CN114213127A - Preparation method of graphite crucible - Google Patents
Preparation method of graphite crucible Download PDFInfo
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- CN114213127A CN114213127A CN202111672612.1A CN202111672612A CN114213127A CN 114213127 A CN114213127 A CN 114213127A CN 202111672612 A CN202111672612 A CN 202111672612A CN 114213127 A CN114213127 A CN 114213127A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 239000010439 graphite Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 41
- 239000002006 petroleum coke Substances 0.000 claims abstract description 41
- 238000004898 kneading Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 239000011300 coal pitch Substances 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000012774 insulation material Substances 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 28
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 239000011810 insulating material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000007906 compression Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000010426 asphalt Substances 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000007580 dry-mixing Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 238000007731 hot pressing Methods 0.000 abstract description 4
- 238000002679 ablation Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 230000035939 shock Effects 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract description 2
- 238000000641 cold extrusion Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000004904 shortening Methods 0.000 abstract description 2
- 239000011280 coal tar Substances 0.000 abstract 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- 238000003723 Smelting Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011329 calcined coke Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a graphite crucible, which comprises the following steps: s1, preparing raw materials: the raw materials comprise crushed graphite, Acheson furnace petroleum coke resistance material, Acheson furnace petroleum coke heat preservation material and medium temperature coal pitch; s2, batching: grinding graphite into graphite powder, mixing the graphite powder with Acheson furnace petroleum coke resistance material, Acheson furnace petroleum coke resistance material and Acheson furnace petroleum coke heat insulation material according to the mass ratio of 3:2:5, grinding the mixture into mixed powder, and mixing the mixed powder with medium-temperature coal tar, wherein the mass percent of the mixed powder is 65-85% and the mass percent of the medium-temperature coal tar is 15-35% in the mixing process; s3, kneading; s4, profiling; s5, roasting; and S6, processing. The invention adopts a hot-pressing cold-extrusion one-step forming method, the obtained product has excellent performance, and has good thermal shock resistance, ablation performance, leakage resistance and mechanical strength, and the preparation process has the advantages of energy conservation, environmental protection, period shortening and aging improvement.
Description
Technical Field
The invention relates to the technical field of graphite, in particular to a preparation method of a graphite crucible.
Background
Because graphite has the characteristics of high temperature resistance, oxidation resistance, stable chemical performance and the like, the crucible container made of graphite is widely applied to industries needing high-temperature heat treatment, such as lithium battery cathodes, purification of diamond carbon source materials, rare earth smelting, precious metal smelting and the like.
Conventionally, graphite crucibles are usually produced by machining a blank of graphite electrode. However, the method of manufacturing the crucible using the graphite electrode process has the following problems:
1. the crucible processed by the artificial graphite electrode needs to cut off the core part of the electrode, the utilization rate of the electrode is only 20-30%, the material waste is great, the product cost is high, and the crucible is not beneficial to mass use of downstream enterprises of the crucible.
2. The crucible processed by the artificial graphite electrode is limited by the forming mode and the formula of the electrode, the product structure of the crucible is anisotropic, the physical index has defects, and the quality is unstable. Particularly, when the crucible is used for smelting precious metals, the crucible has serious leakage and can not meet the use requirement.
3. The production of graphite electrodes requires calcined coke of coal series or petroleum series, and the manufacturing process of the coke not only pollutes the environment, but also has higher cost, the graphitizing process consumes about 6000kw.h of electricity per ton, and the waste of resources and energy is serious.
4. The production method of the graphite electrode has long manufacturing period and low production efficiency, and cannot meet the requirements of users.
Therefore, the preparation method of the graphite crucible is provided, so that the prepared graphite crucible has good thermal shock resistance, ablation performance, leakage resistance and mechanical strength, and is low in cost, environment-friendly and capable of recycling waste materials, and is expected in the purification and smelting industries of lithium battery negative electrode powder.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a graphite crucible, which utilizes graphite scraps, Acheson furnace petroleum coke resistance materials and Acheson furnace petroleum coke heat insulation materials generated in the electrode production process as raw materials, adopts a hot-pressing cold-extrusion one-step forming method for production, has more economic raw material proportion and more excellent product performance, and has the advantages of energy conservation, environmental protection, cycle shortening and aging improvement of the preparation process.
The technical scheme of the invention is that the preparation method of the graphite crucible comprises the following steps:
s1, preparing raw materials: the raw materials comprise graphite scraps, Acheson furnace petroleum coke resistance materials, Acheson furnace petroleum coke heat-insulating materials and medium-temperature coal pitch, wherein:
the graphite fragments meet the following requirements: the true density is more than or equal to 2.13g/cm3Ash content is less than or equal to 0.03 percent, volatile matter is less than or equal to 0.22 percent, and water content is less than or equal to 0.09 percent;
the Acheson furnace petroleum coke resistance material and the Acheson furnace petroleum coke heat-insulating material simultaneously meet the following requirements: the true density is more than or equal to 2.10g/cm3Ash content is less than or equal to 0.03 percent, volatile matter is less than or equal to 0.22 percent, and water content is less than or equal to 0.09 percent;
the medium temperature coal pitch meets the following requirements: ash content is less than or equal to 0.20 percent, volatile matter is less than or equal to 64.2 percent, and water content is less than or equal to 0.06 percent;
s2, batching: grinding graphite into graphite powder, mixing the graphite powder with the Acheson furnace petroleum coke resistance material and the Acheson furnace petroleum coke heat-preservation material according to a certain mass ratio (the preferred ratio is 3:2:5), grinding the graphite powder into mixed powder, and mixing the mixed powder with the medium-temperature coal tar pitch, wherein the mass percent of the mixed powder is 65-85% and the mass percent of the medium-temperature coal tar pitch is 15-35% in the mixing process;
s3, kneading;
s4, profiling;
s5, roasting;
and S6, processing.
Further, the graphite scraps in the step S1 are graphite electrode production waste, the acheson furnace petroleum coke resistance material and the acheson furnace petroleum coke heat preservation material are waste generated in the production of lithium battery negative electrode materials by the acheson furnace, the pass rate of the ground powder after being screened by a 200-mesh international standard sieve is 80 ± 5%, and the specific particle size comprises the following components in percentage by mass:
the proportion of 1mm granularity is 2-4%;
37-43% of granularity of 0.5-0.15 mm;
37-43% of granularity smaller than 0.075 mm;
the proportion of other particle sizes is 17-23%.
Further, the kneading in the above step S3 is to pour the ingredients into the kneading pot to stir, the kneading pot itself is heated externally by the heat transfer oil, the inside has the reamer to stir the materials, the heat transfer oil inlet temperature of the kneading pot: 230 ℃ to 233 ℃, the temperature of asphalt in the kneading pot is 162 ℃ to 165 ℃, and the dry mixing time of kneading is as follows: 40 minutes at 118-; wet mixing time of kneading: 45 minutes, temperature 162-.
Further, the pressing in step S4 is to pour the kneaded paste into a forming container, the forming container has an upper die and a lower die, the upper die and the lower die have a heating and cooling function respectively, the heating function of the upper die and the lower die is turned on, the paste is poured into the upper die to form the paste under pressure, the density of the paste is monitored, and the cooling function is turned on when the density index is reached; if the density index is not reached, repeatedly heating and pressurizing until the density index is reached; the density index range is 1.7-1.75 g/cm3(ii) a Then, carrying out a cooling compression process, wherein the tamping pressure of the cooling compression process is 20Mpa, the molding pressure is 20Mpa, and the pressing time is 4 minutes to cool the paste material to prepare a green blank; and finally, starting instantaneous secondary heating on the upper die of the forming container to demould.
Further, in the firing in the step S5, the green compact is charged into an industrial ring type firing furnace, and is heated in a reducing atmosphere in a stepwise manner according to the following temperature rise curve: 150 ℃ plus 350 ℃, the temperature rise speed is 4.4 ℃/h and the duration time is 45 h; at the temperature of 400 ℃ in 350 ℃ and the temperature rise speed of 1.7 ℃/h, the duration of 30h, at the temperature of 500 ℃ in 400 ℃, at the temperature rise speed of 1.25 ℃/h, the duration of 80h, at the temperature of 600 ℃ in 500 ℃ and the temperature rise speed of 1.8 ℃/h, the duration of 57h, at the temperature of 700 ℃ in 600 ℃, at the temperature rise speed of 3.8 ℃/h, the duration of 27h, at the temperature of 800 ℃ in 700 ℃ in 800 ℃, at the temperature rise speed of 5.0 ℃/h, at the duration of 20h, at the temperature of 1000 ℃ in 800 ℃, at the temperature rise speed of 8.0 ℃/h, at the duration of 25h, at the temperature of 1200 ℃ in 1200 ℃, at the temperature rise speed of 8.3 ℃/h, at the duration of 20h and at the temperature of 1200 ℃ in 20 h.
Compared with the prior art, the invention has the advantages that:
1. the invention adopts graphite fragments, Acheson furnace petroleum coke resistance material and Acheson furnace petroleum coke heat preservation material as raw materials, wherein the graphite fragments belong to waste materials produced by electrode production, the Acheson furnace petroleum coke resistance material and the Acheson furnace petroleum coke heat preservation material belong to filler used for purifying lithium battery negative electrode powder, the raw materials of the invention belong to the reutilization of waste materials, the average cost of each product with the same specification is low by 800 plus materials, 1000 yuan, the energy is saved, the environment is protected, and the manufacturing cost of the graphite crucible is reduced at the same time, and the method specifically comprises the following steps: in the aspect of power consumption: 3600kw of electric quantity is consumed when a graphite crucible is manufactured according to the traditional process, 240kw of electric quantity is consumed when the crucible is manufactured by the manufacturing method of the product, and 3360kw of electric energy is saved for each crucible; raw material aspect: 450kg of petroleum coke and 150kg of asphalt are consumed for manufacturing a finished crucible by the traditional process, and 150kg of waste graphite powder and 50kg of asphalt are consumed for manufacturing a finished crucible by the method; the method can save 450kg of petroleum coke of 100kg in the production of one crucible compared with the traditional mode, and the method of the invention needs electric energy, labor cost and corresponding carbon emission, accords with the low-carbon, environment-friendly and energy-saving policies proposed by the state, and makes the existing energy more fully utilized.
2. Compared with the crucible produced by the traditional graphite electrode, the invention reduces two processes of dipping and graphitization, which pollute the environment and consume energy greatly; meanwhile, compared with a graphite electrode crucible, the production period is shortened by 30-40 days on average, and the production efficiency is greatly improved while energy conservation and emission reduction are realized.
3. The graphite crucible produced by the method has different acting forces on materials due to the forming method, eliminates anisotropy in the pressing process, avoids longitudinal arrangement of aggregate particles, has an isotropic product structure, plays a role in preventing leakage, and well meets the smelting and using requirements of precious metals.
4. The Acheson furnace petroleum coke resistance material and the Acheson furnace petroleum coke heat preservation material used in the invention have lower elastic modulus, so that the product also has lower elastic modulus, the rejection rate is greatly reduced in the roasting link, the cracking rate is greatly reduced when the product is used by a user, the manufacturing rejection rate is reduced, and the use yield is improved. Simultaneously, this kind of raw materials is the waste material that this patent product is used for lithium cell negative pole production, can realize with the cyclic utilization of user's material, greatly reduced the production of waste material.
The invention provides a method for manufacturing a hot-pressing cold-discharge one-step molding reclaimed material graphite crucible by utilizing waste graphite scraps, Acheson furnace heat-insulating materials and resistance materials, wherein the waste materials produced by electrodes, the Acheson furnace petroleum coke resistance materials and the Acheson furnace petroleum coke heat-insulating materials are utilized, and the hot-pressing cold-discharge one-step molding method is adopted to produce a high-quality graphite crucible with good thermal shock resistance, ablation resistance, leak resistance and mechanical strength so as to meet the requirements of the purification and smelting industry of lithium battery negative electrode powder.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Example 1
A preparation method of a graphite crucible comprises the following steps:
s1, preparing raw materials: the raw materials comprise graphite scraps, Acheson furnace petroleum coke resistance materials, Acheson furnace petroleum coke heat-insulating materials and medium-temperature coal pitch, wherein:
the graphite fragments meet the following requirements: the true density is more than or equal to 2.13g/cm3Ash content is less than or equal to 0.03 percent, volatile matter is less than or equal to 0.22 percent, and water content is less than or equal to 0.09 percent;
the Acheson furnace petroleum coke resistance material and the Acheson furnace petroleum coke heat-insulating material simultaneously meet the following requirements: the true density is more than or equal to 2.10g/cm3Ash content is less than or equal to 0.03 percent, volatile matter is less than or equal to 0.22 percent, and water content is less than or equal to 0.09 percent;
the medium temperature coal pitch meets the following requirements: ash content is less than or equal to 0.20 percent, volatile matter is less than or equal to 64.2 percent, and water content is less than or equal to 0.06 percent;
s2, batching: grinding graphite into graphite powder, and mixing the graphite powder with an Acheson furnace petroleum coke resistance material and an Acheson furnace petroleum coke heat-insulating material according to the proportion of 3:2:5, mixing and grinding the mixture into mixed powder according to the mass ratio, and mixing the mixed powder with the medium-temperature coal pitch, wherein the mass percentage of the mixed powder is 65-85% and the mass percentage of the medium-temperature coal pitch is 15-35% in the mixing process;
s3, kneading;
s4, profiling;
s5, roasting;
and S6, processing.
Specifically, the graphite scraps in the step S1 are waste materials from graphite electrode production, and the acheson furnace petroleum coke resistance material and the acheson furnace petroleum coke heat preservation material are waste materials from the acheson furnace production of lithium battery negative electrode materials. The passing rate of the graphite powder obtained after grinding by sieving with a 200-mesh international standard sieve is 80 +/-5%, and the specific granularity comprises the following components in percentage by mass:
the proportion of 1mm granularity is 2-4%;
37-43% of granularity of 0.5-0.15 mm;
37-43% of granularity smaller than 0.075 mm;
the proportion of other particle sizes is 17-23%.
Specifically, the kneading in the above step S3 is to pour the ingredients into the kneading pot for stirring, the kneading pot itself is externally heated by the heat transfer oil, the inside is provided with a reamer for stirring the materials, and the heat transfer oil inlet temperature of the kneading pot is: 230 ℃ to 233 ℃, the temperature of asphalt in the kneading pot is 162 ℃ to 165 ℃, and the dry mixing time of kneading is as follows: 40 minutes at 118-; wet mixing time of kneading: 45 minutes, temperature 162-.
Specifically, the pressing in step S4 is to pour the kneaded paste into a forming container, where the forming container has an upper die and a lower die, and the upper die and the lower die have a heating and cooling function respectively, and start the heating function of the upper die and the lower die, and pour the paste into the upper die, so that the paste is formed under pressure, monitor the density of the paste, and start the cooling function when the density index is reached; if the density index is not reached, repeatedly heating and pressurizing until the density index is reached; the density index range is 1.7-1.75 g/cm3(ii) a Then, carrying out a cooling compression process, wherein the tamping pressure of the cooling compression process is 20Mpa, the molding pressure is 20Mpa, and the pressing time is 4 minutes to cool the paste material to prepare a green blank; finally, the upper die of the forming container is started for instantaneous secondary heating to ensure that the friction coefficient between the upper die and the product is rapidly reduced, thereby realizing demoulding。
Specifically, the firing in step S5 is to load the green compact into an industrial ring-type firing furnace, and to heat the green compact gradually according to the following temperature rise curve in the case of a reducing atmosphere: 150 ℃ plus 350 ℃, the temperature rise speed is 4.4 ℃/h and the duration time is 45 h; at the temperature of 400 ℃ in 350 ℃ and the temperature rise speed of 1.7 ℃/h, the duration of 30h, at the temperature of 500 ℃ in 400 ℃, at the temperature rise speed of 1.25 ℃/h, the duration of 80h, at the temperature of 600 ℃ in 500 ℃ and the temperature rise speed of 1.8 ℃/h, the duration of 57h, at the temperature of 700 ℃ in 600 ℃, at the temperature rise speed of 3.8 ℃/h, the duration of 27h, at the temperature of 800 ℃ in 700 ℃ in 800 ℃, at the temperature rise speed of 5.0 ℃/h, at the duration of 20h, at the temperature of 1000 ℃ in 800 ℃, at the temperature rise speed of 8.0 ℃/h, at the duration of 25h, at the temperature of 1200 ℃ in 1200 ℃, at the temperature rise speed of 8.3 ℃/h, at the duration of 20h and at the temperature of 1200 ℃ in 20 h.
By adopting three materials to mix ingredients, the roasting cracking rate is reduced to 0.5-1% from 3-4%, and the product cracking rate is reduced by about 2-3% through customer feedback.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (6)
1. A preparation method of a graphite crucible is characterized by comprising the following steps:
s1, preparing raw materials: the raw materials comprise graphite scraps, Acheson furnace petroleum coke resistance materials, Acheson furnace petroleum coke heat-insulating materials and medium-temperature coal pitch, wherein:
the graphite fragments meet the following requirements: the true density is more than or equal to 2.13g/cm3Ash content is less than or equal to 0.03 percent, volatile matter is less than or equal to 0.22 percent, and water content is less than or equal to 0.09 percent;
the Acheson furnace petroleum coke resistance material and the Acheson furnace petroleum coke heat-insulating material simultaneously meet the following requirementsThe method comprises the following steps: the true density is more than or equal to 2.10g/cm3Ash content is less than or equal to 0.03 percent, volatile matter is less than or equal to 0.22 percent, and water content is less than or equal to 0.09 percent;
the medium temperature coal pitch meets the following requirements: ash content is less than or equal to 0.20 percent, volatile matter is less than or equal to 64.2 percent, and water content is less than or equal to 0.06 percent;
s2, batching: grinding graphite into graphite powder, mixing the graphite powder with Acheson furnace petroleum coke resistance material and Acheson furnace petroleum coke heat preservation material according to a certain mass ratio, grinding the mixture into mixed powder, and mixing the mixed powder with medium-temperature coal pitch;
s3, kneading;
s4, profiling;
s5, roasting;
and S6, processing.
2. The method of manufacturing a graphite crucible according to claim 1, wherein in step S2, the mass ratio of the graphite powder to the acheson furnace petroleum coke electrical resistance material to the acheson furnace petroleum coke thermal insulation material is 3:2: 5; the mass percent of the mixed powder in the process of mixing the mixed powder with the medium-temperature coal pitch is 65-85 percent, and the mass percent of the medium-temperature coal pitch is 15-35 percent.
3. The method for preparing a graphite crucible as claimed in claim 1, wherein the graphite in the step S1 is crushed into graphite electrode production waste, the particle size of the graphite powder obtained after grinding is 80 ± 5% by sieving with a 200 mesh international standard sieve, and the specific particle size composition in mass percentage is as follows:
the proportion of 1mm granularity is 2-4%;
37-43% of granularity of 0.5-0.15 mm;
37-43% of granularity smaller than 0.075 mm;
the proportion of other particle sizes is 17-23%.
4. The method for preparing a graphite crucible as claimed in claim 1, wherein the kneading in step S3 is performed by pouring the ingredients into a kneading pot for stirring, the kneading pot itself is externally heated by heat transfer oil, a reamer is provided inside for stirring the ingredients, the heat transfer oil inlet temperature of the kneading pot is: 230 ℃ to 233 ℃, the temperature of asphalt in the kneading pot is 162 ℃ to 165 ℃, and the dry mixing time of kneading is as follows: 40 minutes at 118-; wet mixing time of kneading: 45 minutes, temperature 162-.
5. The method of manufacturing a graphite crucible as claimed in claim 1, wherein the pressing in step S4 is performed by pouring the kneaded paste into a forming container having an upper mold and a lower mold each having a heating and cooling function, turning on the heating function of the upper mold and the lower mold, pouring the paste into the upper mold, forming the paste under pressure, monitoring the density of the paste, and turning on the cooling function when the density index is reached; if the density index is not reached, repeatedly heating and pressurizing until the density index is reached; the density index range is 1.7-1.75 g/cm3(ii) a Then, carrying out a cooling compression process, wherein the tamping pressure of the cooling compression process is 20Mpa, the molding pressure is 20Mpa, and the pressing time is 4 minutes to cool the paste material to prepare a green blank; and finally, starting instantaneous secondary heating on the upper die of the forming container to demould.
6. The method of manufacturing a graphite crucible as claimed in claim 1, wherein the firing in step S5 is performed by charging the green compact into an industrial ring type firing furnace, and heating the green compact in a reducing atmosphere in a stepwise manner according to the following temperature rising curve: 150 ℃ plus 350 ℃, the temperature rise speed is 4.4 ℃/h and the duration time is 45 h; at the temperature of 400 ℃ in 350 ℃ and the temperature rise speed of 1.7 ℃/h, the duration of 30h, at the temperature of 500 ℃ in 400 ℃, at the temperature rise speed of 1.25 ℃/h, the duration of 80h, at the temperature of 600 ℃ in 500 ℃ and the temperature rise speed of 1.8 ℃/h, the duration of 57h, at the temperature of 700 ℃ in 600 ℃, at the temperature rise speed of 3.8 ℃/h, the duration of 27h, at the temperature of 800 ℃ in 700 ℃ in 800 ℃, at the temperature rise speed of 5.0 ℃/h, at the duration of 20h, at the temperature of 1000 ℃ in 800 ℃, at the temperature rise speed of 8.0 ℃/h, at the duration of 25h, at the temperature of 1200 ℃ in 1200 ℃, at the temperature rise speed of 8.3 ℃/h, at the duration of 20h and at the temperature of 1200 ℃ in 20 h.
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