CN111285365A - Method for recycling waste negative electrode graphite material in lithium ion battery production process - Google Patents
Method for recycling waste negative electrode graphite material in lithium ion battery production process Download PDFInfo
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- CN111285365A CN111285365A CN201910002283.6A CN201910002283A CN111285365A CN 111285365 A CN111285365 A CN 111285365A CN 201910002283 A CN201910002283 A CN 201910002283A CN 111285365 A CN111285365 A CN 111285365A
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- negative electrode
- graphite material
- lithium ion
- production process
- ion battery
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 invention relates to a method for recycling a waste negative electrode graphite material in a lithium ion battery production process, which comprises the following steps: step one, disassembling a negative electrode graphite material from a waste lithium ion negative electrode plate and screening; secondly, putting the negative electrode graphite material into a jet mill to be ground into graphite powder; step three, performing spheroidization high-temperature treatment on the graphite powder; and step four, screening the graphite powder obtained in the step three, wherein the screened graphite powder is a negative electrode material, so that the process for recycling the waste negative electrode graphite material in the production process of the lithium ion battery is simplified, the process period is shortened, the production efficiency is effectively improved, the interior and the surface of the negative electrode material are modified, and the utilization rate of graphite is improved.
Description
Technical Field
The invention relates to the technical field of recycling of lithium ion batteries, in particular to a method for recycling a waste negative electrode graphite material in a lithium ion battery production process.
Background
Lithium ion secondary batteries are widely used because of their advantages of high voltage, light weight, good safety, no memory effect, long cycle life, no environmental pollution, etc. With the development of the lithium ion battery industry, a large amount of scrapped batteries are produced every year, and the manufacturing process of the negative graphite material has high reaction energy consumption, strict equipment requirements, long production period and limited graphite resources, so that the situation that the supply of the graphite material is not in demand is caused.
The existing process for recovering the negative electrode graphite material generally comprises basic screening, crushing, spherical treatment, purification treatment and screening, acid washing, water washing and drying are required in the purification treatment process, the treatment steps are multiple, the period is long, the cost is high, and the production requirements of the existing enterprises cannot be continuously met.
Disclosure of Invention
In order to solve the problems, the invention provides a method for recycling the waste negative electrode graphite material in the production process of the lithium ion battery, which has the advantages of simple process and short manufacturing period.
In order to achieve the aim, the invention adopts the following technical scheme that the method for recycling the waste cathode graphite material in the production process of the lithium ion battery comprises the following steps:
firstly, disassembling a negative electrode graphite material from waste negative electrode waste sheets generated in the production process of a lithium ion battery and screening;
secondly, putting the negative electrode graphite material into a jet mill to be ground into graphite powder;
step three, performing spheroidization high-temperature treatment on the graphite powder;
and step four, screening the graphite powder obtained in the step three, wherein the screened graphite powder is a negative electrode material.
Preferably, in the third step, the spheroidization high-temperature treatment time is 30 to 40 minutes.
Preferably, in the third step, the temperature of the spheroidization high-temperature treatment is 280-350 ℃.
Preferably, in step two, the median diameter of the graphite powder is 14 ± 2.0 μm.
Preferably, the negative electrode graphite material is an artificial graphite material, a natural graphite material or a composite graphite material.
Preferably, in the second step, the negative electrode graphite material is placed in a crushing chamber of the jet mill, compressed air is injected into the crushing chamber at a high speed through a laval nozzle after being filtered and dried, the negative electrode graphite material is repeatedly collided, rubbed and sheared at the intersection point of a plurality of high-pressure air flows to be crushed, the crushed negative electrode graphite material moves to a classification area along with an ascending air flow under the suction action of a fan, under the action of a strong centrifugal force generated by a classification turbine rotating at a high speed, the thick and thin negative electrode graphite materials are separated, graphite powder meeting the particle size requirement enters a cyclone separator and a dust remover through a classification wheel to be collected, and the coarse stone ink powder falls to the crushing area to be continuously crushed.
The invention has the beneficial effects that: the invention simplifies the recycling process flow of the negative electrode graphite material, shortens the process period, effectively improves the production efficiency, modifies the interior and the surface of the negative electrode material, improves the utilization rate of graphite, effectively removes surface colloid after the graphite powder is treated for a period of time at high temperature by sphericizing, and simultaneously utilizes a shaping machine to remove the surface differential in a grading way, and evaporates and removes volatile matters at high temperature, so that the graphite powder meets the use requirement of the lithium ion negative electrode material, does not need to be purified, and greatly reduces the treatment time of the whole process.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a scanning electron micrograph of graphite.
FIG. 3 is a second drawing of a scanning electron microscope for graphite.
Fig. 4 is a data diagram of capacity test one.
Fig. 5 is a data diagram of capacity test two.
Detailed Description
Referring to fig. 1-3, the present invention relates to a method for recycling waste negative graphite material in the production process of lithium ion battery, comprising the following steps:
step one, disassembling a negative electrode graphite material from a waste lithium ion negative electrode sheet and screening;
secondly, putting the negative electrode graphite material into a jet mill to be milled into graphite powder with the median diameter of 14 +/-2.0 mu m;
the negative electrode graphite material is placed in a crushing chamber of an air flow crusher, compressed air is filtered and dried and then is injected into the crushing chamber at a high speed through a Laval nozzle, the negative electrode graphite material is repeatedly collided, rubbed and sheared at the intersection of a plurality of high-pressure air flows to be crushed, the crushed negative electrode graphite material moves to a classification area along with ascending air flow under the suction action of a fan, under the action of strong centrifugal force generated by a classification turbine rotating at a high speed, the thick negative electrode graphite material and the thin negative electrode graphite material are separated, graphite powder meeting the granularity requirement enters a cyclone separator and a dust remover through a classification wheel to be collected, and the thick graphite particles fall to the crushing area to be continuously crushed.
Step three, performing high-temperature treatment for spheroidizing the graphite powder for 30 minutes to remove colloid attached to the surface, and simultaneously, drawing out the differential of the surface by a shaper in stages, and evaporating and removing volatile matters at the temperature of 300 ℃;
and step four, screening the graphite powder obtained in the step three, wherein the screened graphite powder is a negative electrode material.
Preferably, the negative electrode graphite material is an artificial graphite material, a natural graphite material or a composite graphite material.
The technical indexes of the graphite powder prepared by the invention are as follows:
fixed carbon content (%): not less than 99.50(BT-9300S Baite laser particle size analyzer)
Particle size distribution (μm): d50 ═ 14.0 +/-2.0 (BT-9300S Baite laser particle size analyzer)
Tap density (g/cm 3): not less than 0.90(FZS-4B type automatic tap density meter Beijing Steel research institute)
Specific surface area (m 2/g): not more than 5.0 (dynamic nitrogen adsorption specific surface determinator Jing Weigaobo JW-DX type)
Moisture (%): not more than 0.20 (GB/T3521 + 2008 constant temperature drying oven 110 degree to constant weight)
Discharge capacity (mAh/g): > 340(0.2C/Half cell test)
First discharge efficiency (%): not less than 90(0.2C/Half cell test)
As can be seen from the technical indexes and the figures 4 and 5, the fixed carbon content of the graphite powder recovered and prepared by the method is more than 99.50%, the discharge capacity is more than 340mAh/g, the first discharge efficiency is more than 90%, and the use requirement of the negative electrode material of the lithium ion battery is met.
The invention simplifies the recycling process of the waste cathode graphite material in the production process of the lithium ion battery, effectively removes impurities on the graphite material by increasing the time of spheroidization high-temperature treatment, shortens the whole process period, greatly improves the production efficiency, improves the recycling of the graphite material, does not need to use chemical solvent for acid cleaning, reduces the pollution to the environment,
the above embodiments are merely illustrative of the preferred embodiments of the present invention, and not restrictive, and various changes and modifications to the technical solutions of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are intended to fall within the scope of the present invention defined by the appended claims.
Claims (6)
1. A method for recycling waste negative electrode graphite materials in the production process of lithium ion batteries is characterized by comprising the following steps: the method comprises the following steps:
firstly, disassembling a negative electrode graphite material from waste negative electrode waste sheets generated in the production process of a lithium ion battery and screening;
secondly, putting the negative electrode graphite material into a jet mill to be ground into graphite powder;
step three, performing spheroidization high-temperature treatment on the graphite powder;
and step four, screening the graphite powder obtained in the step three, wherein the screened graphite powder is a negative electrode material.
2. The method for recycling the waste negative electrode graphite material in the production process of the lithium ion battery according to claim 1, is characterized in that: in the third step, the spheroidization high-temperature treatment time is 30-40 minutes.
3. The method for recycling the waste negative electrode graphite material in the production process of the lithium ion battery according to claim 1, is characterized in that: in the third step, the temperature of the spheroidization high-temperature treatment is 280-350 ℃.
4. The method for recycling the waste negative electrode graphite material in the production process of the lithium ion battery according to claim 1, is characterized in that: in the second step, the median diameter of the graphite powder is 14 +/-2.0 μm.
5. The method for recycling the waste negative electrode graphite material in the production process of the lithium ion battery according to claim 1, is characterized in that: the negative electrode graphite material is an artificial graphite material, a natural graphite material or a composite graphite material.
6. The method for recycling the waste negative electrode graphite material in the production process of the lithium ion battery according to claim 1, is characterized in that: in the second step, the negative electrode graphite material is placed in a crushing chamber of an airflow crusher, compressed air is sprayed into the crushing chamber at a high speed through a Laval nozzle after being filtered and dried, the negative electrode graphite material is repeatedly collided, rubbed and sheared at the intersection point of a plurality of high-pressure airflows to be crushed, the crushed negative electrode graphite material moves to a classification area along with an ascending airflow under the suction action of a fan, under the action of a strong centrifugal force generated by a classification turbine rotating at a high speed, the thick and thin negative electrode graphite material is separated, graphite powder meeting the granularity requirement enters a cyclone separator and a dust remover through the classification wheel to be collected, and the coarse stone ink powder falls to the crushing area to be continuously crushed.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112768629A (en) * | 2021-01-15 | 2021-05-07 | 内蒙古恒科新材料科技有限公司 | Method for preparing lithium ion battery negative electrode material by taking waste graphite electrode as raw material |
| CN115043398A (en) * | 2022-06-21 | 2022-09-13 | 广东凯金新能源科技股份有限公司 | Simplified method for preparing lithium ion negative electrode material by utilizing micro-powder raw material |
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| CN105356001A (en) * | 2015-12-14 | 2016-02-24 | 天津理工大学 | Repairing modifying method of cathode waste material of waste lithium ion battery |
| CN106058355A (en) * | 2016-08-15 | 2016-10-26 | 四川兴能新材料有限公司 | Method for recycling lithium titanate electrode slice |
| CN106450545A (en) * | 2016-10-08 | 2017-02-22 | 合肥国轩高科动力能源有限公司 | Recycle method of lithium battery negative electrode material |
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| CN108110364A (en) * | 2017-12-27 | 2018-06-01 | 东莞鑫茂新能源技术有限公司 | A kind of lithium cell cathode material recoverying and utilizing method |
| CN108376807A (en) * | 2018-04-09 | 2018-08-07 | 湖南省正源储能材料与器件研究所 | A kind of waste and old lithium ion battery graphite cathode material restorative procedure |
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2019
- 2019-01-02 CN CN201910002283.6A patent/CN111285365B/en active Active
Patent Citations (7)
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| JP2012195073A (en) * | 2011-03-15 | 2012-10-11 | Mitsui Mining & Smelting Co Ltd | Method for producing recycled material |
| CN105356001A (en) * | 2015-12-14 | 2016-02-24 | 天津理工大学 | Repairing modifying method of cathode waste material of waste lithium ion battery |
| CN106058355A (en) * | 2016-08-15 | 2016-10-26 | 四川兴能新材料有限公司 | Method for recycling lithium titanate electrode slice |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112768629A (en) * | 2021-01-15 | 2021-05-07 | 内蒙古恒科新材料科技有限公司 | Method for preparing lithium ion battery negative electrode material by taking waste graphite electrode as raw material |
| CN115043398A (en) * | 2022-06-21 | 2022-09-13 | 广东凯金新能源科技股份有限公司 | Simplified method for preparing lithium ion negative electrode material by utilizing micro-powder raw material |
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| CN111285365B (en) | 2023-03-10 |
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Address after: 518000 factory building a, 174-1 Xiangshan Avenue, Luotian community, Yanluo street, Bao'an District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Xinmao New Energy Technology Co.,Ltd. Address before: 518000 factory building a, 174-1 Xiangshan Avenue, Luotian community, Yanluo street, Bao'an District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Xinmao New Energy Technology Co.,Ltd. |
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