CN116573937A - Efficient special carbon preparation method and kneading process thereof - Google Patents
Efficient special carbon preparation method and kneading process thereof Download PDFInfo
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- CN116573937A CN116573937A CN202310476605.7A CN202310476605A CN116573937A CN 116573937 A CN116573937 A CN 116573937A CN 202310476605 A CN202310476605 A CN 202310476605A CN 116573937 A CN116573937 A CN 116573937A
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- 238000004898 kneading Methods 0.000 title claims abstract description 87
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010426 asphalt Substances 0.000 claims abstract description 107
- 239000000654 additive Substances 0.000 claims abstract description 49
- 230000000996 additive effect Effects 0.000 claims abstract description 49
- 239000000571 coke Substances 0.000 claims abstract description 37
- 238000001816 cooling Methods 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 27
- 239000006253 pitch coke Substances 0.000 claims description 19
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 18
- 238000007599 discharging Methods 0.000 claims description 15
- 239000003245 coal Substances 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000004939 coking Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 239000002006 petroleum coke Substances 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000007493 shaping process Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 18
- 238000007598 dipping method Methods 0.000 abstract description 8
- 238000009739 binding Methods 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract description 2
- 238000005087 graphitization Methods 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/62625—Wet mixtures
- C04B35/62635—Mixing details
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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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
Abstract
The invention discloses a high-efficiency special carbon preparation method which comprises the following steps: raw material preparation, kneading, crushing, forming, roasting, dipping and graphitization; wherein, the kneading comprises the following steps: preheating, kneading and cooling. The coke powder consists of additive with average grain size less than 1-80 microns and asphalt coke, and has large specific surface area, and after the modified asphalt is used as adhesive to mix with the coke powder under pressure, the modified asphalt can be made to permeate into the pores of the coke powder and be coated on the surface of the coke powder; compared with the traditional process, the invention omits the binding sheet, one-time dipping and one-time roasting, thereby not only improving the efficiency and greatly reducing the cost, but also greatly improving the physicochemical property of the final product by improving the microcosmic form, so that the prepared product has compact structure, good uniformity and isotropy, and greatly improved flexural strength and volume density; and the yield is improved by 10-30%, so that the method has good industrialization prospect.
Description
Technical Field
The invention relates to the technical field of carbon materials, in particular to a high-efficiency special carbon preparation method and a kneading process thereof.
Background
The term "special carbon" refers to a special carbon product, and the narrow definition refers to a carbon product prepared by a special process and having higher or specific physical and chemical performance indexes. Compared with common carbon products, the special carbon has the advantages of good electric conduction and thermal conductivity, high-temperature strength, small thermal expansion coefficient, self lubrication, high temperature resistance, acid and alkali salt resistance, corrosion resistance, high volume density, easy processing and the like. The special carbon has the main application fields of crystal continuous casting, electric spark processing, semiconductors, nuclear industry, aerospace and the like.
The preparation method of the special carbon comprises the working procedures of grinding, kneading, binding, forming, roasting, dipping, graphitizing and the like, wherein the kneading working procedure is one of the most critical working procedures for determining the qualification rate and the stability of the product. The conventional kneading process method in the field has the defects of low kneading efficiency, non-uniformity, poor effect and the like, and greatly influences the stability and qualification rate of products. Both chinese patent CN 108640681A and chinese patent CN 109336605A overcome the disadvantages of kneading, and ensure the stability and qualification rate of the product by secondary impregnation and secondary baking, but the design of secondary impregnation and secondary baking greatly prolongs the reaction path, and the energy consumption is larger, and in addition, the increase of the impregnation time and times can result in the increase of the thermal expansion coefficient of the carbon material. Therefore, there is a need to propose a solution to the above-mentioned problem.
Disclosure of Invention
In view of the above, the present invention aims at overcoming the defects of the prior art, and its main objective is to provide a high-efficiency special carbon preparation method and a kneading process thereof, which omits the rolling sheet, the one-time dipping and the one-time roasting of the traditional preparation method, not only improves the preparation efficiency, reduces the energy consumption and reduces the preparation cost, but also the prepared product has compact structure, good uniformity and isotropy, and greatly improves the flexural strength and the bulk density.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a kneading process for preparing special carbon is characterized in that: the method comprises the following steps:
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 140-300 ℃, and stirring for 10-60min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 1-10 parts, and the weight part of the asphalt coke is 65-80 parts;
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 140-300 ℃ in advance, stirring for 1-5min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, keeping the pressure in the kneading pot at 0.1-3Mpa, and continuing kneading for 0.3-8h to obtain paste; wherein, the weight part of the modified asphalt is 10-70 parts;
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches RT-60 ℃.
As a preferable scheme, the additive is one or a mixture of two or more of petroleum coke, graphite powder and carbon fiber.
As a preferable scheme, the additive is graphite powder.
As a preferable scheme, the pitch coke is calcined pitch coke.
As a preferable scheme, the modified asphalt is medium-temperature coal asphalt or high-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
As a preferred embodiment, the particle size of the additive and the particle size of the pitch coke are both 1-80 μm.
An efficient method for preparing special carbon comprises the following steps: raw material preparation, the kneading process for preparing special carbon, crushing, forming, roasting, dipping and graphitizing.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and in particular, the technical scheme can be as follows:
the coke powder consists of additive with average grain size less than 1-80 microns and asphalt coke, and has large specific surface area, and after the modified asphalt is used as adhesive to mix with the coke powder under pressure, the modified asphalt can be made to permeate into the pores of the coke powder and be coated on the surface of the coke powder; compared with the traditional process, the invention omits binding sheets, one-time dipping and one-time roasting, thereby not only improving the efficiency and greatly reducing the cost, but also greatly improving the physicochemical property of the final product by improving the microcosmic shape, so that the prepared product has compact structure, good uniformity and isotropy, and greatly improved flexural strength and volume density; and the yield is improved by 10-30%, so that the method has good industrialization prospect.
In order to more clearly illustrate the invention and its efficacy, the invention is explained in detail below with reference to specific examples.
Detailed Description
The invention discloses a high-efficiency special carbon preparation method, which comprises the following steps: raw material preparation, kneading, crushing, forming, roasting, dipping and graphitization.
The kneading process comprises the following steps:
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 140-300 ℃, and stirring for 10-60min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 1-10 parts, and the weight part of the asphalt coke is 65-80 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is one or a mixture of two or more of petroleum coke, graphite powder and carbon fiber, preferably graphite powder; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 140-300 ℃ in advance, stirring for 1-5min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, keeping the pressure in the kneading pot at 0.1-3Mpa, and continuing kneading for 0.3-8h to obtain paste; wherein, the weight part of the modified asphalt is 10-70 parts; the modified asphalt is medium-temperature coal asphalt or high-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches RT-60 ℃.
The following describes in detail specific embodiments.
Example 1
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 140 ℃, and stirring for 30min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 6 parts, and the weight part of the asphalt coke is 65 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is petroleum coke; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 140 ℃ in advance, stirring for 5min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, keeping the pressure in the kneading pot to be 0.5Mpa at 140 ℃, and continuing kneading for 8h to obtain a paste; wherein, the weight part of the modified asphalt is 50 parts; the modified asphalt is medium-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches RT.
And after discharging, sequentially crushing, forming, roasting, impregnating and graphitizing the discharged blanks to finally obtain the finished product.
Example 2
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 240 ℃, and stirring for 10min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 1 part, and the weight part of the asphalt coke is 75 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is carbon fiber; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 240 ℃ in advance, stirring for 3min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, and introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, wherein the temperature of the inert gas is 240 ℃, the pressure in the kneading pot is kept to be 0.1Mpa, and continuing kneading for 6h to obtain a paste; wherein, the weight part of the modified asphalt is 10; the modified asphalt is medium-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches 50 ℃.
And after discharging, sequentially crushing, forming, roasting, impregnating and graphitizing the discharged blanks to finally obtain the finished product.
Example 3
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 300 ℃, and stirring for 42min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 10 parts, and the weight part of the asphalt coke is 68 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is graphite powder; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 300 ℃ in advance, stirring for 1min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, keeping the pressure in the kneading pot at 2.5Mpa, and continuing kneading for 0.3h to obtain a paste; wherein, the weight part of the modified asphalt is 26 parts; the modified asphalt is medium-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches 38 ℃.
And after discharging, sequentially crushing, forming, roasting, impregnating and graphitizing the discharged blanks to finally obtain the finished product.
Example 4
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 210 ℃, and stirring for 60min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 8 parts, and the weight part of the asphalt coke is 80 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is petroleum coke and carbon fiber; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 210 ℃ in advance, stirring for 4min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, and introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, wherein the temperature of the inert gas is 210 ℃, the pressure in the kneading pot is kept to be 3Mpa, and continuing kneading for 2h to obtain a paste; wherein, the weight part of the modified asphalt is 70 parts; the modified asphalt is high-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches 60 ℃.
And after discharging, sequentially crushing, forming, roasting, impregnating and graphitizing the discharged blanks to finally obtain the finished product.
Example 5
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 280 ℃, and stirring for 52min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 5 parts, and the weight part of the asphalt coke is 72 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is graphite powder; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 280 ℃ in advance, stirring for 3min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, keeping the pressure in the kneading pot to be 1.5Mpa at the temperature of 280 ℃, and continuing kneading for 6h to obtain a paste; wherein the modified asphalt is 64 parts by weight; the modified asphalt is high-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches 36 ℃.
And after discharging, sequentially crushing, forming, roasting, impregnating and graphitizing the discharged blanks to finally obtain the finished product.
Example 6
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 180 ℃, and stirring for 42min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 3 parts, and the weight part of the asphalt coke is 62 parts; the particle size of the additive and the particle size of the asphalt coke are 1-80 mu m; in addition, the additive is graphite powder and petroleum coke; the pitch coke is calcined pitch coke.
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, heating the temperature of the kneading pot to 180 ℃ in advance, stirring for 3min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, and introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, wherein the temperature of the inert gas is 180 ℃, the pressure in the kneading pot is kept to be 2.5Mpa, and continuing kneading for 6h to obtain a paste; wherein, the weight part of the modified asphalt is 34 parts; the modified asphalt is medium-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches 56 ℃.
And after discharging, sequentially crushing, forming, roasting, impregnating and graphitizing the discharged blanks to finally obtain the finished product.
The performance test was performed on the above-described examples, and the results of the performance test are shown in table 1.
TABLE 1
It is apparent from the data in table 1 that the finished product prepared by the preparation process of the present invention has good conductivity, high temperature resistance, high strength, high bulk density and excellent isotropy, and that the finished product with such excellent properties can be prepared by the kneading process of the present invention with reduced one-time dipping and one-time baking processes, and thus the increase of the thermal expansion coefficient of the product is avoided.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical principles of the present invention are still within the scope of the technical solutions of the present invention.
Claims (7)
1. A kneading process for preparing special carbon is characterized in that: the method comprises the following steps:
(1) Preheating: placing the additive and the crushed asphalt coke into a preheater, increasing the temperature to 140-300 ℃, and stirring for 10-60min to uniformly mix the additive and the asphalt coke to obtain coke powder; wherein, the weight part of the additive is 1-10 parts, and the weight part of the asphalt coke is 65-80 parts;
(2) Kneading: transferring the coke powder obtained in the step (1) into a kneading pot, wherein the temperature of the kneading pot is raised to 140-300 ℃ in advance, stirring for 1-5min, adding melted modified asphalt into the kneading pot through an asphalt pipeline, sealing a pipeline for introducing the modified asphalt after adding the modified asphalt, introducing a certain amount of preheated inert gas into the kneading pot through another pipeline, keeping the pressure in the kneading pot at 0.1-3Mpa, and continuing kneading for 0.3-8h to obtain paste; wherein, the weight part of the modified asphalt is 10-70 parts;
(3) And (3) cooling: and (3) transferring the paste obtained in the step (2) into a cooling machine for cooling, stirring while cooling, and discharging for standby when the temperature of the paste reaches RT-60 ℃.
2. The kneading process for producing extra-carbon according to claim 1, wherein: the additive is one or two or more of petroleum coke, graphite powder and carbon fiber.
3. The kneading process for producing extra-carbon according to claim 2, wherein: the additive is graphite powder.
4. The kneading process for producing extra-carbon according to claim 1, wherein: the pitch coke is calcined pitch coke.
5. The kneading process for producing extra-carbon according to claim 1, wherein: the modified asphalt is medium-temperature coal asphalt or high-temperature coal asphalt, and the performance indexes are as follows: the softening point is 100-250 ℃, the mass ratio of toluene insoluble matters is 30-60%, the mass ratio of quinoline insoluble matters is 2-30%, and the coking value is more than 50.
6. The kneading process for producing extra-carbon according to claim 1, wherein: the particle size of the additive and the particle size of the asphalt coke are both 1-80 mu m.
7. A high-efficiency special carbon preparation method is characterized in that: the method comprises the following steps: raw material preparation, kneading process for preparing special carbon according to any one of claims 1 to 6, pulverizing, shaping, baking, impregnating and graphitizing.
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| CN202310476605.7A CN116573937A (en) | 2023-04-28 | 2023-04-28 | Efficient special carbon preparation method and kneading process thereof |
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