CN116253565A - Large-specification isostatic pressing graphite cylinder material and preparation method thereof - Google Patents
Large-specification isostatic pressing graphite cylinder material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 239000010439 graphite Substances 0.000 title claims abstract description 68
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 68
- 238000000462 isostatic pressing Methods 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 239000000571 coke Substances 0.000 claims abstract description 59
- 238000000227 grinding Methods 0.000 claims abstract description 39
- 238000004898 kneading Methods 0.000 claims abstract description 39
- 229920001971 elastomer Polymers 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims description 37
- 229910001220 stainless steel Inorganic materials 0.000 claims description 34
- 239000010935 stainless steel Substances 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 30
- 238000005470 impregnation Methods 0.000 claims description 22
- 238000007873 sieving Methods 0.000 claims description 20
- 238000005087 graphitization Methods 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 238000011049 filling Methods 0.000 claims description 13
- 239000013590 bulk material Substances 0.000 claims description 12
- 238000010000 carbonizing Methods 0.000 claims description 12
- 239000002006 petroleum coke Substances 0.000 claims description 12
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 230000004584 weight gain Effects 0.000 claims description 10
- 235000019786 weight gain Nutrition 0.000 claims description 10
- 239000011300 coal pitch Substances 0.000 claims description 9
- 239000007849 furan resin Substances 0.000 claims description 9
- 238000005056 compaction Methods 0.000 claims description 8
- 239000006253 pitch coke Substances 0.000 claims description 8
- 239000012774 insulation material Substances 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920003002 synthetic resin Polymers 0.000 claims description 4
- 239000000057 synthetic resin Substances 0.000 claims description 4
- 238000004939 coking Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 239000007770 graphite material Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims 4
- 239000006004 Quartz sand Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 239000011294 coal tar pitch Substances 0.000 description 10
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011325 microbead Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 101150114468 TUB1 gene Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000000945 filler Substances 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention relates to a large-specification isostatic pressing graphite cylinder material and a preparation method thereof, wherein the raw materials comprise 50-80 parts of secondary coke, 30-60 parts of binder and 0-10 parts of high-purity flake graphite powder by weight. Mixing secondary coke with high-purity flake graphite powder, adding a binder optimized by raw materials, kneading, cooling, granulating, grinding, and placing into a rubber sleeve with a special structure, wherein the rubber sleeve can ensure that isostatic pressures in the inner and outer directions are received in the subsequent isostatic pressing process, so that the internal and external uniformity of isostatic pressure graphite is improved, the product quality is improved, and finally, on the basis of obtaining an isostatic pressure graphite cylinder material with larger size by using optimized roasting and graphitizing processes, the structure is compact, the uniformity, the volume density, the mechanical strength and the isotropy are improved.
Description
Technical Field
The invention relates to the technical field of graphite materials, in particular to a preparation method of a large-specification isostatic pressing graphite cylinder material.
Background
Isostatic pressure graphite refers to a graphite product with high strength, high density and high purity, also called as three-high graphite and special graphite, and is widely applied to the industrial fields of metallurgy, chemical industry, aerospace, electronics, machinery, nuclear energy and the like. Especially, the large-size high-quality isostatic pressing graphite is used as an alternative material, has very wide application space in the fields of high technology and new technology, has wide application prospect, and is praised as the most promising material in centuries.
In recent years, with the development of Chinese manufacturing, particularly the photovoltaic power generation reaches the condition of low price and internet surfing, the technology of the photovoltaic industry is iterated continuously, a Czochralski silicon single crystal thermal field is rapidly updated from an original 28-inch thermal field to a 36-inch thermal field and a 40-inch thermal field, and a large-specification isostatic pressing graphite cylinder material is required to be processed and manufactured into a heat preservation barrel, a heater and the like. All the requirements have high requirements on the specification of isostatic graphite, a 40-inch single crystal thermal field needs an isostatic graphite cylinder material with the specification of phi 1200 multiplied by 1000mm, and certain graphite thermal field components need to be coated on the surface, so that the thermal expansion coefficient of the coating material is required to be close to that of a graphite substrate, and the coating falling off caused by repeated temperature rise and drop of the thermal field components is avoided.
In summary, the larger the specification of the isostatic graphite is, the finer the granularity is, the more difficult the production is, and the larger the requirement on production equipment is. The existing isostatic pressing graphite production process is developed based on the high-purity flake graphite powder production process, and the produced isostatic pressing graphite cannot meet the requirements of the photovoltaic industry and other industries on the isostatic pressing graphite in the aspects of size, strength, isotropy degree and the like, so that the stable and high-speed development of the photovoltaic industry in China is directly affected.
Disclosure of Invention
In order to further improve the product quality of the isostatic pressing graphite, the invention provides a large-size isostatic pressing graphite cylinder material and a preparation method thereof, and the isostatic pressing graphite with larger size, compact structure, good uniformity, high volume density, high mechanical strength and high isotropy is obtained by optimizing raw material powder and an optimized binder formula and using more advanced roasting and graphitizing processes and a special rubber sleeve structure.
The technical scheme adopted by the invention is as follows:
the large-specification isostatic pressing graphite cylinder material comprises the following raw materials in parts by weight: 50-80 parts of secondary coke, 30-60 parts of binder and 0-10 parts of high-purity crystalline flake graphite powder.
Preferably, the low ash calcined pitch coke: the fixed carbon content is more than or equal to 99 percent, the ash content is less than or equal to 0.5 percent, the water content is less than or equal to 0.3 percent, and the sulfur content is less than or equal to 0.3 percent;
low ash petroleum coke: the fixed carbon content is more than or equal to 99 percent, the ash content is less than or equal to 0.5 percent, the water content is less than or equal to 0.5 percent, and the sulfur content is less than or equal to 0.5 percent;
mesophase carbon microbeads: d50:20-50um, volatile matter: 12-15%, ash content less than or equal to 0.5%, toluene insoluble matter more than or equal to 95%, quinoline insoluble matter more than or equal to 95%;
further, the raw material of the secondary coke is at least one of low ash content calcined pitch coke, low ash content petroleum coke and mesophase carbon microspheres.
Further, the secondary coke is obtained by sequentially carrying out the working procedures of grinding, kneading, secondary grinding, profiling and roasting on the raw materials.
In a specific embodiment, the grinding is specifically that a Raymond mill is adopted to grind low ash calcined pitch coke, low ash petroleum coke and mesophase carbon microspheres respectively, and parameters of the powder are controlled by a winnowing classifier: d50 is 10-20um, and D3 is more than or equal to 0.5um; d97 is less than or equal to 30um.
The kneading is specifically to add the raw materials in proportion for kneading, wherein the kneading temperature is 190-380 ℃ and the kneading time is 80-300min, so as to prepare the mixed bulk material with certain plasticity.
The secondary grinding is specifically to granulate the mixed bulk materials by a high-speed cooling mixer, and then crush the mixed bulk materials to 300 meshes of powder by a mechanical crusher to prepare pressed powder.
The compacting is to put the compacting powder obtained by secondary grinding into a cylindrical steel mould with the diameter of 500-900mm, to stand and exhaust, to vibrate for 10-30s, to balance weight for 20-50kg, to be compacted under the pressure of 30-70MPa for 10-50min, to obtain the green compact.
The roasting is specifically to put the prepared green body into a stainless steel crucible, wherein quartz sand is used as a filling material at the bottom and the side, the filling thickness is 80-200mm, fine coke powder is covered at the top and used as a heat insulation material, and the filling thickness is 150-300mm. And (3) placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing. The temperature difference in the car bottom furnace is controlled to be 50-100 ℃, the roasting highest temperature is 900-1200 ℃, and the roasting time is 60-100 days.
Preferably, in the secondary coke, the mass percentage of fixed carbon is more than or equal to 99%, the mass percentage of ash is less than or equal to 0.5%, the mass percentage of moisture is less than or equal to 0.5%, and the thermal expansion coefficient (room temperature-600 ℃) is the same as that of the secondary coke: 4-5×10 -6 /℃。
Preferably, the binder is coal tar pitch, the mass percentage of ash content of the coal tar pitch is less than or equal to 0.5%, the mass percentage of volatile matters is 45% -70%, the coking value is 55% -65%, the softening point is 80-220 ℃, the mass percentage of quinoline insoluble matters is 10% -30%, and the mass percentage of toluene insoluble matters is 25% -55%.
Preferably, the binder is a synthetic resin.
Preferably, the adhesive is at least one of furan resin, phenolic resin and epoxy resin.
Preferably, the binder is a mixture of coal pitch and synthetic resin in a 1:1-4:1 composition.
Preferably, the high-purity flake graphite powder is prepared from fixed carbon with a mass percentage of more than or equal to 99%, ash with a mass percentage of less than or equal to 0.5% and water with a mass percentage of less than or equal to 0.5%.
The invention also provides a preparation method of the large-specification isostatic pressing graphite cylinder material, which comprises the following steps:
s1, placing secondary coke and high-purity flake graphite powder into a ball mill for mixing and grinding, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor;
s2, adding a binder into the aggregate precursor for kneading to obtain a mixed bulk material;
s3, placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder;
s4, filling the pressed powder into a rubber membrane tool, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic compaction to obtain a green body;
s5, placing the green body into a stainless steel crucible, placing filling materials between the green body and the bottom and side parts of a stainless steel clamp pot, covering a heat insulation material on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasted product;
s6, impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a finished product of the large-specification isostatic pressing graphite cylinder.
Preferably, in step S1, the aggregate precursor particle size is 20um-40um.
Preferably, in the step S2, the kneading temperature is 220-280 ℃, and the kneading time is 150-180 min.
Preferably, in the step S4, the isostatic pressing pressure is 140MPa-180MPa, and the dwell time is 120min-150min.
Preferably, in the step S5, the temperature difference in the car bottom furnace is controlled to be 5-10 ℃, the roasting maximum temperature is 1000-10500 ℃, and the roasting time is 80-90 days.
Preferably, in step S5, the filler is quartz sand, and the thermal insulation material is fine coke powder.
Preferably, in the step S5, the thickness of the filling material is 1500-180mm, and the thickness of the heat insulation material is 200-250mm.
Preferably, in the step S6, the impregnation pressure is 5-10MPa, the impregnation preheating temperature is 300-350 ℃, the impregnation temperature is 400-500 ℃, and the weight gain rate after impregnation is 7-20%.
Preferably, the high temperature graphitization temperature is 2700 ℃ to 2800 ℃ for 60 days to 70 days.
Preferably, in step S4, the rubber mold is a hollow cylinder, and includes an outer film barrel (1) and a barrel cover (2), the outer film barrel (1) is a hollow cylindrical barrel structure, and the barrel cover (2) is covered on the outer film barrel (1); an inner pressure pipe (4) is vertically arranged in the middle part in the outer film barrel (1), and the inner pressure pipe (4) is of a hollow tubular structure; the barrel cover (2) is provided with an air vent (3), after the barrel cover (2) is put, the air vent (3) can be communicated with the internal pressure pipe (4), and the air vent (3) is provided with an air valve (5).
The preparation methodThe diameter of the large-specification isostatic pressing graphite cylinder prepared by the method can reach 1300-1500mm, and the height is 800-1000 mm. The volume density of the large-specification isostatic pressing graphite material cylinder is 1.75-1.90g/cm 3 The breaking strength is 40-55MPa, the compressive strength is 80-100MPa, the tensile strength is 26-32MPa, the room temperature heat conductivity is 110-127W/mK, the ash content is 180-400ppm, and the fracture toughness is 0.5-1.05 MPa.m 1/2 The isotropy is 1.05-1.08.
The beneficial effects of the invention are as follows:
the isostatic pressing graphite cylinder material is preferably raw material powder, adopts secondary coke, high-purity flake graphite powder and an adhesive as raw materials, optimizes the adhesive formula, creatively uses artificial resins such as furan resin, phenolic resin, epoxy resin and the like as the adhesive, and particularly uses the artificial resins and coal tar pitch together as the adhesive, and the synergistic effect between the artificial resins and the coal tar pitch effectively improves compactness and uniformity.
The pretreatment of the secondary coke greatly improves the mixing uniformity of the raw materials and improves the stability of the thermal expansion coefficient of the finished product. Further, the secondary coke and the high-purity flake graphite powder are mixed, added with a binder for kneading, cooled and granulated, ground and placed into a rubber sleeve with a special structure, and the rubber sleeve can be stressed internally and externally in the subsequent isostatic compaction process, so that the blank is subjected to isostatic pressures in the internal and external directions, the internal and external uniformity of the isostatic pressure graphite is improved, the product quality is improved, and finally, the structure is compact, the uniformity, the volume density, the mechanical strength and the isotropy are improved on the basis of obtaining the isostatic pressure graphite cylinder material with larger size by using an optimized roasting and graphitizing process.
Drawings
FIG. 1 is a schematic view of a rubber mold according to the present invention.
Reference numerals: 1-an outer membrane barrel, 2-a barrel cover, 3-an air vent, 4-an inner pressure pipe and 5-an air valve.
Detailed Description
The present invention will be described in detail with reference to specific embodiments and drawings.
Raw material standard used in the examples:
coal pitch: the ash content is 0.03% by mass, the volatile content is 60% by mass, the coking value is 60%, the softening point is 200 ℃, the mass percentage of quinoline insoluble is 10%, and the mass percentage of toluene insoluble is 30%.
High-purity flake graphite powder: the mass percentage of the fixed carbon is 99.6%, the mass percentage of the ash is 0.3%, and the mass percentage of the water is 0.1%.
Low ash calcined pitch coke: fixed carbon content 99%, ash content 0.5%, moisture content 0.3%, sulfur content 0.2%;
low ash petroleum coke: fixed carbon content 99%, ash content 0.5%, moisture content 0.3%, sulfur content 0.2%;
mesophase carbon microbeads: d50:20-50um, 13 percent of volatile matter, 0.3 percent of ash, more than or equal to 95 percent of toluene insoluble matters and more than or equal to 95 percent of quinoline insoluble matters.
Example 1: rubber mould
As shown in fig. 1, the rubber mold is a hollow cylinder and comprises an outer film barrel 1 and a barrel cover 2, wherein the outer film barrel 1 is of a cylindrical hollow barrel-shaped structure, and the barrel cover 2 is covered on the outer film barrel 1. The outer film tub 1 and the tub cover 2 are sealably coupled.
The inner middle part of the outer membrane barrel 1 is vertically provided with an inner pressure pipe 4, and the inner pressure pipe 4 is of a hollow tubular structure; the barrel cover 2 is provided with an air vent 3, the air vent 3 can be communicated with the internal pressure pipe 4 after the barrel cover 2 is covered, and the air vent 3 is provided with an air valve 5.
When the novel inner-pressure barrel is used, materials are placed between the outer film barrel 1 and the inner pressure pipe 4, liquid can be introduced into the inner pressure pipe 4, and due to the fact that rubber materials are adopted, certain pressure can be generated on the materials in the barrel through elastic deformation.
Example 2: preparation of secondary coke
In the embodiment, the raw materials of the secondary coke adopt low ash content calcined asphalt coke and low ash content petroleum coke, and the mass ratio of the low ash content calcined asphalt coke to the low ash content petroleum coke is 1:1.
the preparation process of the secondary coke comprises the following steps:
grinding: grinding the low ash calcined asphalt coke and the low ash petroleum coke by adopting a Raymond mill, and controlling parameters of powder by a winnowing classifier: d50 is 10-20um, and D3 is more than or equal to 0.5um; d97 is less than or equal to 30um.
Kneading: and (3) adding the milled low-ash calcined asphalt coke and the low-ash petroleum coke in proportion for kneading, wherein the kneading temperature is 300 ℃, and the kneading time is 300 minutes, so as to prepare the mixed bulk material with certain plasticity.
Secondary grinding: granulating the mixed bulk materials by a high-speed cooling mixer, and crushing the mixed bulk materials to 300-mesh powder by a mechanical crusher to obtain pressed powder.
Profiling: putting the pressed powder into a cylindrical steel mold with the diameter of 800mm, standing and exhausting, vibrating for 30s, balancing weight for 45kg, and performing compression molding under the molding pressure of 60MPa for 45min to obtain a green body.
Roasting: and placing the prepared green body into a stainless steel crucible, wherein quartz sand is used as a filling material at the bottom and the side, the filling thickness is 180mm, fine coke powder is covered at the top and used as a heat insulation material, and the filling thickness is 200mm. And (3) placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing. The temperature difference in the car bottom furnace is 50 ℃, the roasting highest temperature is 1200 ℃, and the roasting time is 90 days.
The secondary coke prepared in this example has a fixed carbon content of 99.3% by mass, an ash content of 0.3% by mass, a moisture content of 0.3% by mass, and a thermal expansion coefficient (room temperature-600 ℃) of 4.5X10 -6 /℃。
Example 3: preparation of secondary coke
In the embodiment, the raw materials of the secondary coke adopt low ash content calcined pitch coke, low ash content petroleum coke and intermediate phase carbon microspheres, and the mass ratio of the low ash content calcined pitch coke to the low ash content petroleum coke to the intermediate phase carbon microspheres is 3:1:1. the procedure and parameters for the preparation of secondary coke were the same as in example 2.
The secondary coke prepared in this example has a mass% of fixed carbon of 99%, a mass% of ash of 0.6%, a mass% of moisture of 0.4% and a thermal expansion coefficient (room temperature-600 ℃) of 4.8X10 -6 /℃。
Example 4: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 70:8. the secondary coke used in this example was the secondary coke prepared in example 3.
(2) Adding coal tar pitch into the aggregate precursor for kneading, wherein the mass ratio of the aggregate precursor to the coal tar pitch is 78:50; the mixing and kneading temperature is 250 ℃, the mixing and kneading time is 165min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) Placing the pressed powder into a rubber membrane, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic pressing to obtain a green blank, wherein the isostatic pressing pressure is 160MPa, and the pressure maintaining time is 130min. The rubber film used in this example was the rubber mold described in example 1.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 160mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 230mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 85 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 8MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 450 ℃, the weight gain rate after impregnation is 10%, the high-temperature graphitization temperature is 2700 ℃ and the time is 60 days, and thus the large-specification isostatic pressing graphite cylinder finished product is obtained.
Example 5: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 70:8. the secondary coke used in this example was the secondary coke prepared in example 3.
(2) Adding furan resin into the aggregate precursor for kneading, wherein the mass ratio of the aggregate precursor to the furan resin is 78:50; the mixing and kneading temperature is 250 ℃, the mixing and kneading time is 165min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) Placing the pressed powder into a rubber membrane, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic pressing to obtain a green blank, wherein the isostatic pressing pressure is 160MPa, and the pressure maintaining time is 130min. In this example, the rubber mold described in example 1 was used.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 160mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 230mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 85 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 8MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 450 ℃, the weight gain rate after impregnation is 10%, the high-temperature graphitization temperature is 2700 ℃ and the time is 60 days, so as to obtain the large-specification isostatic pressing graphite cylinder finished product.
Example 6: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 70:8. the secondary coke used in this example was the secondary coke prepared in example 2.
(2) Adding coal pitch and furan resin into the aggregate precursor according to the mass ratio of 2:1, kneading the mixed binder, wherein the mass ratio of the aggregate precursor to the binder is 78:50; the mixing and kneading temperature is 250 ℃, the mixing and kneading time is 165min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) Placing the pressed powder into a rubber membrane, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic pressing to obtain a green blank, wherein the isostatic pressing pressure is 160MPa, and the pressure maintaining time is 130min. In this example, the rubber mold described in example 1 was used.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 160mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 230mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 85 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 8MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 450 ℃, the weight gain rate after impregnation is 10%, the high-temperature graphitization temperature is 2700 ℃ and the time is 60 days, so as to obtain the large-specification isostatic pressing graphite cylinder finished product.
Example 7: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 70:8. the secondary coke used in this example was the secondary coke prepared in example 2.
(2) Adding coal pitch, furan resin and phenolic resin into an aggregate precursor according to the mass ratio of 2:1:1, kneading the mixed binder, wherein the mass ratio of the aggregate precursor to the binder is 78:50; the mixing and kneading temperature is 250 ℃, the mixing and kneading time is 165min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) Placing the pressed powder into a rubber membrane, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic pressing to obtain a green blank, wherein the isostatic pressing pressure is 160MPa, and the pressure maintaining time is 130min. In this example, the rubber mold described in example 1 was used.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 160mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 230mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 85 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 8MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 450 ℃, the weight gain rate after impregnation is 10%, the high-temperature graphitization temperature is 2700 ℃ and the time is 60 days, so as to obtain the large-specification isostatic pressing graphite cylinder finished product.
Example 8: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30um-40um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 50:5. the secondary coke used in this example was the secondary coke prepared in example 2.
(2) Adding coal pitch and furan resin into an aggregate precursor according to the mass ratio of 1:1, kneading the mixed binder, wherein the mass ratio of the aggregate precursor to the binder is 55:30; the mixing and kneading temperature is 220 ℃, the mixing and kneading time is 150min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) Placing the pressed powder into a rubber membrane, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic pressing to obtain a green blank, wherein the isostatic pressing pressure is 140MPa, and the pressure maintaining time is 120min. In this example, the rubber mold described in example 1 was used.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 150mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 200mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 80 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 5MPa, the impregnating preheating temperature is 300 ℃, the impregnating temperature is 400 ℃, the weight gain rate after impregnation is 7%, the high-temperature graphitization temperature is 2700 ℃, and the time is 60 days, so as to obtain the large-specification isostatic pressing graphite cylinder finished product.
Example 9: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 80:10. the secondary coke used in this example was the secondary coke prepared in example 2.
(2) Adding coal pitch and furan resin into an aggregate precursor according to the mass ratio of 1:1, kneading the mixed binder, wherein the mass ratio of the aggregate precursor to the binder is 90:60; the mixing and kneading temperature is 280 ℃, the mixing and kneading time is 180 minutes, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) Placing the pressed powder into a rubber membrane, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic pressing to obtain a green blank, wherein the isostatic pressing pressure is 180MPa, and the pressure maintaining time is 150min. In this example, the rubber mold described in example 1 was used.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 180mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 250mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 10 ℃, the roasting maximum temperature range is 1050 ℃, and the roasting time is 90 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 10MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 500 ℃, the weight gain rate after impregnation is 20%, the high-temperature graphitization temperature is 2800 ℃ and the time is 70 days, so as to obtain the large-specification isostatic pressing graphite cylinder finished product.
Comparative example 1: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 70:8. the secondary coke used in this example was the secondary coke prepared in example 3.
(2) Adding coal tar pitch into the aggregate precursor for kneading, wherein the mass ratio of the aggregate precursor to the coal tar pitch is 78:50; the mixing and kneading temperature is 250 ℃, the mixing and kneading time is 165min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) And (3) filling the pressed powder into a rubber mold, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic compaction to obtain a green body, wherein the isostatic compaction pressure is 160MPa, and the dwell time is 130min. The rubber mold used in this example was a conventional rubber mold, i.e., a mold of a barrel-like structure, and the material was placed in a barrel-shaped grinder, and the main difference from the rubber mold of example 1 was the absence of an internal pressure tube.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 160mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 230mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 85 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 8MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 450 ℃, the weight gain rate after impregnation is 10%, and the high-temperature graphitization temperature is 2700 ℃ and the time is 60 days.
Comparative example 2: preparation of large-size isostatic pressing graphite cylinder
(1) Mixing and grinding the secondary coke and the high-purity flake graphite powder in a ball mill, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor, wherein the granularity of the aggregate precursor is 30-40 um, and the mass ratio of the secondary coke to the high-purity flake graphite powder is 70:8. the secondary coke used in this example was the secondary coke prepared in example 3.
The secondary coke adopted in the embodiment is low ash content calcined pitch coke, low ash content petroleum coke and mesophase carbon microsphere according to the mass ratio of 3:1:1, mixing the obtained mixture.
(2) Adding coal tar pitch into the aggregate precursor for kneading, wherein the mass ratio of the aggregate precursor to the coal tar pitch is 78:50; the mixing and kneading temperature is 250 ℃, the mixing and kneading time is 165min, and finally the mixed bulk material is obtained.
(3) And (3) placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder.
(4) And (3) filling the pressed powder into a rubber mold, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic compaction to obtain a green body, wherein the isostatic compaction pressure is 160MPa, and the dwell time is 130min. The rubber mold used in this example was a conventional rubber mold, i.e., a mold of a barrel-like structure, and the material was placed in a barrel-shaped grinder, and the main difference from the rubber mold of example 1 was the absence of an internal pressure tube.
(5) Placing the green body into a stainless steel crucible, placing quartz sand with the thickness of 160mm between the green body and the bottom and the side parts of a stainless steel clamp pot, covering fine coke powder with the thickness of 230mm on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasting product, wherein the temperature difference in the car bottom furnace is 5 ℃, the roasting maximum temperature range is 1000 ℃, and the roasting time is 85 days.
(6) And (3) impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a large-specification isostatic pressing graphite cylinder finished product, wherein the impregnating pressure is 8MPa, the impregnating preheating temperature is 350 ℃, the impregnating temperature is 450 ℃, the weight gain rate after impregnation is 10%, and the high-temperature graphitization temperature is 2700 ℃ and the time is 60 days.
The large format isostatic graphite cylinders obtained in examples 4-9 and comparative examples 1 and 2 were tested and the results are shown in table 1.
The method for testing the volume density comprises the following steps: GB/T24528-2009 carbon material volume density measuring method;
the method for testing the flexural strength comprises the following steps: GB/T3074.1-2008 graphite electrode flexural strength measuring method;
the method for testing the compressive strength comprises the following steps: GB/T1431-2019 carbon material compressive strength determination method;
the test method of the thermal expansion coefficient comprises the following steps: GB/T3074.4-2016 graphite electrode Coefficient of Thermal Expansion (CTE) determination method;
the method for testing the room temperature thermal conductivity comprises the following steps: a method for measuring the heat conductivity coefficient of a GB/T8722-2019 carbon material;
the ash testing method comprises the following steps: GB/T1429-2009 carbon material ash content determination method;
the fracture toughness test method comprises the following steps: GB/T38338-2019 carbon material fracture toughness determination method;
the isotropy test method comprises the following steps: standard specifications for ASTM D7219-2014 isotropic and near-isotropic nuclear graphite.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The large-specification isostatic pressing graphite cylinder material is characterized by comprising the following raw materials in parts by weight: 50-80 parts of secondary coke, 30-60 parts of binder and 0-10 parts of high-purity crystalline flake graphite powder.
2. The large format isostatic graphite cylinder as claimed in claim 1, wherein the secondary coke is at least one of low ash calcined pitch coke, low ash petroleum coke and mesophase carbon microsphere.
3. The large-size isostatic pressing graphite cylinder material according to claim 1, wherein the binder is coal pitch, the mass percentage of ash content of the coal pitch is less than or equal to 0.5%, the mass percentage of volatile matters is 45% -70%, the coking value is 55% -65%, the softening point is 80-220 ℃, the mass percentage of quinoline insoluble matters is 10% -30%, and the mass percentage of toluene insoluble matters is 25% -55%.
4. The large format isostatic pressing graphite cylinder as recited in claim 1, wherein the binder is a synthetic resin, preferably the binder is at least one of furan resin, phenolic resin, epoxy resin.
5. The large format isostatic graphite cylinder as claimed in claim 1, wherein the binder is a mixture of coal pitch and synthetic resin in the ratio of 1:1-4:1.
6. The method for preparing the large-size isostatic pressing graphite cylinder material as claimed in claim 1, comprising the following steps:
s1, placing secondary coke and high-purity flake graphite powder into a ball mill for mixing and grinding, and sieving with a 300-mesh sieve after grinding to obtain an aggregate precursor;
s2, adding a binder into the aggregate precursor for kneading to obtain a mixed bulk material;
s3, placing the mixed bulk materials into a high-speed cooler, cooling, granulating, transferring into a ball mill, grinding, and sieving with a 200-mesh sieve to obtain pressed powder;
s4, filling the pressed powder into a rubber membrane tool, standing, exhausting, vibrating, sealing, vacuumizing, and performing isostatic compaction to obtain a green body;
s5, placing the green body into a stainless steel crucible, placing filling materials between the green body and the bottom and side parts of a stainless steel clamp pot, covering a heat insulation material on the top of the green body, and then placing the stainless steel crucible with the green body into a car bottom furnace with uniform temperature field for roasting and carbonizing to obtain a roasted product;
s6, impregnating the roasted product with an impregnant, and carrying out high-temperature graphitization treatment after impregnation to obtain a finished product of the large-specification isostatic pressing graphite cylinder.
7. The method for preparing the large-size isostatic pressing graphite cylinder material as claimed in claim 6, wherein the method comprises the following steps: in the step S4, the isostatic compaction pressure is 140MPa-180MPa, and the dwell time is 120min-150min.
8. The method for preparing large-sized isostatic pressing graphite cylinder material according to claim 6, wherein in the step S6, the dipping pressure is 5-10MPa, the dipping preheating temperature is 300-350 ℃, the dipping temperature is 400-500 ℃, and the weight gain rate after dipping is 7% -20%.
9. The method for preparing the large-size isostatic pressing graphite cylinder material as claimed in claim 6, wherein the method comprises the following steps: in the step S4, the rubber mold is a hollow cylinder and comprises an outer film barrel (1) and a barrel cover (2), wherein the outer film barrel (1) is of a cylindrical hollow barrel-shaped structure, and the barrel cover (2) is covered on the outer film barrel (1); an inner pressure pipe (4) is vertically arranged in the middle part in the outer film barrel (1), and the inner pressure pipe (4) is of a hollow tubular structure; the barrel cover (2) is provided with an air vent (3), after the barrel cover (2) is put, the air vent (3) can be communicated with the internal pressure pipe (4), and the air vent (3) is provided with an air valve (5).
10. The method for preparing the large-size isostatic pressing graphite cylinder material as claimed in claim 6, wherein the method comprises the following steps: the diameter of the large-specification isostatic pressing graphite cylinder is 1300-1500mm, and the height is 800-1000 mm; the volume density of the large-specification isostatic pressing graphite material cylinder is 1.75-1.90g/cm 3 The breaking strength is 40-55MPa, the compressive strength is 80-100MPa, the tensile strength is 26-32MPa, the room temperature heat conductivity is 110-127W/mK, the ash content is 180-400ppm, and the fracture toughness is 0.5-1.05 MPa.m 1/2 The isotropy is 1.05-1.08.
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| CN117550896A (en) * | 2024-01-12 | 2024-02-13 | 山东红点新材料有限公司 | High-strength high-purity isostatic graphite and preparation method thereof |
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