step S4, the graphite powder subjected to the low-temperature heat treatment in the step S3 is mixed with distilled water according to the mass ratio of 1 (0.6-2).
8. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in the step S4, the graphite powder subjected to the low-temperature heat treatment in the step S3 and distilled water are mixed according to the mass ratio of 1:1, heated to 120 ℃ and kneaded, wherein the kneading speed is 50rpm, and the kneading time is 5 hours.
9. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in step S5, the temperature of the carbonization treatment was 700 ℃, and the time of the carbonization treatment was 2 hours.
10. The recycling and regenerating process of the graphite negative electrode of the lithium ion battery according to claim 1, characterized in that: in step S5, the protective atmosphere is carbon dioxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115646981A (en) * | 2022-12-22 | 2023-01-31 | 湖南金阳烯碳新材料股份有限公司 | Method for lossless recovery of graphite negative plate of waste lithium ion battery |
| CN115692910A (en) * | 2022-12-28 | 2023-02-03 | 湖南金阳烯碳新材料股份有限公司 | Method for recovering waste negative electrode material of lithium ion battery |
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2021
- 2021-03-13 CN CN202110272840.3A patent/CN115084695A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115646981A (en) * | 2022-12-22 | 2023-01-31 | 湖南金阳烯碳新材料股份有限公司 | Method for lossless recovery of graphite negative plate of waste lithium ion battery |
| CN115646981B (en) * | 2022-12-22 | 2023-03-10 | 湖南金阳烯碳新材料股份有限公司 | Method for lossless recovery of graphite negative plate of waste lithium ion battery |
| CN115692910A (en) * | 2022-12-28 | 2023-02-03 | 湖南金阳烯碳新材料股份有限公司 | Method for recovering waste negative electrode material of lithium ion battery |
| CN115692910B (en) * | 2022-12-28 | 2023-03-03 | 湖南金阳烯碳新材料股份有限公司 | Method for recovering waste negative electrode material of lithium ion battery |
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