CN110451501B - Artificial graphite negative electrode material prepared from graphite electrode joint powder and preparation method thereof - Google Patents
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Abstract
The invention discloses a method for preparing an artificial graphite cathode material by using graphite electrode joint powder, which comprises the following steps: s1: collecting graphite electrode joint powder, and carrying out crushing and grading treatment on the graphite electrode joint powder to obtain graphite particles; s2: spheroidizing the graphite particles to obtain spheroidized graphite particles; s3: demagnetizing the spheroidized graphite particles to obtain demagnetized spherical graphite particles; s4: mixing and granulating the demagnetized spherical graphite particles and the wrapping granulating agent to obtain wrapping and granulating particles; s5: carrying out pyrolysis carbonization treatment on the coated granulation particles, and then carrying out grading demagnetization to obtain coated granulation powder; s6: and shaping and grading the wrapped and granulated powder to obtain the high-performance artificial graphite cathode material. The invention overcomes the problems of high specific surface area and overproof magnetic substance content of the graphite electrode joint powder, widens the application field of the graphite electrode joint powder, realizes resource regeneration, transformation and utilization, and is easy for industrialized mass production.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an artificial graphite cathode material prepared from graphite electrode joint powder and a preparation method of the artificial graphite cathode material.
Background
The lithium ion battery is a new battery widely applied to the industries of rail transit, electronic communication, wearable equipment and the like. At present, graphite is one of the first choices of lithium ion battery cathodes, and mainly comprises natural graphite and artificial graphite, wherein the natural graphite material is mainly natural crystalline flake graphite and is obtained by crushing, spheroidizing, grading, purifying, surface treating and other processes. The artificial graphite is prepared by using coal-based needle coke and petroleum coke as aggregates and coal pitch as a binder through the procedures of batching, kneading, molding, carbonization, high-temperature graphitization and the like. In the carbon industry, the preparation process of the graphite electrode is similar to the production process of artificial graphite. A large amount of electrode joint powder is generated in the mechanical forming process of the graphite electrode, the electrode joint powder is already graphitized, the graphitization degree is extremely high, but because more impurities such as resistance materials, silicon carbide, iron rust and the like are adhered to the surface of the graphite electrode joint powder, the ash content and the impurity content of the graphite electrode joint powder are high, and the content of magnetic substances exceeds the standard. Therefore, the electrode joint powder can not be directly applied to the preparation of graphite cathode materials of lithium ion batteries. A large amount of raw materials of the electrode joint powder are wasted, and the production concept of green and environmental protection at present is not met. Therefore, how to develop a novel preparation method of a graphite negative electrode material, which overcomes the problems in the prior art, makes full use of graphite joint powder generated in the mechanical forming process of a graphite electrode, and realizes the preparation of the graphite negative electrode material so as to achieve the technical effects of energy conservation, environmental protection and resource regeneration and conversion utilization is the direction of research needed by technical personnel in the field.
Disclosure of Invention
The invention aims to provide a method for preparing an artificial graphite cathode material by using graphite electrode joint powder, which is used for preparing the artificial graphite cathode material and achieves the technical effects of energy conservation, environmental protection and resource regeneration and conversion utilization.
The technical scheme is as follows:
a method for preparing an artificial graphite negative electrode material by using graphite electrode joint powder comprises the following steps: s1: collecting graphite electrode joint powder, and carrying out crushing and grading treatment on the graphite electrode joint powder by using a jet mill to obtain graphite particles; s2: spheroidizing the graphite particles obtained in the step S1 by using a spheroidizing machine to obtain spherical graphite particles; s3: demagnetizing the spherical graphite particles obtained in the step S2 by using an electromagnetic iron remover to obtain demagnetized spherical graphite particles; s4: uniformly mixing the demagnetized spherical graphite particles obtained in the step S3 with a coating granulating agent, and mixing and granulating in a coating granulator to obtain coated granulated particles; s5: carrying out pyrolysis carbonization treatment and grading demagnetization on the coated and granulated particles obtained in the step S4 in a heat treatment furnace in an inert gas atmosphere to obtain coated and granulated powder; s6: and (4) shaping and grading the wrapped and granulated powder obtained in the step (S5) in a graphite shaping machine to obtain the graphite cathode material.
By adopting the technical scheme: based on steps S1 and S2, the collected graphite electrode tab powder is crushed into fine graphite particles with high surface roundness, so as to facilitate mixing, coating and granulating in the subsequent steps. The spherical graphite particles are demagnetized based on step S3, and the iron content thereof is reduced. Based on the steps S4 and S5, the demagnetized spherical graphite particles and a granulating agent are mixed for granulation and pyrolytic carbonization treatment, so that a coating layer on the particle surface forms a stable carbon layer, the specific surface area of the carbon layer is reduced, the particle size of the particles is homogenized, and finally the iron content is reduced to below 30ppm through further demagnetization, shaping and grading treatment, thus obtaining the graphite cathode material
Preferably, in the method for preparing the artificial graphite negative electrode material using the graphite electrode tab powder, the method comprises the following steps: the particle size of the graphite particles in the step S1 is D10Is 0-8 μm, D50Is 10-15 μm, D90Is 20-50 μm.
More preferably, in the method for preparing the artificial graphite negative electrode material using the graphite electrode tab powder, the method comprises the steps of: the coating granulating agent in the step S4 is any one of asphalt, phenolic resin and epoxy resin.
More preferably, in the method for preparing the artificial graphite negative electrode material using the graphite electrode tab powder, the method comprises: and step S5, the heat treatment furnace is any one of a box furnace, a tube furnace, a pusher kiln, a roller kiln and a rotary furnace. More preferably, in the method for preparing the artificial graphite negative electrode material: in step S5, the inert gas is nitrogen or argon.
Still more preferably, in the above method for preparing an artificial graphite negative electrode material using the graphite electrode tab powder: and S5, the temperature environment of the pyrolysis carbonization treatment is 700-1200 ℃, and the heat preservation time is 1-5 hours.
The invention also discloses an artificial graphite cathode material prepared by using the graphite electrode joint powder, which is prepared by adopting the preparation method of the artificial graphite cathode material.
Preferably, the above-mentioned utilizationIn the artificial graphite cathode material prepared from the graphite electrode joint powder: the particle size distribution of the artificial graphite negative electrode is D10Is 0-16 μm, D5020-28 μm, D9030-60 μm, and specific surface area of 1.5-2.5m2(ii) g, tap density of 0.7-1.1g/cm3The fixed carbon content is 99.0-99.9%, and the graphitization degree is 91-96%.
More preferably, in the artificial graphite negative electrode material prepared using the graphite electrode tab powder as described above: the coating granulating agent accounts for 2-10% of the mass of the artificial graphite cathode material.
Compared with the prior art, the invention can realize the preparation of the artificial graphite material by utilizing the graphite electrode joint powder, and achieves the technical effects of energy conservation, environmental protection and resource regeneration and conversion utilization.
Drawings
FIG. 1 is a process flow diagram of the present invention;
fig. 2 is a charge/discharge curve diagram of a lithium ion battery using the graphite negative electrode material obtained in example 1.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following will be further described with reference to various embodiments.
It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention. In the following examples, all percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
a method for preparing an artificial graphite negative electrode material by using graphite electrode joint powder comprises the following implementation steps:
s1: collecting graphite electrode joint powder, and crushing and grading the graphite electrode joint powder by using a jet mill to obtain particle size distribution D107.5 μm, D50Is 14.0 μm, D90Graphite particles of 32.0 μm;
s2: spheroidizing the graphite particles obtained in the step S1 by using a spheroidizing machine to obtain spherical graphite particles;
s3: demagnetizing the spherical graphite particles obtained in the step S2 by using an electromagnetic iron remover to obtain demagnetized spherical graphite particles, and reducing the iron content in the particles to be below 30 ppm;
s4: pouring asphalt into the demagnetized spherical graphite particles obtained in S3 to form a mixture by taking the asphalt as a wrapping granulating agent, wherein the mass of the asphalt accounts for 10% of the total mass of the mixture, and mixing and granulating the mixture in a coating granulator to obtain wrapping and granulating particles;
s5: carrying out pyrolysis carbonization treatment and graded demagnetization on the coated and granulated particles obtained in the step S4 in a rotary furnace at 1200 ℃ under the protection of nitrogen atmosphere for 1h to obtain coated and granulated powder;
s6: shaping and grading the wrapped and granulated powder obtained in the step S5 to obtain the graphite cathode material with the particle size distribution D1010.0 μm, D5019.0 μm, D9034.0 μm and a specific surface area of 2.5m2(ii)/g, tap density 0.90g/cm3The fixed carbon content was 99.4%, and the graphitization degree was 94%.
Example 2:
a method for preparing an artificial graphite negative electrode material by using graphite electrode joint powder comprises the following implementation steps:
s1: collecting graphite electrode joint powder, and crushing and grading the graphite electrode joint powder by using a jet mill to obtain particle size distribution D107.5 μm, D5015.0 μm, D90Graphite particles of 32.0 μm;
s2: spheroidizing the graphite particles obtained in the step S1 by using a spheroidizing machine to obtain spherical graphite particles;
s3: demagnetizing the spherical graphite particles obtained in the step S2 by using an electromagnetic iron remover to obtain demagnetized spherical graphite particles, so that the iron content of the demagnetized spherical graphite particles is reduced to be below 30 ppm;
s4: epoxy resin is used as a wrapping granulating agent, the epoxy resin is added into the demagnetized spherical graphite particles obtained from S3 to form a mixture, and the mass of the epoxy resin accounts for 3% of the total mass of the mixture; coating and granulating the mixture in a coating granulator to obtain coated and granulated particles;
s5: carrying out pyrolysis carbonization treatment on the coated and granulated particles obtained in the step S4 in a box furnace at the temperature of 1000 ℃ in the argon gas atmosphere for 3h, and then carrying out grading demagnetization to obtain coated and granulated powder;
s6: shaping and grading the wrapped and granulated powder obtained in the step S5 to obtain the graphite cathode material with the particle size distribution D109.0 μm, D5016.0 μm, D9030.0 μm and a specific surface area of 2.3m2(g) tap density of 0.85g/cm3The fixed carbon content was 99.2%, and the graphitization degree was 93%.
Example 3
A method for preparing an artificial graphite negative electrode material by using graphite electrode joint powder comprises the following implementation steps:
s1: collecting graphite electrode joint powder, and crushing and grading the graphite electrode joint powder by using a jet mill to obtain particle size distribution D107.5 μm, D5017.0 μm, D90Graphite particles of 32.0 μm;
s2: spheroidizing the graphite particles obtained in the step S1 by using a spheroidizing machine to obtain spherical graphite particles;
s3: demagnetizing the spherical graphite particles obtained in the step S2 by using an electromagnetic iron remover to obtain demagnetized spherical graphite particles, so that the iron content in the particles is reduced to be below 30 ppm;
s4: phenolic resin is adopted as a wrapping granulating agent, phenolic resin is added into the demagnetized spherical graphite particles obtained in the step S3 to form a mixture, the mass of the phenolic resin is controlled to be 5% of that of the mixture, and the mixture is fully mixed and granulated in a coating granulator to obtain wrapping granulated particles;
s5: carrying out pyrolysis carbonization treatment on the coated granulation particles obtained in the step S4 in a tube furnace under the protection of nitrogen atmosphere at the temperature of 800 ℃ for 5 hours, and then carrying out grading demagnetization to obtain coated granulation powder;
s6: obtained in S5Shaping and grading the wrapped and granulated powder to obtain the graphite cathode material with the particle size distribution D1011.0 μm, D5020.0 μm, D9034.0 μm and a specific surface area of 1.5m2(ii)/g, tap density 0.86g/cm3The fixed carbon content was 99.4%, and the graphitization degree was 93%.
Through detection, the specific parameters of the artificial graphite anode material prepared by the three embodiments are shown in the following table 1:
TABLE 1
Obviously, the preparation method provided by the invention can produce the artificial graphite cathode material with excellent performance, and meanwhile, the production cost is reduced by 50-70%.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. The protection scope of the present invention is subject to the protection scope of the claims.
Claims (6)
1. A method for preparing an artificial graphite negative electrode material by using graphite electrode joint powder is characterized by comprising the following steps:
s1: collecting graphite electrode joint powder, and carrying out crushing and grading treatment on the graphite electrode joint powder by using a jet mill to obtain graphite particles;
s2: spheroidizing the graphite particles obtained in the step S1 by using a spheroidizing machine to obtain spheroidized graphite particles;
s3: demagnetizing the spheroidized graphite particles obtained in the step S2 by using an electromagnetic iron remover to obtain demagnetized spheroidized graphite particles;
s4: uniformly mixing the demagnetized spheroidized graphite particles obtained in the step S3 with a coating granulating agent, and mixing and granulating in a coating granulator to obtain coated granulated particles;
s5: carrying out pyrolysis carbonization treatment and grading demagnetization on the coated and granulated particles obtained in the step S4 in a heat treatment furnace in an inert gas atmosphere to obtain coated and granulated powder;
s6: and (5) shaping and grading the coated and granulated powder obtained in the step (S5) in a graphite shaping machine to obtain the artificial graphite cathode material.
2. The method for preparing an artificial graphite negative electrode material using the graphite electrode tab powder as claimed in claim 1, wherein: the particle size of the graphite particles in the step S1 is D10Is 0-8 μm, D50Is 10-15 μm, D90Is 20-50 μm.
3. The method for preparing an artificial graphite negative electrode material using the graphite electrode tab powder as claimed in claim 1, wherein: the coating granulating agent in the step S4 is any one of asphalt, phenolic resin and epoxy resin.
4. The method for preparing an artificial graphite negative electrode material using the graphite electrode tab powder as claimed in claim 1, wherein: and step S5, the heat treatment furnace is any one of a box furnace, a tube furnace, a pusher kiln, a roller kiln and a rotary furnace.
5. The method for preparing an artificial graphite negative electrode material using the graphite electrode tab powder as claimed in claim 1, wherein: in step S5, the inert gas is nitrogen or argon.
6. The method for preparing an artificial graphite negative electrode material using the graphite electrode tab powder as claimed in claim 1, wherein: and S5, the temperature environment of the low-temperature pyrolysis treatment is 700-1200 ℃, and the heat preservation time is 1-5 hours.
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| KR102691473B1 (en) * | 2019-12-03 | 2024-08-05 | 컨템포러리 엠퍼렉스 테크놀로지 씨오., 리미티드 | Artificial graphite, secondary battery, manufacturing method and device |
| CN113104845B (en) * | 2020-01-13 | 2022-07-29 | 上海昱瓴新能源科技有限公司 | Method for preparing porous artificial graphite cathode material by using electrode joint powder as raw material |
| CN111600091A (en) * | 2020-06-05 | 2020-08-28 | 深圳鑫茂新能源技术有限公司 | Method for recycling graphite of negative electrode of lithium ion battery |
| CN112645318A (en) * | 2020-11-19 | 2021-04-13 | 上海杉杉科技有限公司 | Method for preparing artificial graphite cathode material by using resistance material |
| CN112713264A (en) * | 2020-12-28 | 2021-04-27 | 宁波杉杉新材料科技有限公司 | Artificial graphite negative electrode material, preparation method, application and battery |
| CN115739394A (en) * | 2022-11-23 | 2023-03-07 | 青岛泰达华润新能源科技有限公司 | Manufacturing method for reducing content of magnetic substances in natural graphite negative electrode material |
| CN115893402A (en) * | 2022-11-24 | 2023-04-04 | 银硅(宁波)科技有限公司 | Method for preparing low-expansion high-rate graphite negative electrode material by using crucible waste |
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| CN102610795B (en) * | 2011-01-20 | 2016-04-27 | 宁波宏远炭素工业有限公司 | A kind of preparation method of carbon negative electrode material of lithium ion cell coating layer |
| CN102544629B (en) * | 2012-01-17 | 2015-05-13 | 广东邦普循环科技有限公司 | Method for regenerating waste and old graphite anode materials |
| CN103811758B (en) * | 2014-02-19 | 2016-04-20 | 新乡市赛日新能源科技有限公司 | A kind of preparation method of synthetic graphite particle negative material |
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