CN116081613A - Preparation method of high-strength fine-particle isostatic graphite material - Google Patents

Preparation method of high-strength fine-particle isostatic graphite material Download PDF

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CN116081613A
CN116081613A CN202111304053.9A CN202111304053A CN116081613A CN 116081613 A CN116081613 A CN 116081613A CN 202111304053 A CN202111304053 A CN 202111304053A CN 116081613 A CN116081613 A CN 116081613A
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吕尊华
冯奕钰
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Shanghai Fucarbon New Material Co ltd
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Abstract

The invention provides a preparation technology of high-strength fine particle isostatic graphite, which uses coke as a raw material to prepare raw material powder with stable granularity, optimizes the powder to obtain the raw material powder with specific particle distribution characteristics and average granularity of 10-13 mu m, and performs batching, kneading, secondary grinding and profiling to obtain green compact, and then performs roasting, dipping and graphitization treatment to obtain isotropic high-performance fine particle isostatic graphite.

Description

Preparation method of high-strength fine-particle isostatic graphite material
Technical Field
The invention belongs to the field of preparation of graphite materials, and particularly relates to a preparation method of a high-strength isotropic fine-particle isostatic graphite material.
Background
The isostatic graphite is a novel graphite material, has a series of excellent performances such as isotropy, low linear expansion coefficient, stable chemical property, strength increase along with temperature rise at high temperature, can withstand severe temperature change, has good lubrication and abrasion resistance, good mechanical processing performance and the like, and can be applied to the fields of semiconductors, solar photovoltaics, nuclear power high-temperature gas cooled reactor materials, dies, powder metallurgy, vacuum heat treatment and the like. At present, the high-performance isostatic graphite can be produced in China, but the problems of low performance, large performance index range, unstable quality, small specification and the like generally exist, and the method is only suitable for the field of high-temperature resistant materials with low requirements, and a large amount of high-performance, stable-quality and large-specification fine-particle isostatic graphite also needs to be imported to meet the requirements, so that a large amount of foreign exchange is lost every year, and the national strategic industry applied to the high-end isostatic graphite is limited by people at any time and possibly clamped around the neck.
To meet the requirements of high-end manufacturing industries for high-performance isostatic graphite, each graphite manufacturer generally uses isostatic pressing with high-pressure pressurizing capabilityAnd reducing the fineness of the raw material particles. At present, the particle fineness of main raw materials in China is mainly 15-25 mu m, and the typical performance of the produced isostatic pressing graphite is that the density of the body is 1.78g/cm 3 The resistance is 15uΩ.m, the flexural strength is 40MPa, and the main particle fineness of the high-end isostatic pressing graphite raw material produced internationally is 5-10 μm, even the material with the particle fineness of 1-3 μm can be provided in batch. For example, POCO in the United states can provide products with average granularity of 1 μm, the flexural strength can reach 95MPa, the compressive strength can reach 140MPa, the Shore hardness can reach 100MPa, SGL in Germany can provide products with average granularity of 3 μm, the flexural strength can reach 90MPa, the compressive strength can reach 145MPa, the Shore hardness can reach 78MPa, but core technologies such as raw material pulverizing process, compounding and kneading process of foreign manufacturers are always kept strictly secret, and only the machining of products is put in domestic production. Compared with foreign countries, the domestic isostatic pressing graphite material also has the problems of insufficient fine raw material particles, immature corresponding formula design and kneading process, related roasting, missing graphitization process and the like.
Along with the further improvement of the industrialization degree of China, the isostatic graphite material is gradually and vigorously developed in various application fields in a new cycle of industrial revolution surge, and under the background of global epidemic situation tired economic growth, the related carbon material industry of the western traditional developed countries is subjected to great impact, and the supply of the global isostatic graphite material is influenced. Therefore, the preparation technology of the isostatic pressing graphite material in China is developed at the present stage, the market of high-end material application is occupied, and the problem that the graphite material for the national strategic industry is clamped in the neck and the like is particularly important to be solved.
Disclosure of Invention
1 the invention relates to a preparation technology of high-strength fine particle isostatic pressing graphite, which adopts the following technical scheme:
1) The true density is more than 1.90g/cm 3 Petroleum coke or asphalt coke with volatile matter content less than 0.5%, sulfur content less than 0.5%, water content less than 0.5%, ash content less than 0.5% and powder resistivity of 300-800 [ mu ] ohm.m is used as the material for producing isostatic pressure graphite.
2) Crushing the raw coke by a crusher to obtain granules with the particle size of less than 10mm, and grinding by a Raymond mill to obtain coke powder with the average particle size of 50-60 mu m;
3) Grinding the 50-60 mu m of coke powder by using a vertical superfine grinding machine, and obtaining primary dust collecting powder with average particles of 12-20 mu m and secondary dust collecting powder with average particles of 3-8 mu m by using a secondary dust collecting process;
4) Further, the primary dust collection powder and the secondary dust collection powder are prepared according to the proportion of (60.0-80.0) wt% to (40.0-20.0) wt%, and are mixed for 1.5-3.0 h by a three-dimensional rotary mixer, and then are screened by a 200-mesh vibrating screen with an ultrasonic function, so that powder with average particle size of 10-13 mu m and stable distribution is obtained as raw material powder for producing fine-particle isostatic graphite materials;
5) Preheating the powder with the particle size of 10-13 mu m and stable distribution to 200-220 ℃ in a raw material bin with material heating and conveying functions, and simultaneously heating the powder with the softening point of 160-180 ℃ and coking value of more than 60% and true density of more than 1.25g/cm 3 Heating high-temperature asphalt with volatile matter 45-60% and ash content less than 0.5% in a melting tank to 230 ℃ to fully melt the asphalt, adding the raw material powder and the high-temperature asphalt into a kneader with strong kneading capacity according to the ratio of (1.8-2.3) to 1 for pressurizing and kneading, controlling the kneading temperature to be 225-230 ℃ and the kneading time to be 1.5-4.0 h, cooling the kneaded paste in a cooling pot to 50 ℃ at the speed of 10-30 ℃/h, crushing to below 10mm by a hammer crusher, and then performing secondary grinding in a paste mill to obtain paste powder with the average granularity of 15-60 mu m;
6) Filling the obtained paste powder into a rubber mold with a special size, filling the rubber mold into a porous steel mold, sealing and vacuumizing the whole body after being treated by a high-frequency vibration compacting process for 1-5 h, and hanging the whole body of the steel mold into a cylinder diameter after the completion of the vacuumizing
Figure BSA0000256898580000021
Isostatic compaction is carried out in a cold isostatic press with the molding pressure of 100-180 MPa, and the density of 1.50-1.60 g/cm is obtained 3 Is a green body of (c);
7) Filling the pressed green compact into a steel tank, filling the steel tank and the pressed green compact with filling materials with the particle range of 0-3 mm, vibrating and compacting, then filling the steel tank and the pressed green compact into a roasting furnace, roasting at the heating rate of 0.1-2.8 ℃/h to fully carbonize the steel tank and introducing inert protective gas in the process, and roasting the total heating curve time is more than 800 hours.
8) Loading the carbonized baked blank into an impregnating tank, heating impregnating asphalt with a softening point of 90-120 ℃ and a quinoline insoluble content of less than 2.0% to 190 ℃, then injecting the impregnating asphalt into the impregnating tank, applying a pressure of 1.5-5.0 MPa for impregnating operation, and discharging the impregnated blank from the tank after the duration of 20-30 hours to obtain an impregnated blank;
9) Loading the impregnated blank into a roasting furnace, heating to 750 ℃ by adopting a bare burning process, cooling to 200 ℃ and discharging to obtain a secondary roasting blank;
10 Charging the secondary roasting blank into an Acheson graphitizing furnace, filling the periphery and the furnace bottom of the furnace chamber with heat preservation materials and resistance materials, electrifying and heating to 1800-2400 ℃, introducing halogen gas at a high temperature stage for purification, slowly cooling the product to below 100 ℃, and discharging to obtain the high-strength fine-particle isostatic graphite.
Preferably, as in step 1), a true density of > 1.90g/cm is selected 3 Petroleum coke or asphalt coke is used as raw material for producing isostatic pressure graphite.
Preferably, the coke powder is pulverized as in step 2) to an average particle size of 50 to 60. Mu.m.
Preferably, step 3) uses a secondary dust collection process to obtain primary dust collection powder with average particles of 12-20 mu m and secondary dust collection powder with average particles of 3-8 mu m.
Preferably, powder with average particle size of 10-13 μm and stable distribution is obtained as step 4) as raw material powder for producing fine particle isostatic graphite material.
Preferably, a paste powder with an average particle size of 15-60 μm is obtained as in step 5).
Preferably, the molding pressure is 100-180 MPa as in the step 6).
Preferably, as in step 7), the roasting is performed at a heating rate of 0.1-2.8 ℃/h to fully carbonize the material for more than 800 hours.
Preferably, the dipping operation is carried out by applying a pressure of 1.5-5.0 MPa as in the step 8), and the dipping blank is obtained after the duration of 20-30 hours.
Preferably, in the step 9), the bare burning process is adopted to heat to 750 ℃, then cooled to 200 ℃ and discharged from the furnace, and the secondary roasting blank is obtained.
Preferably, in the step 10), the secondary roasting blank is filled into an Acheson graphitization furnace, the temperature is increased to 1800-2400 ℃, and halogen gas is introduced in the high-temperature stage for purification, so that the high-strength fine-particle isostatic graphite is obtained.
The invention provides a preparation technology of high-strength fine particle isostatic graphite, which uses coke as a raw material to prepare raw material powder with stable granularity, optimizes the powder to obtain the raw material powder with specific particle distribution characteristics and average granularity of 10-13 mu m, and performs batching, kneading, secondary grinding and profiling to obtain green compact, and then performs roasting, dipping and graphitization treatment to obtain isotropic high-performance fine particle isostatic graphite.
Description of the drawings:
FIG. 1 is a flow chart of the preparation of a high strength fine particulate isostatic graphite material according to the present invention;
FIG. 2 is a scanning electron microscope image of a method for preparing a high-strength fine-particle isostatic graphite material according to the present invention;
FIG. 3 is a Raman spectrum of a method for preparing a high-strength fine-particle isostatic graphite material according to the present invention.
Detailed Description
The following 3 examples of the invention are given as further illustration of the invention and are not intended to limit the scope of the invention.
Example 1
1) The true density is more than 1.90g/cm 3 Petroleum coke or asphalt coke with volatile matter content less than 0.5%, sulfur content less than 0.5%, water content less than 0.5%, ash content less than 0.5% and powder resistivity of 300-800 [ mu ] ohm.m is used as the material for producing isostatic pressure graphite.
2) Crushing the raw coke by a crusher to obtain granules with the particle size of less than 10mm, and grinding by a Raymond mill to obtain coke powder with the average particle size of 50-60 mu m;
3) Grinding the 50-60 mu m of coke powder by using a vertical superfine grinding machine, and obtaining primary dust collecting powder with average particles of 12-20 mu m and secondary dust collecting powder with average particles of 3-8 mu m by using a secondary dust collecting process;
4) Further, the primary dust collection powder and the secondary dust collection powder are prepared according to the proportion of (60.0-80.0) wt% to (40.0-20.0) wt%, and are mixed for 1.5-3.0 h by a three-dimensional rotary mixer, and then are screened by a 200-mesh vibrating screen with an ultrasonic function, so that powder with average particle size of 10 mu m and stable distribution is obtained as raw material powder for producing fine-particle isostatic-pressure graphite materials;
5) Preheating the powder with the particle size of 10-13 mu m and stable distribution to 200-220 ℃ in a raw material bin with material heating and conveying functions, and simultaneously heating the powder with the softening point of 160-180 ℃ and coking value of more than 60% and true density of more than 1.25g/cm 3 Heating high-temperature asphalt with volatile matter 45-60% and ash content less than 0.5% in a melting tank to 230 ℃ to fully melt the asphalt, then adding the raw material powder and the high-temperature asphalt into a kneader with strong kneading capacity according to the proportion of 1.8:1 for pressurized kneading, controlling the kneading temperature to be 225-230 ℃ and the kneading time to be 1.5-4.0 h under the pressure of 60.0-100.0 MPa, cooling the kneaded paste in a cooling pot to 50 ℃ at the speed of 10-30 ℃/h, crushing to less than 10mm by a hammer crusher, and then feeding the paste into a paste mill for secondary milling to obtain paste powder with the average granularity of 15-60 mu m;
6) Filling the obtained paste powder into a rubber mold with a special size, filling the rubber mold into a porous steel mold, sealing and vacuumizing the whole body after being treated by a high-frequency vibration compacting process for 1-5 h, and hanging the whole body of the steel mold into a cylinder diameter after the completion of the vacuumizing
Figure BSA0000256898580000041
Isostatic compaction is carried out in a cold isostatic press with the molding pressure of 150MPa, and the density of 1.50-1.60 g/cm is obtained 3 Is a green body of (c);
7) Filling the pressed green compact into a steel tank, filling the steel tank and the pressed green compact with filling materials with the particle range of 0-3 mm, vibrating and compacting, then filling the steel tank and the pressed green compact into a roasting furnace, roasting at the heating rate of 0.1-2.8 ℃/h to fully carbonize the steel tank and introducing inert protective gas in the process, and roasting the total heating curve time is more than 800 hours.
8) Loading the carbonized baked blank into an impregnating tank, heating impregnating asphalt with a softening point of 90-120 ℃ and a quinoline insoluble content of less than 2.0% to 190 ℃, then injecting the impregnating asphalt into the impregnating tank, applying a pressure of 1.5-5.0 MPa for impregnating operation, and discharging the impregnated blank from the tank after the duration of 20-30 hours to obtain an impregnated blank;
9) Loading the impregnated blank into a roasting furnace, heating to 750 ℃ by adopting a bare burning process, cooling to 200 ℃ and discharging to obtain a secondary roasting blank;
10 Placing the secondary roasting blank into an Acheson graphitizing furnace, filling the periphery and the furnace bottom of a furnace chamber with heat preservation materials and resistance materials, electrifying and heating to 2000 ℃, introducing halogen gas at a high temperature stage for purification, slowly cooling the product to below 100 ℃, and discharging to obtain the high-strength fine-particle isostatic graphite.
Example 2
1) The true density is more than 1.90g/cm 3 Petroleum coke or asphalt coke with volatile matter content less than 0.5%, sulfur content less than 0.5%, water content less than 0.5%, ash content less than 0.5% and powder resistivity of 300-800 [ mu ] ohm.m is used as the material for producing isostatic pressure graphite.
2) Crushing the raw coke by a crusher to obtain granules with the particle size of less than 10mm, and grinding by a Raymond mill to obtain coke powder with the average particle size of 50-60 mu m;
3) Grinding the 50-60 mu m of coke powder by using a vertical superfine grinding machine, and obtaining primary dust collecting powder with average particles of 12-20 mu m and secondary dust collecting powder with average particles of 3-8 mu m by using a secondary dust collecting process;
4) Further, the primary dust collection powder and the secondary dust collection powder are prepared according to the proportion of (60.0-80.0) wt% to (40.0-20.0) wt%, and are mixed for 1.5-3.0 h by a three-dimensional rotary mixer, and then are screened by a 200-mesh vibrating screen with an ultrasonic function, so that powder with average particle size of 10-13 mu m and stable distribution is obtained as raw material powder for producing fine-particle isostatic graphite materials;
5) Preheating the powder with the particle size of 10-13 mu m and stable distribution to 200-220 ℃ in a raw material bin with material heating and conveying functions, and simultaneously heating the powder with the softening point of 160-180 ℃ and coking value of more than 60% and true density of more than 1.25g/cm 3 Heating high-temperature asphalt with volatile matter 45-60% and ash content less than 0.5% in a melting tank to 230 ℃ to fully melt the asphalt, then adding the raw material powder and the high-temperature asphalt into a kneader with strong kneading capacity according to the proportion of 2:1 for pressurized kneading, controlling the kneading temperature to be 225-230 ℃ and the kneading time to be 1.5-4.0 h under the pressure of 60.0-100.0 MPa, cooling the kneaded paste in a cooling pot to 50 ℃ at the speed of 10-30 ℃/h, crushing to less than 10mm by a hammer crusher, and then performing secondary grinding in a paste mill to obtain paste powder with the average granularity of 15-60 mu m;
6) Filling the obtained paste powder into a rubber mold with a special size, filling the rubber mold into a porous steel mold, sealing and vacuumizing the whole body after being treated by a high-frequency vibration compacting process for 1-5 h, and hanging the whole body of the steel mold into a cylinder diameter after the completion of the vacuumizing
Figure BSA0000256898580000061
Isostatic compaction is carried out in a cold isostatic press with the molding pressure of 100MPa, and the density of 1.50-1.60 g/cm is obtained 3 Is a green body of (c);
7) Filling the pressed green compact into a steel tank, filling the steel tank and the pressed green compact with filling materials with the particle range of 0-3 mm, vibrating and compacting, then filling the steel tank and the pressed green compact into a roasting furnace, roasting at the heating rate of 0.1-2.8 ℃/h to fully carbonize the steel tank and introducing inert protective gas in the process, and roasting the total heating curve time is more than 800 hours.
8) Loading the carbonized baked blank into an impregnating tank, heating impregnating asphalt with a softening point of 90-120 ℃ and a quinoline insoluble content of less than 2.0% to 190 ℃, then injecting the impregnating asphalt into the impregnating tank, applying a pressure of 1.5-5.0 MPa for impregnating operation, and discharging the impregnated blank from the tank after the duration of 20-30 hours to obtain an impregnated blank;
9) Loading the impregnated blank into a roasting furnace, heating to 750 ℃ by adopting a bare burning process, cooling to 200 ℃ and discharging to obtain a secondary roasting blank;
10 Charging the secondary roasting blank into an Acheson graphitizing furnace, filling the periphery and the furnace bottom of the furnace chamber with heat preservation materials and resistance materials, electrifying and heating to 1800 ℃, introducing halogen gas at a high temperature stage for purification, slowly cooling the product to below 100 ℃, and discharging to obtain the high-strength fine-particle isostatic graphite.
Example 3
1) The true density is more than 1.90g/cm 3 Petroleum coke or asphalt coke with volatile matter content less than 0.5%, sulfur content less than 0.5%, water content less than 0.5%, ash content less than 0.5% and powder resistivity of 300-800 [ mu ] ohm.m is used as the material for producing isostatic pressure graphite.
2) Crushing the raw coke by a crusher to obtain granules with the particle size of less than 10mm, and grinding by a Raymond mill to obtain coke powder with the average particle size of 50-60 mu m;
3) Grinding the 50-60 mu m of coke powder by using a vertical superfine grinding machine, and obtaining primary dust collecting powder with average particles of 12-20 mu m and secondary dust collecting powder with average particles of 3-8 mu m by using a secondary dust collecting process;
4) Further, the primary dust collection powder and the secondary dust collection powder are prepared according to the proportion of (60.0-80.0) wt% to (40.0-20.0) wt%, and are mixed for 1.5-3.0 h by a three-dimensional rotary mixer, and then are screened by a 200-mesh vibrating screen with an ultrasonic function, so that powder with average particle size of 10-13 mu m and stable distribution is obtained as raw material powder for producing fine-particle isostatic graphite materials;
5) Preheating the powder with the particle size of 10-13 mu m and stable distribution to 200-220 ℃ in a raw material bin with material heating and conveying functions, and simultaneously heating the powder with the softening point of 160-180 ℃ and coking value of more than 60% and true density of more than 1.25g/cm 3 Heating high-temperature asphalt with 45-60% volatile matter and less than 0.5% ash content to 230 deg.c in a melting tank to make asphalt melt fully, adding the above-mentioned raw material powder and high-temperature asphalt in the ratio of 2.3:1 into a kneader with strong kneading capacity to make pressure kneading, the pressure is 60.0-100.0 MPa, the kneading temperature range is 225-230 deg.c, and kneading time is 15-4.0 h, cooling the kneaded paste to 50 ℃ in a cooling pot at a speed of 10-30 ℃/h, crushing to below 10mm by a hammer crusher, and then performing secondary grinding in a paste grinding machine to obtain paste powder with an average particle size of 15-60 mu m;
6) Filling the obtained paste powder into a rubber mold with a special size, filling the rubber mold into a porous steel mold, sealing and vacuumizing the whole body after being treated by a high-frequency vibration compacting process for 1-5 h, and hanging the whole body of the steel mold into a cylinder diameter after the completion of the vacuumizing
Figure BSA0000256898580000071
Isostatic compaction is carried out in a cold isostatic press with the forming pressure of 180MPa, and the density of 1.50-1.60 g/cm is obtained 3 Is a green body of (c);
7) Filling the pressed green compact into a steel tank, filling the steel tank and the pressed green compact with filling materials with the particle range of 0-3 mm, vibrating and compacting, then filling the steel tank and the pressed green compact into a roasting furnace, roasting at the heating rate of 0.1-2.8 ℃/h to fully carbonize the steel tank and introducing inert protective gas in the process, and roasting the total heating curve time is more than 800 hours.
8) Loading the carbonized baked blank into an impregnating tank, heating impregnating asphalt with a softening point of 90-120 ℃ and a quinoline insoluble content of less than 2.0% to 190 ℃, then injecting the impregnating asphalt into the impregnating tank, applying a pressure of 1.5-5.0 MPa for impregnating operation, and discharging the impregnated blank from the tank after the duration of 20-30 hours to obtain an impregnated blank;
9) Loading the impregnated blank into a roasting furnace, heating to 750 ℃ by adopting a bare burning process, cooling to 200 ℃ and discharging to obtain a secondary roasting blank;
10 Placing the secondary roasting blank into an Acheson graphitizing furnace, filling the periphery and the furnace bottom of a furnace chamber with heat preservation materials and resistance materials, electrifying and heating to 2400 ℃, introducing halogen gas at a high temperature stage for purification, slowly cooling the product to below 100 ℃, and discharging to obtain the high-strength fine-particle isostatic graphite.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.

Claims (12)

1. The invention relates to a preparation technology of high-strength fine particle isostatic pressing graphite, and the implementation process of the invention is described below with reference to figure 1.
1) The true density is more than 1.90g/cm 3 Petroleum coke or asphalt coke with volatile matter content less than 0.5%, sulfur content less than 0.5%, water content less than 0.5%, ash content less than 0.5% and powder resistivity of 300-800 [ mu ] ohm.m is used as the material for producing isostatic pressure graphite.
2) Crushing the raw coke by a crusher to obtain granules with the particle size of less than 10mm, and grinding by a Raymond mill to obtain coke powder with the average particle size of 50-60 mu m;
3) Grinding the 50-60 mu m of coke powder by using a vertical superfine grinding machine, and obtaining primary dust collecting powder with average particles of 12-20 mu m and secondary dust collecting powder with average particles of 3-8 mu m by using a secondary dust collecting process;
4) Further, the primary dust collection powder and the secondary dust collection powder are prepared according to the proportion of (60.0-80.0) wt% to (40.0-20.0) wt%, and are mixed for 1.5-3.0 h by a three-dimensional rotary mixer, and then are screened by a 200-mesh vibrating screen with an ultrasonic function, so that powder with average particle size of 10-13 mu m and stable distribution is obtained as raw material powder for producing fine-particle isostatic graphite materials;
5) Preheating the powder with the particle size of 10-13 mu m and stable distribution to 200-220 ℃ in a raw material bin with material heating and conveying functions, and simultaneously heating the powder with the softening point of 160-180 ℃ and coking value of more than 60% and true density of more than 1.25g/cm 3 Heating high-temperature asphalt with 45-60% volatile matter and less than 0.5% ash content in a melting tank to 230 ℃ to fully melt the asphalt, adding the raw material powder and the high-temperature asphalt into a kneader with powerful kneading capacity according to the ratio of (1.8-2.3) to 1 for pressurizing and kneading, controlling the kneading temperature to be 225-230 ℃ and the kneading time to be 1.5-4.0 h under the pressurizing pressure of 60.0-100.0 MPa, cooling the kneaded paste to 50 ℃ in a cooling pot at the speed of 10-30 ℃/h, and crushing by a hammer crusherThe paste powder is fed into a paste mill for secondary milling until the size is less than 10mm, and the paste powder with the average granularity of 15-60 mu m is obtained;
6) Filling the obtained paste powder into a rubber mold with a special size, filling the rubber mold into a porous steel mold, sealing and vacuumizing the whole body after being treated by a high-frequency vibration compacting process for 1-5 h, and hanging the whole body of the steel mold into a cylinder diameter after the completion of the vacuumizing
Figure FSA0000256898570000011
Isostatic compaction is carried out in a cold isostatic press with the molding pressure of 100-180 MPa, and the density of 1.50-1.60 g/cm is obtained 3 Is a green body of (c);
7) Filling the pressed green compact into a steel tank, filling the steel tank and the pressed green compact with filling materials with the particle range of 0-3 mm, vibrating and compacting, then filling the steel tank and the pressed green compact into a roasting furnace, roasting at the heating rate of 0.1-2.8 ℃/h to fully carbonize the steel tank and introducing inert protective gas in the process, and roasting the total heating curve time is more than 800 hours.
8) Loading the carbonized baked blank into an impregnating tank, heating impregnating asphalt with a softening point of 90-120 ℃ and a quinoline insoluble content of less than 2.0% to 190 ℃, then injecting the impregnating asphalt into the impregnating tank, applying a pressure of 1.5-5.0 MPa for impregnating operation, and discharging the impregnated blank from the tank after the duration of 20-30 hours to obtain an impregnated blank;
9) Loading the impregnated blank into a roasting furnace, heating to 750 ℃ by adopting a bare burning process, cooling to 200 ℃ and discharging to obtain a secondary roasting blank;
2. and (3) filling the secondary roasting blank into an Acheson graphitizing furnace, filling the periphery and the furnace bottom of a furnace chamber with heat preservation materials and resistance materials, electrifying and heating to 1800-2400 ℃, introducing halogen gas at a high temperature stage for purification, slowly cooling the product to below 100 ℃, and discharging to obtain the high-strength fine-particle isostatic graphite.
3. The method of claim 1, wherein step 1) is carried out with a true density of > 1.90g/cm 3 Petroleum coke or asphalt coke is used as raw material for producing isostatic pressure graphite.
4. A method according to claim 1, characterized in that step 2) is performed by pulverizing the coke powder into an average particle size of 50-60 μm.
5. The method of claim 1, wherein step 3) uses a secondary dust collection process to obtain primary dust collection powder with average particles of 12-20 μm and secondary dust collection powder with average particles of 3-8 μm.
6. The method of claim 1, wherein in the step 4), the primary dust collecting powder and the secondary dust collecting powder are prepared according to the proportion of (60.0-80.0) wt% to (40.0-20.0) wt%, and are screened by a 200-mesh vibrating screen with an ultrasonic function, so that powder with average particle size of 10-13 μm and stable distribution is obtained as raw material powder for producing fine-particle isostatic pressing graphite materials.
7. The method according to claim 1, wherein step 5) yields a paste powder having an average particle size of 15 to 60 μm.
8. The method of claim 1, wherein step 6) is carried out at a molding pressure of 100 to 180MPa to obtain a density of 1.50 to 1.60g/cm 3 Is a green body of (c).
9. The method of claim 1, wherein the step 7) is performed with a heating rate of 0.1-2.8 ℃/h to fully carbonize for more than 800 hours.
10. The method of claim 1, wherein in step 8), the impregnating operation is performed by applying a pressure of 1.5 to 5.0MPa for 20 to 30 hours, and then the impregnated blank is obtained by discharging from the tank.
11. The method of claim 1, wherein step 9) adopts a bare firing process to raise the temperature to 750 ℃, then cools the bare firing process to 200 ℃ and discharges the bare firing process to obtain a secondary roasting blank.
12. The method of claim 1, wherein step 10) is carried out by charging the secondary baked blank into an Acheson graphitizing furnace, heating to 1800-2400 ℃, introducing halogen gas at high temperature stage for purifying, and obtaining high-strength fine-particle isostatic graphite.
CN202111304053.9A 2021-11-05 2021-11-05 Preparation method of high-strength fine-particle isostatic graphite material Pending CN116081613A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116903373A (en) * 2023-07-28 2023-10-20 鄯善隆盛碳素制造有限公司 Graphitized furnace end guard plate processing technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116903373A (en) * 2023-07-28 2023-10-20 鄯善隆盛碳素制造有限公司 Graphitized furnace end guard plate processing technology

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