CN114478042A - Preparation method of fiber-reinforced special isostatic pressing graphite - Google Patents
Preparation method of fiber-reinforced special isostatic pressing graphite Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000462 isostatic pressing Methods 0.000 title claims abstract description 38
- 239000010439 graphite Substances 0.000 title claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000010426 asphalt Substances 0.000 claims abstract description 51
- 238000004898 kneading Methods 0.000 claims abstract description 36
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 26
- 239000004917 carbon fiber Substances 0.000 claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 23
- 238000000465 moulding Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000005087 graphitization Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000012216 screening Methods 0.000 claims abstract description 11
- 238000007598 dipping method Methods 0.000 claims abstract description 10
- 239000000571 coke Substances 0.000 claims abstract description 9
- 239000002006 petroleum coke Substances 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 18
- 239000003245 coal Substances 0.000 claims description 9
- 238000004939 coking Methods 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
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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
- 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
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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
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of fiber-reinforced special isostatic pressing graphite, which comprises the following steps: (1) preparation of raw materials: crushing petroleum coke or asphalt coke raw materials on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher; (2) kneading; (3) crushing and screening: crushing the cooled paste to 10-50 μm; (4) molding; (5) roasting; (6) dipping; (7) graphitization: and (4) graphitizing the product obtained in the step (6) at 2500-3000 ℃ to obtain a finished product. The mechanical property index of the product can be effectively improved by adding a proper amount of carbon fiber in the preparation process, a better forming effect can be obtained by matching with isostatic pressing without performing, and the modified asphalt has a better bonding effect with the material by selecting and using the modified asphalt, so that better product performance is obtained.
Description
Technical Field
The invention relates to the technical field of graphite products, in particular to a preparation method of fiber-reinforced special isostatic pressing graphite.
Background
As a global manufacturing industry major country and the largest photovoltaic product producing countries, china has kept a huge demand for isostatic pressing graphite. Currently, with the rapid development of the domestic photovoltaic industry, the demand of the Chinese isostatic pressing graphite is increased year by year. Meanwhile, because the technical basis of China isostatic pressing graphite production enterprises is weak, and the technology of foreign enterprises is blocked, the yield and the quality of the China isostatic pressing graphite are not effectively improved. In 2011, the demand of Chinese isostatic pressing graphite reaches 1.8 ten thousand tons, while the production of the isostatic pressing graphite in the same period is only 9500 tons, and the supply gap reaches 8500 tons. At present, the problems of insufficient technical reserve, unreasonable product structure and the like commonly existing in enterprises of China newly involved in isostatic pressing graphite business are difficult to solve in a short time.
The isostatic pressing graphite is formed by pressing high-purity graphite. Isostatic pressing graphite is a new product developed in the last 50 years internationally and is closely linked with the high technology of the present day. Because the isostatic pressing graphite has higher embedding end, density, purity, corrosion resistance and other properties, the isostatic pressing graphite is widely applied to the fields of metallurgy, chemical engineering, aerospace, electronics, machinery, nuclear energy and the like. But the performance of the isostatic pressing graphite produced by the prior art is greatly limited due to poor plasticity, impact resistance, elastic modulus and the like. Therefore, there is a need to develop a solution to the above problems.
Disclosure of Invention
In view of the above, the present invention is directed to the defects existing in the prior art, and the main object of the present invention is to provide a method for preparing fiber-reinforced special isostatic pressing graphite, which significantly improves the performance indexes of strength and toughness of graphite materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing petroleum coke or asphalt coke raw materials on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher;
(2) kneading: putting a certain proportion of the coke powder and the fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, then increasing the temperature to 140-300 ℃, adding a certain proportion of modified asphalt, and continuing to knead for 0.3-8 h; after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain paste;
(3) crushing and screening: crushing the cooled paste to 10-50 μm, and sieving with a 50-300 mesh sieve;
(4) molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; the forming pressure is 50-300 MPa, and the blank is obtained after the pressure maintaining time is 10-180 min and demoulding;
(5) roasting: performing heat preservation on the blank obtained in the step (4) at the temperature of 750-1050 ℃ for roasting for 10-100 h;
(6) dipping: preheating the blank obtained in the step (5) at 300-500 ℃ for 2-24 h, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 1.5-5 Mpa for 1-5 h; the impregnated product is further repeated in the step (5);
(7) graphitization: and (4) graphitizing the product obtained in the step (6) at 2500-3000 ℃ to obtain a finished product.
Preferably, the mass percentage of the carbon fiber short fibers is 0.1-5%.
Preferably, the mass ratio of the carbon fiber short fibers is 1-3%.
As a preferable scheme, the mass ratio of the coke powder is 55-75%; the mass ratio of the modified asphalt is 25-45%.
As a preferable scheme, the modified asphalt is medium-temperature and high-temperature coal asphalt, and typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
the mechanical property index of the product can be effectively improved by adding a proper amount of carbon fiber in the preparation process, a better forming effect can be obtained by matching with isostatic pressing without performing, and the modified asphalt has a better bonding effect with the material by selecting and using the modified asphalt, so that better product performance is obtained.
Detailed Description
The invention discloses a preparation method of fiber-reinforced special isostatic pressing graphite, which comprises the following steps:
(1) preparation of raw materials: crushing petroleum coke or asphalt coke raw materials on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting coke powder and fluffy powder in a certain proportion into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 140-300 ℃, adding modified asphalt in a certain proportion, and continuing kneading for 0.3-8 h; and after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass ratio of the carbon fiber short fibers is 0.1-5%. Preferably, the mass ratio of the carbon fiber short fibers is 1-3%. The mass ratio of the coke powder is 55-75%; the mass ratio of the modified asphalt is 25-45%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: the cooled paste is crushed to 10-50 μm and passed through a 50-300 mesh screen.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; and (3) demoulding to obtain a blank body after the forming pressure is 50-300 MPa and the pressure maintaining time is 10-180 min.
(5) Roasting: and (5) insulating the blank obtained in the step (4) at 750-1050 ℃ and roasting for a reasonable time of 10-100 h.
(6) Dipping: preheating the blank obtained in the step (5) at 300-500 ℃ for 2-24 h, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 1.5-5 Mpa for 1-5 h; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (4) graphitizing the product obtained in the step (6) at 2500-3000 ℃ to obtain a finished product.
The invention is illustrated in more detail below by means of a number of examples and comparative examples:
example 1:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing a petroleum coke raw material on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting a certain proportion of coke powder and fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 140 ℃, adding a certain proportion of modified asphalt, and continuing kneading for 2 h; and (5) after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass percentage of the carbon fiber short fiber is 5%. The mass percentage of the coke powder is 75%; the mass ratio of the modified asphalt is 25%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: the cooled paste is crushed to 10-50 μm and passed through a 250 mesh screen.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; the molding pressure is 200MPa, and the blank is obtained after the pressure maintaining time is 100min and demoulding.
(5) Roasting: and (4) preserving the temperature of the blank obtained in the step (4) at 750 ℃, and roasting for a reasonable time of 30 h.
(6) Dipping: preheating the blank obtained in the step (5) at 400 ℃ for 8 hours, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 3Mpa for 5 hours; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (4) carrying out graphitization treatment on the product obtained in the step (6) at 3000 ℃ to obtain a finished product.
Example 2:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing a petroleum coke raw material on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting a certain proportion of coke powder and fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 160 ℃, adding a certain proportion of modified asphalt, and continuing kneading for 0.3 h; and (5) after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass percentage of the carbon fiber short fiber is 1%. The mass ratio of the coke powder is 70%; the mass percentage of the modified asphalt is 29%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: the cooled paste is crushed to 10-50 μm and passed through a 50 mesh screen.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; the molding pressure is 100MPa, and the blank is obtained after 10min of pressure maintaining.
(5) Roasting: and (5) keeping the temperature of the blank obtained in the step (4) at 850 ℃ and roasting for reasonable time of 10 h.
(6) Dipping: preheating the blank obtained in the step (5) at 300 ℃ for 2h, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 1.5Mpa for 4 h; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (5) graphitizing the product obtained in the step (6) at 2800 ℃ to obtain a finished product.
Example 3:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing the asphalt coke raw material on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting a certain proportion of coke powder and fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 200 ℃, adding a certain proportion of modified asphalt, and continuing kneading for 8 h; and (5) after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass percentage of the carbon fiber short fiber is 1.5%. The mass percentage of the coke powder is 65%; the mass ratio of the modified asphalt is 32%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: and crushing the cooled paste to 10-50 mu m, and sieving the paste by a 100-mesh sieve.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; and (4) demoulding to obtain a blank after the forming pressure is 50MPa and the pressure maintaining time is 50 min.
(5) Roasting: and (4) keeping the temperature of the blank obtained in the step (4) at 850 ℃ and roasting for a reasonable time of 80 h.
(6) Dipping: preheating the blank obtained in the step (5) at 300 ℃ for 20 hours, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 2Mpa for 3 hours; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (4) carrying out graphitization treatment on the product obtained in the step (6) at 3000 ℃ to obtain a finished product.
Example 4:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing the asphalt coke raw material on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting a certain proportion of coke powder and fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 250 ℃, adding a certain proportion of modified asphalt, and continuing kneading for 5 h; and (5) after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass ratio of the carbon fiber short fibers is 0.1%. The mass percentage of the coke powder is 65%; the mass percentage of the modified asphalt is 33.5%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: the cooled paste is crushed to 10-50 μm and passed through a 200 mesh screen.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; and (4) demoulding to obtain a blank after the forming pressure is 240MPa and the pressure maintaining time is 130 min.
(5) Roasting: and (4) keeping the temperature of the blank obtained in the step (4) at 950 ℃ and roasting for 100 hours.
(6) Dipping: preheating the blank obtained in the step (5) at 450 ℃ for 24 hours, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 3.5Mpa for 2 hours; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (4) carrying out graphitization treatment on the product obtained in the step (6) at 3000 ℃ to obtain a finished product.
Example 5:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing the asphalt coke raw material on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting a certain proportion of coke powder and fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 300 ℃, adding a certain proportion of modified asphalt, and continuing kneading for 4 h; and (5) after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass percentage of the carbon fiber short fiber is 0.5%. The mass percentage of the coke powder is 65%; the mass percentage of the modified asphalt is 33.5%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: the cooled paste is crushed to 10-50 μm and sieved with a 300-mesh screen.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; the molding pressure is 300MPa, and the blank is obtained after the pressure maintaining time is 180min and demoulding.
(5) Roasting: and (4) keeping the temperature of the blank obtained in the step (4) at 1050 ℃ and roasting for 50 h.
(6) Dipping: preheating the blank obtained in the step (5) at 500 ℃ for 13h, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 2.5Mpa for 1 h; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (5) graphitizing the product obtained in the step (6) at 2900 ℃ to obtain a finished product.
Example 6:
a preparation method of fiber-reinforced special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials: crushing petroleum coke and asphalt coke raw materials on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; and (3) crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher.
(2) Kneading: putting a certain proportion of coke powder and fluffy powder into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 250 ℃, adding a certain proportion of modified asphalt, and continuing kneading for 3 h; and (5) after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain the paste. The mass percentage of the carbon fiber short fiber is 2.5%. The coke powder accounts for 60% by mass, wherein the petroleum coke accounts for 30% and the asphalt coke accounts for 30%; the mass percentage of the modified asphalt is 33.5%. The modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
(3) Crushing and screening: and crushing the cooled paste to 10-50 mu m, and screening the paste through a 280-mesh screen.
(4) Molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; the molding pressure is 280MPa, and the blank is obtained after the pressure maintaining time is 80min and demoulding.
(5) Roasting: and (4) keeping the temperature of the blank obtained in the step (4) at 850 ℃ for roasting for 60 hours.
(6) Dipping: preheating the blank obtained in the step (5) at 480 ℃ for 15 hours, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 2.5Mpa for 1-5 hours; and (5) further repeating the operation of the step (5) on the impregnated product.
(7) Graphitization: and (4) carrying out graphitization treatment on the product obtained in the step (6) at 3000 ℃ to obtain a finished product.
Comparative example:
the preparation method was substantially the same as that of example 4 except that no carbon fiber short fiber was added.
The above examples and comparative examples were subjected to the following performance tests, and the test results are shown in the following table:
the method for testing the flexural strength comprises the following steps: refer to national standard GB/T3001-2007.
Method for testing elastic modulus: refer to national standard GB/T3074.2-2008.
The design of the invention is characterized in that: the mechanical property index of the product can be effectively improved by adding a proper amount of carbon fiber in the preparation process, a better forming effect can be obtained by matching with isostatic pressing without performing, and the modified asphalt has a better bonding effect with the material by selecting and using the modified asphalt, so that better product performance is obtained.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (5)
1. A preparation method of fiber-reinforced special isostatic pressing graphite is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of raw materials: crushing petroleum coke or asphalt coke raw materials on a crusher to a reasonable particle size to prepare coke powder with an average particle size of 5-30 mu m; crushing the carbon fiber short fibers into fluffy powder of 10-50 mu m by a crusher;
(2) kneading: putting coke powder and fluffy powder in a certain proportion into a kneading machine, stirring for 10-60 min, uniformly mixing, raising the temperature to 140-300 ℃, adding modified asphalt in a certain proportion, and continuing kneading for 0.3-8 h; after the kneading is finished, putting the mixture into a material cooling machine for cooling to obtain paste;
(3) crushing and screening: crushing the cooled paste material to 10-50 mu m, and sieving the paste material by a 50-300 mesh sieve;
(4) molding: putting the crushed paste into a rubber mold, vacuum charging, and then putting into an isostatic pressing machine for molding; the forming pressure is 50-300 MPa, and the blank is obtained after the pressure maintaining time is 10-180 min and demoulding;
(5) roasting: performing heat preservation on the blank obtained in the step (4) at the temperature of 750-1050 ℃ for roasting for 10-100 h;
(6) dipping: preheating the blank obtained in the step (5) at 300-500 ℃ for 2-24 h, and then carrying out impregnation treatment on the blank by using impregnating pitch under the pressure of 1.5-5 Mpa for 1-5 h; the impregnated product is further repeated in the step (5);
(7) graphitization: and (4) graphitizing the product obtained in the step (6) at 2500-3000 ℃ to obtain a finished product.
2. The method for preparing fiber-reinforced special isostatic graphite according to claim 1, wherein: the mass ratio of the carbon fiber short fibers is 0.1-5%.
3. The method for preparing fiber-reinforced special isostatic graphite according to claim 2, wherein: the mass ratio of the carbon fiber short fibers is 1-3%.
4. The method for preparing fiber-reinforced special isostatic graphite according to claim 1, wherein: the mass ratio of the coke powder is 55-75%; the mass ratio of the modified asphalt is 25-45%.
5. The method for preparing fiber-reinforced special isostatic graphite according to claim 1, wherein: the modified asphalt is medium-temperature and high-temperature coal asphalt, and the typical performance indexes are as follows: the softening point is 100-250 ℃, the toluene insoluble substance is 30-60, the quinoline insoluble substance is 2-30, and the coking value is more than 50.
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