CN110828888A - All-dry purification method of lithium ion battery anode material and lithium ion battery anode material obtained by purification - Google Patents
All-dry purification method of lithium ion battery anode material and lithium ion battery anode material obtained by purification Download PDFInfo
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- 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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- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention belongs to the technical field of comprehensive utilization of lithium ion battery anode materials, and particularly relates to a full-dry purification method of a lithium ion battery anode material and a lithium ion battery anode material obtained by purification. The method comprises the following steps: 1) heating the crushed materials of the lithium battery anode recycled material at a low temperature until the adhesive fails to work, and obtaining a mixture obtained by separating a current collector from the lithium battery anode material to be purified; 2) carrying out vibration screening on a mixture obtained by separating a current collector and a material to be purified of the positive electrode of the lithium battery to obtain the material to be purified of the positive electrode of the lithium battery from which the current collector is separated; 3) and sintering the material to be purified of the lithium battery anode with the current collector separated off to obtain the purified material of the lithium battery anode. The invention realizes the full dry purification of the lithium ion battery anode material, and the purified lithium ion battery anode material has high purity.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of lithium ion battery anode materials, and particularly relates to a full-dry purification method of a lithium ion battery anode material and a lithium ion battery anode material obtained by purification.
Background
The lithium ion battery industry is rapidly developing, and in 2020, 320 billion dollars are expected to be sold in the world. Its life is about 5-10 years, and it is expected that 50 ten thousand tons of retired batteries will be available in 2020. Materials such as transition metal, lithium, copper, current collectors and the like in the waste lithium ion battery can generate huge economic benefit if being recycled, and can not waste resources and pollute the environment if being directly discarded. Therefore, from the aspects of environmental protection and precious resource recycling, the development of a simple, environment-friendly and strong-operability lithium ion battery recycling method is urgent.
Because the positive electrode material accounts for a large part of the value of the whole battery, the recycling of the retired lithium ion battery is mainly focused on the treatment of the positive electrode piece and the recycling of the positive electrode material.
The existing recycling process of the anode material mainly comprises pyrometallurgy, hydrometallurgy and direct recovery and regeneration. A method for separating a current collector by high-temperature treatment, acid-leaching powder containing a positive electrode material, extracting valuable elements by extraction, and synthesizing a corresponding precursor by blending the ratio has been studied. The purity of the material synthesized by the metallurgical method is high, the main content component accords with the design value, but the original structure of the anode material is damaged, the steps are complex, the energy consumption is high, and the large-scale industrial production is difficult to realize. The technology has the advantages that the cost investment is greatly reduced, the technology has certain practicability, but the technology of flotation impurity removal is adopted, the treatment of waste water and the selection investment of appropriate reagents are still complex.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a full-dry purification method of a lithium ion battery anode material and the lithium ion battery anode material obtained by purification. The repairing method is a full-dry method repairing method, has no wastewater pollution and strong acid/alkali input, has mild treatment temperature compared with pyrometallurgical method, keeps the original structure of the material, is green and energy-saving, has good repeatability, simple process and high efficiency, and has commercial feasibility.
The technical scheme provided by the invention is as follows:
a full dry purification method of a lithium ion battery anode material comprises the following steps:
1) heating the crushed materials of the lithium battery anode recycled material at a low temperature until the adhesive fails to work, and obtaining a mixture obtained by separating a current collector from the lithium battery anode material to be purified;
2) carrying out vibration screening on the current collector obtained in the step 1) and the mixture separated from the material to be purified of the positive electrode of the lithium battery to obtain the material to be purified of the positive electrode of the lithium battery with the current collector separated;
3) sintering the lithium battery positive electrode to-be-purified material with the current collector separated, which is obtained in the step 2), so as to obtain the lithium battery positive electrode purified material.
In the above technical scheme:
in the step 1), the adhesive, such as PVDF, can be pyrolyzed into a pyrolysis intermediate and/or partially carbonized by adopting low-temperature heating treatment, so that the adhesive loses the adhesive capacity;
in the step 2), aluminum or copper of the current collector can be basically separated through vibration screening;
in the step 3), the residual binder pyrolysis intermediate and/or the partially carbonized binder can be completely carbonized through high-temperature sintering, so that the carbon content is reduced.
Based on the technical scheme, the invention realizes the full-dry purification of the lithium ion battery anode material, has no wastewater pollution and strong acid/alkali input in each treatment stage, has mild treatment temperature compared with pyrometallurgy, and can keep the original structure of the material. The purified lithium battery anode material has high purity, the content of impurities such as aluminum and copper is lower than 0.2%, the content of carbon is lower than 0.1%, the content of aluminum is obviously lower than that of a primary high-temperature heat treatment method, the anode material is directly crushed and recovered, and the like.
Specifically, in the step 1), the powder of the lithium battery anode recycling material is as follows:
the method comprises the following steps of (1) processing powder obtained after a pole piece made of a lithium battery positive electrode material fails, for example, the powder obtained after the failed waste pole piece is processed, wherein the processing step can comprise separating a current collector;
alternatively, the powder obtained after processing the leftover materials of the positive electrode materials of the lithium battery, for example, the powder obtained after processing the leftover materials without contacting the electrolyte, and the processing step can comprise separating the current collector.
Specifically, in step 1):
the positive electrode material of the lithium battery is layered LiMeO2Me is Ni, Co or Mn; or the positive electrode material of the lithium battery is olivine-structured LiMePO4Me is Fe or Mn;
the size of the crushed aggregates of the lithium battery positive electrode recycled material is 0.5cm2～100cm2。
Specifically, in the step 2):
the heating rate of the low-temperature heating is 2-10 ℃/min;
the constant temperature section of the low-temperature heating is 300-500 ℃;
the constant temperature duration of the low-temperature heating is 10 min-3 h;
the cooling rate of the low-temperature heating is less than or equal to 10 ℃/min;
the low-temperature heating atmosphere is selected from any one or more of dry air, oxygen, nitrogen or argon; the flow rate is 2.5m3/h～20m3/h。
The above technical solution provides a low temperature heating process condition, and based on the technical solution, the failure of the binder, such as PVDF, can be sufficiently achieved.
Specifically, in the step 2): the screen number of the vibration screening is more than 2 and less than 10, and the vibration screening at least comprises two layers of screens of 50 meshes and 300 meshes; the powder removing time of the vibration screening is 30 s-10 min.
Based on the technical scheme, the current collector and the positive electrode material can be fully separated.
Further, after the vibration screening, the weight percentage of the material to be purified of the lithium battery anode with the separated current collector obtained in the step 2) and the crushed material of the lithium battery anode recycled material in the step 1) is greater than or equal to 95%.
Based on the technical scheme, the high recovery rate of the anode material can be realized.
Specifically, in step 3):
the heating rate of the sintering is as follows: 2 ℃/min to 10 ℃/min;
the sintering temperature is 500-800 ℃;
the constant temperature duration of the sintering is 10 min-3 h;
the temperature reduction rate of the sintering is less than or equal to 10 ℃/min;
the sintering atmosphere is selected from any one or more of dry air, oxygen, nitrogen or argon; the flow rate is 2.5m3/h～20m3/h。
The technical scheme provides the sintering treatment condition, and based on the technical scheme, the residual binder pyrolysis intermediate and/or the partially carbonized binder can be completely carbonized through high-temperature sintering, so that the carbon content is reduced to be lower than 0.1%.
Specifically, the mass content of aluminum in the material to be purified of the lithium battery positive electrode with the separated current collector in the step 2) accounts for less than 0.3% of the total mass of the powder.
The inventor finds that when the aluminum content is less than three thousandth, the material can be coated and superficially doped through the high-temperature effect in the process of lithium supplement, and the cycle performance of the material is improved through the repair.
The invention also provides a lithium battery anode purification material obtained by purification of the lithium battery anode material by the full-dry purification method.
The lithium battery anode purified material obtained by purification provided by the invention has high purity, the content of impurities such as aluminum and copper is lower than 0.2%, the content of carbon is lower than 0.1%, the content of aluminum is obviously lower than that of a primary high-temperature heat treatment method, the method of directly crushing and recovering the anode material and the like is adopted, and the original structure of the material is kept.
Advantages and positive effects of the invention
1) The invention provides a method for recovering and purifying a lithium ion battery anode material, which is characterized in that the recovery rate of the anode material is not lower than 95%, the contents of impurities such as aluminum and copper are lower than 0.2%, and the carbon content is lower than 0.1% on the premise of not damaging the original structure of the anode material. The recovery process is simple, does not need waste water treatment, and the tail gas innocent treatment is environment-friendly.
2) Compared with the method of one-time high-temperature heat treatment method, direct crushing and recycling of the cathode material and the like, the method reduces the Al impurity to be lower than 0.3%.
3) Compared with the flotation and magnetic separation method, no liquid waste is introduced; compared with the method for removing carbon by a primary combustion method, the reduction of energy consumption is more than 10 percent, and meanwhile, the Li loss in the high-temperature sintering process is avoided, and the irreversible change of the structure of the anode material caused by continuous high temperature is relieved.
Drawings
Fig. 1 is an SEM image of the lithium battery positive electrode recycled material after the low temperature spent binder in example 1 of the present invention.
FIG. 2 is an SEM image of a lithium battery cathode recycled material after sintering and impurity removal in example 1 of the present invention.
FIG. 3 is an XRD diagram of a lithium battery cathode recycled material after sintering and impurity removal in example 1 of the present invention.
FIG. 4 is an optical photograph of the separated powder in example 2 of the present invention.
FIG. 5 is an SEM photograph of the delaminated powder and the powder after the secondary sintering in example 2 of the present invention.
FIG. 6 is an SEM photograph of a stripping powder and a high-temperature impurity-removed powder in example 3 of the present invention.
FIG. 7 is a test chart of electrochemical properties of the purified material repairing material of comparative example 1 of the present invention and a comparative repairing material.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
1) The positive plate obtained from the soft package of the retired 523 was cut into 2cm by 2cm size per pot (330 by 100 mm) by a shearing machine3) And (5) filling into 4 bowls.
2) In a dry air atmosphere (5 m)3H), 3 ℃/min heating rate, and pyrolyzing the anode plate under the conditions of 400 ℃/0.5 h.
3) And (3) carrying out ultrasonic vibration screening to separate the powder from the aluminum foil, wherein the mesh number of the screen is 50 meshes and 300 meshes. The powder below 300 meshes is collected for high-temperature impurity removal, the recovery rate is 98.5 percent and is more than 95 percent, and the separation is considered to be complete. Since the aluminum foil was hardly oxidized and pulverized and PVDF was substantially ineffective, the 50 mesh screen was almost clean aluminum foil with 0.13% aluminum impurity in the powder.
4) And (4) removing impurities at high temperature. The loading amount was 4 kg/beaker (330X 100 mm)3) (ii) a Sintering at 600 ℃ for 1h in a dry air atmosphere, and sieving with a 300-mesh sieve to obtain a purified material 1.
The purified material 1 was characterized:
the 523 material is 2-time balls and is large balls formed by agglomeration of small balls, and if the large balls are subjected to cycle test and/or mechanical crushing conditions are not proper, excessive crushing is formed, so that the secondary balls are cracked and crushed. As shown in figure 1, the particle surface of the lithium battery positive electrode recycled material after low-temperature failure of the binder is clean, no obvious breakage is seen, and the secondary sphere structure is well maintained.
As shown in FIG. 2, the surface of the particles of the purified material 1 obtained after sintering and impurity removal was clean and no significant breakage was observed.
As shown in fig. 3, the XRD spectrum of the purified material 1 obtained after sintering and removing impurities shows that there are no other angle impurity peaks on the XRD spectrum except the peak of the ternary layered structure, which indicates that there are no impurity phases and the material is a layered structure; the intensity ratio of 003 peak/104 peak of the material is large, which indicates that the ion mixing is small; a low degree of cleavage between 106 and 012, a low degree of cleavage between 018 and 110, indicating a good layered structure; no miscellaneous phase is generated in the whole body, and the layered structure is complete; the component characterization result shows that the content of Al is 0.13%, the content of C is 0.09%, and the content of impurities is low.
The component contents of the purified material 1 are shown in table 1:
TABLE 1
Example 2
1) Cutting the leftover materials of the lithium iron phosphate positive plate into the size of 10cm by a shearing machine, and filling 100g of the leftover materials into a crucible.
2) And pyrolyzing the anode plate under the conditions of high-purity nitrogen atmosphere (1.6L/min), heating rate of 3 ℃/min and 500 ℃/0.5 h.
3) The powder was separated from the aluminum foil by hand tapping, the separated powder was agglomerated into a sheet, as shown in FIG. 4, and the sheet was ground and sieved through a 300 mesh sieve. Collecting powder below 300 meshes for high-temperature impurity removal, wherein the recovery rate is 99% and is more than 95%, and the separation is considered to be complete.
4) And (4) removing impurities at high temperature. The bowl loading amount is 1cm in depth; sintering at 650 ℃ for 1h in a high-purity nitrogen atmosphere, and sieving with a 300-mesh sieve to obtain the purified material 2.
SEM representation is carried out on the powder obtained by stripping and the powder obtained after secondary sintering, the representation result is shown in figure 5, and the result shows that after secondary sintering, impurities such as carbon tubes and the like and adhesives on the surface of the material are almost completely removed, which shows that the impurity removal according to the scheme is effective.
Example 3
1) The 523 leftover positive plate was cut into 2cm by 2cm size by a shear in 2 kg/bowl (330 x 100 mm)3) And (5) filling into 4 bowls.
2) In a dry air atmosphere (3 m)3H), 5 ℃/min heating rate, and pyrolyzing the anode plate under the conditions of 400 ℃/2 h.
3) And (3) carrying out ultrasonic vibration screening to separate the powder from the aluminum foil, wherein the mesh number of the screen is 50 meshes and 300 meshes. Collecting powder below 300 meshes for high-temperature impurity removal, wherein the recovery rate is more than 95%, and the separation is considered to be complete. Since the aluminum foil was hardly pulverized by oxidation and PVDF was substantially ineffective, the 50 mesh screen was almost clean aluminum foil with 0.216% aluminum impurity in the powder.
4) And (4) removing impurities at high temperature. The loading amount was 1 kg/beaker (330X 100 mm)3) (ii) a Sintering at 600 ℃ for 0.5h in a dry air atmosphere, and sieving with a 300-mesh sieve to obtain a purified material 3.
SEM images of the stripping powder and the high-temperature impurity removal powder are shown in FIG. 6, and the results show that the impurity removal according to the scheme is effective, the surface of the material after impurity removal is clean, and no significant appearance change exists.
Comparative example 1
The purified material 3 obtained in example 3 was added with aluminum oxyhydroxide until the content of aluminum reached 1%, to obtain a comparative material 1.
And (3) respectively carrying out lithium supplement and crystal form recovery on the purified material 3 and the comparative material 1 by adopting the same repair method of dry lithium supplement, namely uniformly mixing the purified material 3, the lithium carbonate/comparative material 1, the aluminum oxyhydroxide and the lithium carbonate according to the proportion of Li/Me 1.05 until white spots do not exist, and sintering at 810 ℃ according to the same conditions to obtain the purified material repair material 3 and the comparative repair material 1.
And carrying out cycle test on the obtained purified material repairing material and the comparative repairing material to manufacture the battery.
The test conditions were: taking the positive electrode powder: adhesive: conductive agent 8: 1: 1, preparing slurry, preparing a 2025 type button half cell, and carrying out electrochemical performance test to obtain a test result shown in fig. 7, wherein the test result comprises a comparison material and a repair material from top to bottom. It can be seen that the constant current charging ratio of the purified material repairing material in the first week of charging and discharging is about 99.5%: the constant voltage charging ratio is about 0.5%; the comparison shows that when the Al content is 1%, the impedance of the material is significantly increased, which is not favorable for the performance of the multiplying power/cycle performance of the material.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. A full dry purification method for a lithium ion battery anode material is characterized by comprising the following steps:
1) heating the crushed materials of the lithium battery anode recycled material at a low temperature until the adhesive fails to work, and obtaining a mixture obtained by separating a current collector from the lithium battery anode material to be purified;
2) carrying out vibration screening on the current collector obtained in the step 1) and the mixture separated from the material to be purified of the positive electrode of the lithium battery to obtain the material to be purified of the positive electrode of the lithium battery with the current collector separated;
3) sintering the lithium battery positive electrode to-be-purified material with the current collector separated, which is obtained in the step 2), so as to obtain the lithium battery positive electrode purified material.
2. The all-dry purification method for the lithium ion battery positive electrode material according to claim 1, characterized in that: in the step 1), the powder of the lithium battery positive electrode recycling material is obtained by processing a pole piece made of the lithium battery positive electrode material after failure, or is obtained by processing leftover materials of the lithium battery positive electrode material.
3. The all-dry purification method for the lithium ion battery positive electrode material according to claim 2, characterized in that in step 1):
the positive electrode material of the lithium battery is layered LiMeO2Me is Ni, Co or Mn; or the positive electrode material of the lithium battery is olivine-structured LiMePO4Me is Fe or Mn;
the size of the crushed aggregates of the lithium battery positive electrode recycled material is 0.5cm2～100cm2。
4. The all-dry purification method for the lithium ion battery positive electrode material according to claim 1, characterized in that in step 1):
the heating rate of the low-temperature heating is 2-10 ℃/min;
the constant temperature section of the low-temperature heating is 300-500 ℃;
the constant temperature duration of the low-temperature heating is 10 min-3 h;
the cooling rate of the low-temperature heating is less than or equal to 10 ℃/min;
the low-temperature heating atmosphere is selected from any one of dry air, oxygen, nitrogen or argonA mixture of one or more; the flow rate is 2.5m3/h～20m3/h。
5. The all-dry purification method for the lithium ion battery positive electrode material according to claim 1, wherein in the step 2): the screen number of the vibration screening is more than 2 and less than 10, and the vibration screening at least comprises two layers of screens of 50 meshes and 300 meshes; the powder removing time of the vibration screening is 30 s-10 min.
6. The all-dry purification method for the lithium ion battery positive electrode material according to claim 5, characterized in that: after vibration screening, the weight percentage of the material to be purified of the lithium battery anode with the separated current collector obtained in the step 2) and the crushed material of the lithium battery anode recycled material in the step 1) is greater than or equal to 95%.
7. The all-dry purification method for the lithium ion battery positive electrode material according to claim 1, wherein in the step 3):
the heating rate of the sintering is as follows: 2 ℃/min to 10 ℃/min;
the sintering temperature is 500-800 ℃;
the constant temperature duration of the sintering is 10 min-3 h;
the temperature reduction rate of the sintering is less than or equal to 10 ℃/min;
the sintering atmosphere is selected from any one or more of dry air, oxygen, nitrogen or argon; the flow rate is 2.5m3/h～20m3/h。
8. The all-dry purification method for the lithium ion battery positive electrode material according to any one of claims 1 to 7, characterized in that: the mass content of aluminum in the material to be purified of the lithium battery positive electrode with the separated current collector in the step 2) accounts for less than 0.3 percent of the total mass of the powder.
9. The lithium battery positive electrode purified material obtained by the full dry purification method of the lithium ion battery positive electrode material according to any one of claims 1 to 8.
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| CN112151902A (en) * | 2020-08-20 | 2020-12-29 | 昆明理工大学 | Method for quickly separating electrode material from current collector and utilizing electrode material and current collector in high-value mode |
| CN112225191A (en) * | 2020-10-09 | 2021-01-15 | 武汉瑞科美新能源有限责任公司 | Method for degrading PVDF in positive electrode of waste lithium iron phosphate battery |
| CN113948787A (en) * | 2021-10-15 | 2022-01-18 | 广东瑞科美电源技术有限公司 | Recycling and regenerating method and application of retired cobalt acid lithium battery and anode material |
| CN113948786A (en) * | 2021-10-15 | 2022-01-18 | 广东瑞科美电源技术有限公司 | Method for recovering and regenerating lithium cobaltate in lithium ion battery, application and positive electrode material |
| CN114068909A (en) * | 2021-11-10 | 2022-02-18 | 中南大学 | Method for regenerating NCMA (non-volatile memory MA) cathode material from retired NCM cathode material |
| CN115636410A (en) * | 2022-09-21 | 2023-01-24 | 安徽清能碳再生科技有限公司 | Intelligent control system of lithium battery negative electrode waste recycling and regenerating reaction system |
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| CN112151902A (en) * | 2020-08-20 | 2020-12-29 | 昆明理工大学 | Method for quickly separating electrode material from current collector and utilizing electrode material and current collector in high-value mode |
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| CN113948786B (en) * | 2021-10-15 | 2023-07-25 | 广东瑞科美电源技术有限公司 | Method for recovering and regenerating lithium cobalt oxide in lithium ion battery, application and positive electrode material |
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