CN115433009A - Sagger for graphitizing and purifying battery negative electrode and preparation method thereof - Google Patents
Sagger for graphitizing and purifying battery negative electrode and preparation method thereof Download PDFInfo
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- CN115433009A CN115433009A CN202211040768.2A CN202211040768A CN115433009A CN 115433009 A CN115433009 A CN 115433009A CN 202211040768 A CN202211040768 A CN 202211040768A CN 115433009 A CN115433009 A CN 115433009A
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- negative electrode
- carburant
- battery negative
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- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 239000011329 calcined coke Substances 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005011 phenolic resin Substances 0.000 claims abstract description 8
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 13
- 238000005087 graphitization Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 239000002006 petroleum coke Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims 3
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000428 dust Substances 0.000 abstract description 2
- 238000000462 isostatic pressing Methods 0.000 abstract description 2
- 238000004898 kneading Methods 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract description 2
- 239000011265 semifinished product Substances 0.000 abstract description 2
- 238000010304 firing Methods 0.000 description 8
- 239000010426 asphalt Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped 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
- C04B35/52—Shaped 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
- C04B35/528—Shaped 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
- C04B35/532—Shaped 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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63472—Condensation polymers of aldehydes or ketones
- C04B35/63476—Phenol-formaldehyde condensation polymers
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0068—Containers
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention relates to the technical field of sagger production, and discloses a sagger for graphitizing and purifying a battery cathode and a preparation method thereof, wherein the raw materials of the sagger comprise, by weight, 50-70% of calcined coke, 20-30% of a carburant, 10-20% of crushed graphite, and additionally 12-18% of a binding agent phenolic resin of the total weight of the raw materials. The raw materials are mixed in the mixing mill, the mixing mill process is adopted to replace the existing wet kneading process, and the mixing process is environment-friendly and free of dust; the isostatic pressing is adopted to replace the existing heating hydraulic forming, the production efficiency and the qualification rate of semi-finished products are improved, and the formed products have high strength and can be randomly operated without being placed; the sintering period is short, and is 3-5 days, so that the energy consumption is greatly reduced, carbon-buried roasting is not needed, and the environment is friendly.
Description
Technical Field
The invention relates to the technical field of sagger production, in particular to a sagger for graphitizing and purifying a battery negative electrode and a preparation method thereof.
Background
After the coating of the lithium ion battery negative electrode material is finished, the graphitization is realized at high temperature, and a sagger is used for containing the negative electrode material to perform high-temperature treatment in a high-temperature furnace, so that the graphitization and purification of the negative electrode are realized.
The traditional preparation process of saggers has many drawbacks: 1) The environment is polluted, asphalt binder is used in the preparation raw materials, the pollution is high, the odor irritation is very large, the liquid asphalt needs to be continuously heated for storage, and the energy consumption is high; 2) The forming process is complex, a grinding tool needs to be heated during forming to ensure the forming performance, and the formed product has low mechanical performance and needs to be maintained in a time-consuming manner; 3) The firing period is long, about 10 days for one firing period, and the energy consumption is high.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a sagger for graphitizing and purifying a battery cathode.
In order to achieve the purpose, the technical scheme of the invention is as follows: a sagger for graphitizing and purifying a battery negative electrode is characterized in that: the raw materials of the sagger comprise, by weight, 50-70% of calcined coke, 20-30% of carburant, 10-20% of crushed graphite and 12-18% of binder phenolic resin in percentage by weight.
Further, the method comprises the following steps of; the carburant is a petroleum coke carburant.
Further, the method comprises the following steps of; the graphite fragments are a by-product produced during the graphitization of the battery negative electrode.
Further, the method comprises the following steps of; the particle size and the corresponding weight percentage of the calcined coke, the carburant and the crushed graphite mixed raw material are as follows: 25% of particles with a diameter of 1-5mm, 35% of particles with a diameter of 0.2-1mm, and 40% of particles with a diameter of less than 0.2 mm.
The other technical scheme of the invention is as follows: a preparation method of a sagger for graphitizing and purifying a battery negative electrode is characterized by comprising the following steps:
weighing calcined coke, a carburant and graphite powder according to the weight percentage, mixing, slowly adding a binding agent phenolic resin in the mixing process, uniformly mixing, and ageing at the humidity of 40-60% and the temperature of 18-30 ℃ for not less than 24 hours;
after ageing, loading the mixture into a mould, putting the mould into a cold isostatic press, and carrying out pressure forming under the pressure of 90-140 MPa;
loading the formed sagger into a kiln, and firing the sagger into a finished product according to a firing curve, wherein the firing curve is increased from room temperature to 300 ℃ and the use time is 1.5 hours; keeping the temperature at 300 ℃ for 0.5h, then heating the temperature from 300 ℃ to 550 ℃, and using the time for 2.5h; keeping 550 deg.C for 0.5h, heating from 550 deg.C to 650 deg.C for 1.5h, keeping 650 deg.C for 0.5h, heating from 650 deg.C to 980 deg.C for 3h, and keeping 980 deg.C for 2h.
The invention has the beneficial effects that:
1) The raw materials of the sagger replace asphalt binder by phenolic resin binder, so that the sagger is environment-friendly and pollution-free; the graphite is crushed into byproducts produced in the graphitization process of the battery cathode, and the byproducts are recycled, so that the discharge pressure is reduced;
2) The raw materials are mixed in a mixing mill, the mixing mill process is adopted to replace the existing wet kneading process, and the mixing process is environment-friendly and free of dust; the isostatic pressing is adopted to replace the existing heating hydraulic forming, the production efficiency and the qualification rate of semi-finished products are improved, and the formed products have high strength and can be randomly operated without being placed;
3) The sintering period is short, and is 3-5 days, so that the energy consumption is greatly reduced, carbon-buried roasting is not needed, and the environment is friendly.
Detailed Description
Example 1:
the sagger for graphitizing and purifying the battery negative electrode comprises, by weight, 60% of calcined coke, 30% of petroleum coke recarburizing agent, 10% of crushed graphite and 16% of binding agent phenolic resin of the total weight of the raw materials.
The petroleum coke recarburizer has high carbon and low sulfur, the C is more than or equal to 99 percent, and the S is less than or equal to 0.1 percent.
The graphite fragments are byproducts generated during the graphitization of the battery cathode.
The particle size and the corresponding weight percentage of the calcined coke, the recarburizing agent and the crushed graphite mixed raw material are as follows: 25% of particles with a diameter of 1-5mm, 35% of particles with a diameter of 0.2-1mm, and 40% of particles with a diameter of less than 0.2 mm.
A preparation method of a sagger for graphitizing and purifying a battery negative electrode is characterized by comprising the following steps:
1) Weighing calcined coke, a carburant and graphite particles according to the weight percentage, mixing for 1h in a mixing mill, slowly adding a binding agent phenolic resin in the mixing process, and ageing at 25 ℃ under 50% humidity for not less than 24h after uniformly mixing;
2) After ageing, putting the mixture into a mould, putting the mould into a cold isostatic press, and carrying out pressure forming under 140 MPa;
3) Loading the formed sagger into a kiln, and firing the sagger into a finished product according to a firing curve, wherein the firing curve is increased from room temperature to 300 ℃ and the use time is 1.5 hours; keeping the temperature at 300 ℃ for 0.5h, then heating the temperature from 300 ℃ to 550 ℃, and using the time for 2.5h; keeping 550 deg.C for 0.5h, heating from 550 deg.C to 650 deg.C for 1.5h, keeping 650 deg.C for 0.5h, heating from 650 deg.C to 980 deg.C for 3h, and keeping 980 deg.C for 2h. The physical indexes of the finished product are as follows: bulk density: 1.6g/cm 3 The porosity is 15-18%, the compressive strength is 26Mpa, and the flexural strength is 8Mpa.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.
Claims (5)
1. A sagger for graphitizing and purifying a battery negative electrode is characterized in that: the raw materials of the sagger comprise, by weight, 50-70% of calcined coke, 20-30% of carburant, 10-20% of crushed graphite and 12-18% of binder phenolic resin in percentage by weight.
2. The sagger for battery negative electrode graphitization and purification according to claim 1, wherein: the carburant is a petroleum coke carburant.
3. The sagger for battery negative electrode graphitization and purification according to claim 1, wherein: the graphite fragments are byproducts generated during the graphitization of the battery cathode.
4. The sagger for battery negative electrode graphitization and purification according to claim 1, wherein the particle size and the corresponding weight percentage of the calcined coke, the carburant and the crushed graphite mixed raw material are as follows: 25% of the granules with the particle size of 1-5mm, 35% of the granules with the particle size of 0.2-1mm and 40% of the granules with the particle size of less than 0.2 mm.
5. A method for preparing the sagger for battery negative electrode graphitization and purification according to any one of claims 1-4, characterized by comprising the following steps:
1) Weighing calcined coke, a carburant and graphite powder according to the weight percentage, mixing, slowly adding a binding agent phenolic resin in the mixing process, uniformly mixing, and ageing at the humidity of 40-60% and the temperature of 18-30 ℃ for not less than 24 hours;
2) After ageing, loading the mixture into a mould, putting the mould into a cold isostatic press, and carrying out pressure forming under the pressure of 90-140 MPa;
3) Loading the formed sagger into a kiln, and sintering the sagger into a finished product according to a sintering curve, wherein the sintering curve is that the temperature is increased from room temperature to 300 ℃, and the time is 1.5 hours; keeping the temperature at 300 ℃ for 0.5h, heating the temperature from 300 ℃ to 550 ℃, and using the time for 2.5h; keeping 550 deg.C for 0.5h, heating from 550 deg.C to 650 deg.C for 1.5h, keeping 650 deg.C for 0.5h, heating from 650 deg.C to 980 deg.C for 3h, and keeping 980 deg.C for 2h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211040768.2A CN115433009A (en) | 2022-08-29 | 2022-08-29 | Sagger for graphitizing and purifying battery negative electrode and preparation method thereof |
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| CN202211040768.2A CN115433009A (en) | 2022-08-29 | 2022-08-29 | Sagger for graphitizing and purifying battery negative electrode and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332650A (en) * | 2023-03-30 | 2023-06-27 | 青岛正望新材料股份有限公司 | Short-process near-net-shape manufacturing method of graphite product |
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2022
- 2022-08-29 CN CN202211040768.2A patent/CN115433009A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332650A (en) * | 2023-03-30 | 2023-06-27 | 青岛正望新材料股份有限公司 | Short-process near-net-shape manufacturing method of graphite product |
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