CN113831126A - Preparation method of isostatic pressing negative electrode carbon material - Google Patents

Preparation method of isostatic pressing negative electrode carbon material Download PDF

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Publication number
CN113831126A
CN113831126A CN202111094399.0A CN202111094399A CN113831126A CN 113831126 A CN113831126 A CN 113831126A CN 202111094399 A CN202111094399 A CN 202111094399A CN 113831126 A CN113831126 A CN 113831126A
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China
Prior art keywords
coke
asphalt
negative electrode
carbon material
preparing
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Pending
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CN202111094399.0A
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Chinese (zh)
Inventor
王志辉
柴万红
武晨洁
张培林
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Datong Xincheng New Material Co Ltd
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Datong Xincheng New Material Co Ltd
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Priority to CN202111094399.0A priority Critical patent/CN113831126A/en
Publication of CN113831126A publication Critical patent/CN113831126A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/528Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
    • C04B35/532Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/20Graphite
    • C01B32/205Preparation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/522Graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures

Abstract

The invention belongs to the technical field of carbon material preparation, and particularly relates to a preparation method of an isostatic pressing negative electrode carbon material, which comprises the following steps: s1, preparing raw materials: preparing asphalt coke, calcined coke and modified asphalt; s2, primary grinding: grinding the calcined coke and the asphalt coke; s3, dry mixing: adding the pulverized calcined coke and the pulverized bituminous coke into a kneading pot for dry mixing; s4, kneading: after the asphalt is fully melted, adding the asphalt into a kneading pot for kneading; s5, secondary grinding: milling the paste kneaded in S4; s6, vacuumizing and pressing: filling the paste pulverized by the S5 into a material bag for vacuum pumping; then the mixture is sent into isostatic pressing for pressing treatment; s7, graphitizing: sending the product after pressing treatment into a graphitization furnace for graphitization treatment; s8, grinding again: and grinding the graphite product after the graphitization treatment. The invention has simple operation, low cost and less labor.

Description

Preparation method of isostatic pressing negative electrode carbon material
Technical Field
The invention belongs to the technical field of carbon material preparation, and particularly relates to a preparation method of an isostatic pressing negative electrode carbon material.
Background
With the development of science and technology, the requirements of the cathode material are continuously improved, especially the electrical properties are more prominent, so that the electrical properties are required in the production of the cathode material by using isostatic pressing equipment at present.
The lithium battery anode materials are roughly divided into the following types: the first is a carbon negative electrode material: the negative electrode materials that have been practically used in lithium ion batteries at present are basically carbon materials such as artificial graphite, natural graphite, mesocarbon microbeads, petroleum coke, carbon fibers, pyrolytic resin carbon, and the like.
The second is a tin-based negative electrode material: the tin-based negative electrode material can be classified into tin oxide and tin-based composite oxide. The oxide refers to the oxide of metallic tin in various valence states. There is currently no commercial product.
The current common production method is as follows: the pitch coke powder is loaded into a crucible and then graphitized. But has a series of problems of difficult index meeting requirements, high cost and the like.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of an isostatic pressing negative electrode carbon material, which is simple to operate and low in cost.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of an isostatic pressing negative electrode carbon material comprises the following steps:
s1, preparing raw materials: preparing asphalt coke, calcined coke and modified asphalt;
s2, primary grinding: grinding the calcined coke and the asphalt coke;
s3, dry mixing: adding the pulverized calcined coke and the pulverized bituminous coke into a kneading pot for dry mixing;
s4, kneading: adding powder into the modified asphalt, and adding the modified asphalt into a kneading pot for kneading after the asphalt is fully melted;
s5, secondary grinding: milling the paste kneaded in S4;
s6, vacuumizing and pressing: filling the paste pulverized by the S5 into a material bag for vacuum pumping; after vacuumizing, sending the mixture into isostatic pressing for pressing;
s7, graphitizing: sending the product after pressing treatment into a graphitization furnace for graphitization treatment;
s8, grinding again: and grinding the graphite product after the graphitization treatment.
In said S1: the content of asphalt coke is 40%, the content of calcined coke is 30%, and the content of modified asphalt is 30%.
In said S2: the particle size of the calcined coke and the pulverized asphalt coke powder is 800.
In said S3: the dry blending time was 2.5 hours and the temperature was 178 ℃.
In said S4: the kneading time was 2 hours and the paste was removed from the pot at 170 ℃.
In said S5: the particle size of the paste milled was 500 mesh.
In said S7: the graphitization temperature is 2800-3000 ℃, and the electric sintering is carried out for 15 days.
In said S8: the milled powder had a particle size of 625 mesh.
Compared with the prior art, the invention has the following beneficial effects:
the invention is a method for preparing special graphite by combining a novel process and a traditional product; the raw materials only need asphalt coke, calcined coke and modified asphalt, and the powder prepared by the formula and the process has the resistance of only 0.2m omega. The invention has simple operation, low cost and less labor.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of an isostatic pressing negative electrode carbon material comprises the following steps:
s1, preparing raw materials: preparing asphalt coke, calcined coke and modified asphalt;
s2, primary grinding: grinding the calcined coke and the asphalt coke;
s3, dry mixing: adding the pulverized calcined coke and the pulverized bituminous coke into a kneading pot for dry mixing;
s4, kneading: adding powder into the modified asphalt, and adding the modified asphalt into a kneading pot for kneading after the asphalt is fully melted;
s5, secondary grinding: milling the paste kneaded in S4;
s6, vacuumizing and pressing: filling the paste pulverized by the S5 into a material bag for vacuum pumping; after vacuumizing, sending the mixture into isostatic pressing for pressing;
s7, graphitizing: sending the product after pressing treatment into a graphitization furnace for graphitization treatment;
s8, grinding again: and grinding the graphite product after the graphitization treatment.
The preferred embodiment of the invention is:
40% of asphalt coke, 30% of calcined coke and 30% of modified asphalt.
Firstly, grinding calcined coke and asphalt coke into powder with the granularity of about 800 meshes, and dry-mixing the calcined coke and the asphalt coke in a kneading pot according to the percentage for 2.5 hours at the kneading temperature of 178 ℃.
And then adding the modified asphalt into powder, fully melting the asphalt, mixing and kneading the mixture in a mixing and kneading pot for 2 hours, and taking the paste out of the pot at 170 ℃.
And then milling the paste into powder of 500 meshes, loading the powder into a material bag for vacuumizing, when the vacuum degree reaches, vacuumizing for 3 hours, then pressing in an isostatic pressing machine, directly feeding the pressed product into a graphitization furnace for graphitization, controlling the graphitization temperature to be about 2800 and 3000 ℃, electrifying and sintering for about 15 days, taking the product out of the furnace after cooling, and milling the graphite product into powder with the milling requirement of 625 meshes after the product is out of the furnace. The powder resistance is only 0.2m omega by testing.
Although only the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art, and all changes are encompassed in the scope of the present invention.

Claims (8)

1. A preparation method of an isostatic pressing negative electrode carbon material is characterized by comprising the following steps:
s1, preparing raw materials: preparing asphalt coke, calcined coke and modified asphalt;
s2, primary grinding: grinding the calcined coke and the asphalt coke;
s3, dry mixing: adding the pulverized calcined coke and the pulverized bituminous coke into a kneading pot for dry mixing;
s4, kneading: adding powder into the modified asphalt, and adding the modified asphalt into a kneading pot for kneading after the asphalt is fully melted;
s5, secondary grinding: milling the paste kneaded in S4;
s6, vacuumizing and pressing: filling the paste pulverized by the S5 into a material bag for vacuum pumping; after vacuumizing, sending the mixture into isostatic pressing for pressing;
s7, graphitizing: sending the product after pressing treatment into a graphitization furnace for graphitization treatment;
s8, grinding again: and grinding the graphite product after the graphitization treatment.
2. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S1: the content of asphalt coke is 40%, the content of calcined coke is 30%, and the content of modified asphalt is 30%.
3. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S2: the particle size of the calcined coke and the pulverized asphalt coke powder is 800.
4. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S3: the dry blending time was 2.5 hours and the temperature was 178 ℃.
5. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S4: the kneading time was 2 hours and the paste temperature was 170 ℃.
6. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S5: the particle size of the paste milled was 500 mesh.
7. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S7: the graphitization temperature is 2800-3000 ℃, and the electric sintering is carried out for 15 days.
8. The method for preparing an isostatic negative electrode carbon material as claimed in claim 1, wherein in S8: the milled powder had a particle size of 625 mesh.
CN202111094399.0A 2021-09-17 2021-09-17 Preparation method of isostatic pressing negative electrode carbon material Pending CN113831126A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114213128A (en) * 2021-12-28 2022-03-22 成都炭素有限责任公司 Preparation method for preparing fluorocarbon anode plate by isostatic pressing

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000007436A (en) * 1998-06-26 2000-01-11 Ibiden Co Ltd Graphite material and its production
CN101913593A (en) * 2010-08-26 2010-12-15 大同市新成特炭有限公司 Graphite material for producing nanogate carbon and preparation method thereof
CN107721425A (en) * 2017-10-24 2018-02-23 大同新成新材料股份有限公司 A kind of preparation method of negative material
CN108530078A (en) * 2018-06-01 2018-09-14 大同新成新材料股份有限公司 A kind of forming method of big specification isostatic pressing formed graphite product
CN108585865A (en) * 2018-06-06 2018-09-28 大同新成新材料股份有限公司 A kind of preparation method of graphene carbon material used as anode
CN110330336A (en) * 2019-07-05 2019-10-15 鞍山炭素有限公司 The production method that graphite anode is used in the production of lithium metal sodium

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000007436A (en) * 1998-06-26 2000-01-11 Ibiden Co Ltd Graphite material and its production
CN101913593A (en) * 2010-08-26 2010-12-15 大同市新成特炭有限公司 Graphite material for producing nanogate carbon and preparation method thereof
CN107721425A (en) * 2017-10-24 2018-02-23 大同新成新材料股份有限公司 A kind of preparation method of negative material
CN108530078A (en) * 2018-06-01 2018-09-14 大同新成新材料股份有限公司 A kind of forming method of big specification isostatic pressing formed graphite product
CN108585865A (en) * 2018-06-06 2018-09-28 大同新成新材料股份有限公司 A kind of preparation method of graphene carbon material used as anode
CN110330336A (en) * 2019-07-05 2019-10-15 鞍山炭素有限公司 The production method that graphite anode is used in the production of lithium metal sodium

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114213128A (en) * 2021-12-28 2022-03-22 成都炭素有限责任公司 Preparation method for preparing fluorocarbon anode plate by isostatic pressing

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Application publication date: 20211224