CN115609940B - Production process of graphite crucible - Google Patents
Production process of graphite crucible Download PDFInfo
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- CN115609940B CN115609940B CN202211635973.3A CN202211635973A CN115609940B CN 115609940 B CN115609940 B CN 115609940B CN 202211635973 A CN202211635973 A CN 202211635973A CN 115609940 B CN115609940 B CN 115609940B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000010439 graphite Substances 0.000 title claims abstract description 89
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 89
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000000428 dust Substances 0.000 claims abstract description 72
- 239000000203 mixture Substances 0.000 claims abstract description 53
- 239000010426 asphalt Substances 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000011810 insulating material Substances 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 230000004927 fusion Effects 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
- B29C67/24—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 characterised by the choice of material
-
- 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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/26—Bituminous materials, e.g. tar, pitch
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2103/00—Use of resin-bonded materials as moulding material
- B29K2103/04—Inorganic materials
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A production process of a graphite crucible belongs to the field of graphite crucibles, and comprises the following steps: a: fusing graphite dust and modified liquid asphalt according to a certain mass ratio at the temperature of 80-100 ℃ to obtain a dust mixture; b: weighing 16 parts of graphitized heat-insulating material, 24 parts of middle material, 18 parts of small material and 30 parts of fine powder, and uniformly mixing to obtain a primary mixture; c: weighing 30 parts of dust mixture and 14 parts of modified liquid asphalt, and uniformly mixing the dust mixture, the modified liquid asphalt and the primary mixture at 170-180 ℃ to obtain a secondary mixture; d: and (4) putting the secondary mixture into a crucible mold, heating and pressing to form to obtain the graphite crucible. According to the invention, graphite dust is fused with asphalt at a lower temperature, and then the dust mixture is mixed with other raw materials at a higher temperature, so that the graphite dust can be uniformly mixed with other raw materials of the graphite crucible to prepare the graphite crucible, and the graphite dust is effectively recycled.
Description
Technical Field
The invention belongs to the field of graphite crucibles, and particularly relates to a production process of a graphite crucible.
Background
In the production process of the crucible, graphite dust is generated, generally, in order to improve the working environment, a bag-type dust collector is used for recovering the graphite dust in the production process of the crucible, the graphite dust is ultrafine dust generated by mutual friction of graphitized heat-insulating materials in the production process of the graphite crucible, the particle size of the fine powder in the graphitized heat-insulating materials required by normal filling is smaller than that of the graphite dust recovered by the bag-type dust collector, the part of the dust is too fine and is below 200 meshes, wherein the proportion of the part below 300 meshes (the fineness is 0.05 mm) is more than nine mm, the part of the dust cannot be returned to a raw material position to be directly added into other raw materials of the graphite crucible for mixing use, and the direct addition can cause poor homogeneity of the prepared graphite crucible, so that the graphite dust is easy to crack and cannot meet the use requirements of finished products.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a production process of a graphite crucible. According to the invention, the graphite dust is firstly fused with the asphalt at a lower temperature, and then the dust mixture is mixed with other raw materials at a higher temperature, so that the graphite dust can be uniformly mixed with other raw materials of the graphite crucible to prepare the graphite crucible, and the prepared graphite crucible contains about 15% of the graphite dust, thereby realizing effective recycling of the graphite dust and reducing the production cost of the graphite crucible.
The invention adopts the specific technical scheme that:
the production process of the graphite crucible is characterized by comprising the following steps of:
A. mixing graphite dust with fineness less than 0.07mm and the reformed liquid asphalt according to the mass ratio (8-12): 1, fusing to obtain a dust mixture, wherein the temperature during fusing is 80-100 ℃;
B. selecting raw materials, weighing graphitized heat-insulating materials with different fineness, uniformly mixing 12-18 parts of large materials with the fineness of 3-6mm, 20-28 parts of middle materials with the fineness of 2-3mm, 16-20 parts of small materials with the fineness of 1-2 mm and 24-32 parts of fine powder with the fineness of 0.075-1mm in parts by mass to obtain a primary mixture;
C. weighing 28 to 32 parts of dust mixture and 10 to 18 parts of modified liquid asphalt, and uniformly mixing the dust mixture, the modified liquid asphalt and the primary mixture for the second time to obtain a secondary mixture, wherein the temperature during the secondary mixing is 170 to 180 ℃;
D. and D, placing the secondary mixture obtained in the step C into a crucible mold, heating and pressing to form the graphite crucible, wherein the forming temperature is 140-145 ℃.
And B, putting the graphite dust and the reformed liquid asphalt into a fusion machine for fusion, wherein the fusion temperature is 90 ℃, and the fusion time is 30-40min.
In the step A, the ratio of the graphite dust with the fineness less than 0.05mm to the reformed liquid asphalt by mass is 10:1, fusion is carried out.
The fineness of the graphite dust in the step A is 0.01-0.03mm.
In the step B, the graphitized heat preservation material has the volatile content of less than 1.3 percent, the ash content of less than 1.2 percent, the sulfur content of less than 0.3 percent and the resistivity of less than 160 percent.
The graphitized heat preservation material in the step B comprises 16 parts of a large material with the fineness of 3-6mm, 24 parts of a medium material with the fineness of 2-3mm, 18 parts of a small material with the fineness of 1-2 mm and 30 parts of fine powder with the fineness of 0.075-1mm by weight; 30 parts of the dust mixture and 14 parts of modified liquid asphalt in the step C; the secondary mixing temperature was 170 ℃.
The temperature during the primary mixing in the step B is 160-170 ℃.
The temperature at the time of the primary mixing in step B was 165 ℃.
The beneficial effects of the invention are:
1. the production process of the graphite crucible recycles the graphite dust with the fineness less than 0.07mm generated in the production process, wherein the proportion of the graphite dust with the particle size of less than 0.05mm is more than nine percent, and the graphite dust replaces about 15 percent of the raw materials for producing the graphite crucible, thereby reducing the production cost. In the prior art, graphite dust is directly mixed with a primary mixture, but the graphite dust has too small fineness, so that the graphite dust is positioned at the bottom of the secondary mixture and cannot be uniformly mixed with other raw materials, and the powder in the area near the outer surface of a pressed graphite crucible has poor flowability, so that the crucible forming pressure distribution is not uniform, the prepared graphite crucible has poor homogeneity, cracks are easy to appear in the using process, and the graphite dust cannot be recycled as a graphite crucible raw material.
2. According to the production process of the graphite crucible, 12 to 18 percent of production raw materials of the graphite crucible are replaced by the graphite dust, when the proportion of the graphite dust is further increased, the finished density of the graphite crucible is too high, so that the fluidity of the internal structure of the graphite crucible is poor, the hardness is reduced, meanwhile, the surface area of the material is increased due to the use of a large amount of graphite dust, and in order to ensure the cohesiveness among the materials, the use amount of asphalt is suddenly increased, so that the economic benefit is not met.
3. The fusion time of the graphite dust and the asphalt is 30-40min, if the fusion time is too low, the graphite dust cannot be fully and uniformly fused with the asphalt, a small part of the graphite dust cannot be well fused with the asphalt, resources are wasted, if the fusion time is too long, the bonding degree between the graphite dust and the asphalt is too high, and in the process of heating and mixing the graphitized heat-insulating material, the graphite dust cannot be well separated from the asphalt, so that the homogeneity of the prepared graphite crucible is poor.
4. The wall-hanging rate of the graphite crucible is low, the graphite crucible is usually used for melting materials with higher melting points, the molten materials usually have higher viscosity, the wall-hanging rate of the traditional graphite crucible after heating is about 15%, the wall-hanging rate of the graphite crucible is only about 6%, and gaps among raw materials of the graphite crucible are reduced by adding graphite dust, so that the inner surface of the prepared graphite crucible is smoother and smoother, and the wall-hanging rate of the graphite crucible is reduced.
Detailed Description
1. Detailed description of the preferred embodiments
Example 1
A: mixing graphite dust with the fineness of 0.01-0.03mm and the reformed liquid asphalt according to the mass ratio of 10:1 in a fusion machine for fusion to obtain a dust mixture, wherein the fusion temperature is 90 ℃ and the fusion time is 35min;
b: selecting raw materials, weighing graphitized heat-insulating materials with different fineness, uniformly mixing 16 parts of large material with the fineness of 3-6mm, 24 parts of medium material with the fineness of 2-3mm, 18 parts of small material with the fineness of 1-2 mm and 30 parts of fine powder with the fineness of 0.075-1mm at 165 ℃ to obtain a primary mixture according to parts by weight;
c: weighing 30 parts of dust mixture and 14 parts of modified liquid asphalt, and uniformly mixing the dust mixture, the modified liquid asphalt and the primary mixture for the second time to obtain a secondary mixture, wherein the temperature during the secondary mixing is 175 ℃;
d: and D, placing the secondary mixture obtained in the step C into a crucible mold, heating and pressing to form the graphite crucible, wherein the forming temperature is 142 ℃.
Example 2
A: mixing graphite dust with the fineness of 0.035-0.05mm and the reformed liquid asphalt according to the mass ratio of 9:1 to obtain a dust mixture, and the temperature during fusion is 85 ℃ and the fusion time is 37min.
B: selecting raw materials, weighing graphitized heat-insulating materials with different fineness, uniformly mixing 12 parts of large materials with the fineness of 3-6mm, 28 parts of medium materials with the fineness of 2-3mm, 20 parts of small materials with the fineness of 1-2 mm and 32 parts of fine powder with the fineness of 0.075-1mm at 162 ℃ to obtain a primary mixture according to parts by weight;
c: weighing 32 parts of dust mixture and 10 parts of modified liquid asphalt, and uniformly mixing the dust mixture, the modified liquid asphalt and the primary mixture for the second time to obtain a secondary mixture, wherein the temperature during the secondary mixing is 170 ℃;
d: and D, placing the secondary mixture obtained in the step C into a crucible mold, heating and pressing to form the graphite crucible, wherein the forming temperature is 140 ℃.
Example 3
A: graphite dust with the fineness of 0.055-0.065mm and the modified liquid asphalt are mixed according to the mass ratio of 11:1, putting the mixture into a fusion machine for fusion to obtain a dust mixture, wherein the fusion temperature is 95 ℃, and the fusion time is 33min;
b: selecting raw materials, weighing graphitized heat-insulating materials with different finenesses, uniformly mixing 18 parts of large materials with the fineness of 3-6mm, 20 parts of middle materials with the fineness of 2-3mm, 16 parts of small materials with the fineness of 1-2 mm and 24 parts of fine powder with the fineness of 0.075-1mm at 168 ℃ to obtain a primary mixture;
c: weighing 28 parts of dust mixture and 18 parts of modified liquid asphalt, and uniformly mixing the dust mixture, the modified liquid asphalt and the primary mixture for the second time to obtain a secondary mixture, wherein the temperature during the secondary mixing is 180 ℃;
d: and D, placing the secondary mixture obtained in the step C into a crucible mold, heating and pressing to form the graphite crucible, wherein the forming temperature is 145 ℃.
Comparative example 1
Comparative example 1 differs from example 1 only in that the secondary mixing temperature in step B of comparative example 1 is the same as the temperature at the time of fusion, both 145 ℃.
2. Performance testing
Comparing the performances of the graphite crucibles prepared in the above examples and comparative examples, wherein the hardness is measured by randomly taking 10 points on the surface of the crucible; the wall hanging prevention property is that the crucible is adopted to heat the negative electrode powder at 900 ℃, after the negative electrode powder is poured out, the percentage of the mass of the negative electrode powder stuck on the inner wall of the crucible to the mass of the heated negative electrode powder is calculated; the wear resistance is expressed by the difference between the actual weight of the anode powder after scraping and the ideal weight of the anode powder adhered on the inner wall; use number test the crucibles prepared in the different examples and comparative examples were heated several times at the same temperature and the number of times used before the occurrence of cracks was recorded, the results of which are shown in table 1.
TABLE 1
As can be seen from Table 1, the crucible special for the negative electrode powder has the advantages that the average surface hardness is not less than 55HCR, the difference between the maximum surface hardness and the minimum surface hardness is not more than 2HCR, the wear resistance is not more than 37g, the wall hanging rate is not more than 6.8%, the use frequency is not less than 7 times, and the crucible is excellent in performance.
It can be seen from comparison between comparative example 1 and example 1 that the crucible formed by pressing the crucible mold subjected to heat treatment in example 1 has different degrees of improvement in hardness, homogeneity, service life and other properties, because asphalt and graphite dust are heated and fused at 80-100 ℃ in example 1, so that the graphite dust is aggregated under the action of the asphalt to obtain a whole dust mixture, and then the primary mixture formed by mixing the dust mixture and graphitized heat-insulating materials with different fineness is mixed at 170-180 ℃, because of the improvement of temperature, the viscosity of the asphalt is reduced, when the temperature is in the range of 170-180 ℃, the viscosity between the asphalt and the graphite dust is reduced while a certain viscosity of the asphalt is maintained, at the moment, the graphite dust and the graphitized heat-insulating materials with different fineness are uniformly mixed and mutually bonded, and the graphite dust can be filled in all corners of the secondary mixture, and the prepared graphite crucible has good homogeneity, high density, large hardness and long service life.
Claims (4)
1. The production process of the graphite crucible is characterized by comprising the following steps of:
A. mixing graphite dust with the fineness of 0.01-0.03mm and the reformed liquid asphalt according to the mass ratio of 10:1, fusing to obtain a dust mixture, wherein the fusing temperature is 90 ℃, and the fusing time is 30 to 40min;
B. selecting raw materials, weighing graphitized heat-insulating materials with different fineness, and uniformly mixing 12-18 parts of large materials with the fineness of 3-6mm, 20-28 parts of medium materials with the fineness of 2-3mm, 16-20 parts of small materials with the fineness of 1-2 mm and 24-32 parts of fine powder with the fineness of 0.075-1mm in parts by weight to obtain a primary mixture;
C. weighing 28-32 parts of the dust mixture and 10-18 parts of modified liquid asphalt, and uniformly mixing the dust mixture, the modified liquid asphalt and the primary mixture for the second time to obtain a secondary mixture, wherein the temperature during the secondary mixing is 170-180 ℃;
D. c, placing the secondary mixture obtained in the step C into a crucible mold, heating and pressing to form the graphite crucible, wherein the forming temperature is 140-145 ℃;
b, putting the graphite dust and the reformed liquid asphalt into a fusion machine for fusion in the step A;
the temperature during the primary mixing in the step B is 160-170 ℃.
2. The process for producing a graphite crucible as claimed in claim 1, wherein the graphitized insulating material in the step B has a volatile content of less than 1.3%, an ash content of less than 1.2%, sulfur content of less than 0.3%, and a resistivity of less than 160.
3. The production process of the graphite crucible as claimed in claim 1, wherein the graphitized heat preservation material in the step B comprises 16 parts by mass of a large material with fineness of 3-6mm, 24 parts by mass of a medium material with fineness of 2-3mm, 18 parts by mass of a small material with fineness of 1-2 mm, and 30 parts by mass of fine powder with fineness of 0.075-1 mm; 30 parts of the dust mixture and 14 parts of modified liquid asphalt in the step C; the secondary mixing temperature was 170 ℃.
4. The process for producing a graphite crucible as claimed in claim 3, wherein the temperature at the time of the primary mixing in the step B is 165 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211635973.3A CN115609940B (en) | 2022-12-20 | 2022-12-20 | Production process of graphite crucible |
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| CN115609940B true CN115609940B (en) | 2023-04-07 |
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| CN119080495B (en) * | 2024-09-30 | 2025-02-11 | 贝特瑞新材料集团股份有限公司 | Graphite crucible repair material and method for repairing graphite crucible |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105272287A (en) * | 2015-10-15 | 2016-01-27 | 大同新成新材料股份有限公司 | Method for preparing graphite crucible with recycled graphite |
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| CN104529450B (en) * | 2014-12-04 | 2016-11-30 | 大同新成新材料股份有限公司 | A kind of forming method of big specification isostatic pressing formed graphite goods |
| CN105218098A (en) * | 2015-10-29 | 2016-01-06 | 武陟县虹桥碳素有限责任公司 | A kind of negative material high temperature purification special graphite crucible manufacturing |
| CN105645397B (en) * | 2016-03-03 | 2018-06-29 | 湖南省长宇新型炭材料有限公司 | It is a kind of for hyperfine structure graphite of EDM and preparation method thereof |
| CN108046812A (en) * | 2017-12-12 | 2018-05-18 | 中国平煤神马能源化工集团有限责任公司 | A kind of Delanium crucible and preparation method thereof |
| CN111087249A (en) * | 2019-12-27 | 2020-05-01 | 重庆东星炭素材料有限公司 | Graphite porous crucible and preparation method thereof |
| CN112062569B (en) * | 2020-09-04 | 2022-04-08 | 汨罗市福缘新材料有限公司 | A kind of method for preparing graphite crucible using recycled material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105272287A (en) * | 2015-10-15 | 2016-01-27 | 大同新成新材料股份有限公司 | Method for preparing graphite crucible with recycled graphite |
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