CN114478011A - Preparation method of microcrystalline graphite doped special isostatic pressing graphite - Google Patents
Preparation method of microcrystalline graphite doped special isostatic pressing graphite Download PDFInfo
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- CN114478011A CN114478011A CN202210331033.9A CN202210331033A CN114478011A CN 114478011 A CN114478011 A CN 114478011A CN 202210331033 A CN202210331033 A CN 202210331033A CN 114478011 A CN114478011 A CN 114478011A
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- 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
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- C04B35/521—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 by impregnation of carbon products with a carbonisable material
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- 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
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Abstract
The invention discloses a preparation method of microcrystalline graphite doped special isostatic pressing graphite, which comprises the following steps: preparing raw materials, kneading, crushing and screening, molding, roasting and dipping. The finished product prepared by the method has obviously improved performance indexes such as flexural strength, volume density and the like, the yield is improved by about 10 percent compared with the traditional preparation method, and the preparation method is the improvement of the traditional preparation method, so that the method has good industrialization and operability.
Description
Technical Field
The invention relates to the technical field of microcrystalline graphite, in particular to a preparation method of microcrystalline graphite doped with special isostatic pressing graphite.
Background
The isostatic pressing graphite is a novel graphite material, is a fine product in the graphite material, has high embedding end, density, purity, corrosion resistance and other properties, is one of the most valuable new materials in the 21 st century, and is widely applied to the fields of metallurgy, chemical industry, aerospace, electronics, machinery, nuclear energy and the like. With the economic development, the domestic and international market capacity of the isostatic pressing graphite is increased day by day, the development potential is huge, and China keeps a huge demand for the isostatic pressing graphite as a large world manufacturing industry country and a largest photovoltaic product producing country. Currently, with the rapid development of the domestic photovoltaic industry, the demand of the Chinese isostatic pressing graphite is increased year by year. For this reason, one strand of isostatic pressing graphite is currently producing heat in China.
The raw material of isostatic pressing graphite generally adopts petroleum coke or pitch coke as raw material, which can be raw coke or calcined coke, and in the preparation process, the higher the density of the blank, the finer the particles and the larger the volume, the higher the requirement on the uniformity of a temperature field, so that the coke is more likely to crack in the later roasting and graphitization post-treatment process, and the yield and the qualification rate of the product are reduced. Therefore, there is a need to provide a new preparation method to improve the existing preparation method of isostatic pressing graphite.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing microcrystalline graphite doped with special isostatic pressing graphite, wherein the performance indexes of the finished product prepared by the method, such as flexural strength, volume density, etc., are all significantly improved, and the yield is improved by about 10% compared with the conventional preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of microcrystalline graphite doped special isostatic pressing graphite comprises the following steps:
(1) preparation of raw materials:
crushing petroleum coke or asphalt coke raw materials on a crusher to a reasonable particle size to prepare coke powder with the average particle size of 1-30 mu m; shaping microcrystalline graphite to powder of 1-10 μm with shaper, and tap density>1.0g/cm3；
(2) Kneading:
putting the coke powder and the powder obtained in the step (1) into a kneading machine according to a certain proportion, stirring for 10-60min to uniformly mix the coke powder and the powder, then increasing the temperature to 140-300 ℃, adding modified asphalt with a certain proportion, continuing kneading for 0.3-8h, and after kneading, putting into a cooling machine to cool to obtain a paste; the mass percentage of the powder is 1-10%, and the mass percentage of the modified asphalt is 25-45%;
(3) crushing and screening:
crushing the paste obtained in the step (2) to 10-50 mu m, and sieving the paste with a 50-300 mesh sieve until the paste is crushed;
(4) molding:
putting the crushed paste obtained in the step (3) into a rubber mold, vacuum charging, then placing into an isostatic press for molding treatment, wherein the molding pressure is 50-300MPa, and demolding is carried out after the pressure maintaining time is 10-180min to obtain a blank;
(5) roasting:
performing heat preservation on the green body obtained in the step (4) at the temperature of 750-1050 ℃ for roasting treatment for 10-100h to obtain a roasted green body;
(6) dipping:
preheating the roasted blank obtained in the step (5) at the temperature of 300-500 ℃ for 2-24h, and then carrying out impregnation treatment by using impregnating pitch under the pressure of 1.5-5Mpa for 1-5 h; and (5) further repeating the operation of the step (5) on the impregnated product, and performing graphitization treatment on the obtained product at the temperature of 2500-.
Preferably, the mass percentage of the powder in the step (2) is 3-6%.
Preferably, the modified asphalt in the step (2) is medium-temperature coal asphalt or high-temperature coal asphalt, the softening point is 100-250 ℃, the mass percentage of toluene insoluble substances is 30-60%, the mass percentage of quinoline insoluble substances is 2-30%, and the coking value is more than 50.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
the finished product prepared by the method has obviously improved performance indexes such as flexural strength, volume density and the like, the yield is improved by about 10 percent compared with the traditional preparation method, and the preparation method is the improvement of the traditional preparation method, so that the method has good industrialization and operability.
The present invention will be described in detail with reference to specific embodiments in order to more clearly illustrate the structural features and effects of the present invention.
Detailed Description
The invention discloses a preparation method of microcrystalline graphite doped special isostatic pressing graphite, which comprises the following steps:
(1) preparation of raw materials:
pulverizing petroleum coke or pitch coke raw material on a pulverizer to a reasonable particle size to prepareCoke powder with average grain diameter of 1-30 μm; shaping microcrystalline graphite to powder of 1-10 μm with a shaping machine>1.0g/cm3；
(2) Kneading:
putting the coke powder and the powder obtained in the step (1) into a kneading machine according to a certain proportion, stirring for 10-60min to uniformly mix the coke powder and the powder, then increasing the temperature to 140-300 ℃, adding modified asphalt with a certain proportion, continuing kneading for 0.3-8h, and after kneading, putting into a cooling machine to cool to obtain a paste; the mass percentage of the powder is 1-10%, and the effect is better when the mass percentage of the powder is 3-6%; the mass ratio of the modified asphalt is 25-45%; the modified asphalt is medium-temperature coal asphalt or high-temperature coal asphalt, the softening point of the modified asphalt is 100-250 ℃, the mass percentage of toluene insoluble substances is 30-60%, the mass percentage of quinoline insoluble substances is 2-30%, and the coking value is more than 50.
(3) Crushing and screening:
crushing the paste obtained in the step (2) to 10-50 μm, and sieving with a 50-300 mesh sieve until the paste is crushed.
(4) Molding:
and (4) putting the crushed paste obtained in the step (3) into a rubber mold, vacuum charging, then placing into an isostatic press for molding treatment, wherein the molding pressure is 50-300MPa, and demolding is carried out after the pressure maintaining time is 10-180min, so as to obtain a blank.
(5) Roasting:
and (4) preserving the heat of the green body obtained in the step (4) at 750-1050 ℃ for roasting treatment for 10-100h to obtain a roasted green body.
(6) Dipping:
preheating the roasted blank obtained in the step (5) at the temperature of 300-500 ℃ for 2-24h, and then carrying out impregnation treatment by using impregnating pitch under the pressure of 1.5-5Mpa for 1-5 h; and (5) further repeating the operation of the step (5) on the impregnated product, and performing graphitization treatment on the obtained product at the temperature of 2500-.
The invention is described in detail below by way of a list with reference to specific examples.
Comparative example:
the preparation method was substantially the same as that of example 1 except that microcrystalline graphite was not added.
The formulations of the examples and comparative examples and the corresponding parameters during their preparation are shown in table 1.
TABLE 1
The following performance tests were conducted on each of the examples and comparative examples, and the test results are shown in Table 2.
TABLE 2
The test method comprises the following steps:
the method for testing the flexural strength comprises the following steps: reference national standard GB/T3001-2007
Method for testing bulk density: reference national standard YB/T908-1997
The design of the invention is characterized in that: the invention improves the kneading effect by doping, improves the volume density and all-directional mechanical property indexes of the product, and achieves higher product performance and yield by the selection of the formula and the control of the raw materials; and, the invention is an improvement of the original scheme, is particularly suitable for large-scale batch manufacturing of products, and is beneficial to improving the batch stability of the products.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (3)
1. A preparation method of microcrystalline graphite doped special isostatic pressing graphite is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of raw materials:
putting petroleum coke or asphalt coke raw material on a pulverizerPulverizing to reasonable particle size to obtain coke powder with average particle size of 1-30 μm; shaping microcrystalline graphite to powder of 1-10 μm with a shaping machine>1.0g/cm3；
(2) Kneading:
putting the coke powder and the powder obtained in the step (1) into a kneading machine according to a certain proportion, stirring for 10-60min to uniformly mix the coke powder and the powder, then increasing the temperature to 140-300 ℃, adding modified asphalt with a certain proportion, continuing kneading for 0.3-8h, and after kneading, putting into a cooling machine to cool to obtain a paste; the mass percentage of the powder is 1-10%, and the mass percentage of the modified asphalt is 25-45%;
(3) crushing and screening:
crushing the paste obtained in the step (2) to 10-50 mu m, and sieving the paste with a 50-300 mesh sieve until the paste is crushed;
(4) molding:
putting the crushed paste obtained in the step (3) into a rubber mold, vacuum charging, then placing into an isostatic press for molding treatment, wherein the molding pressure is 50-300MPa, and demolding is carried out after the pressure maintaining time is 10-180min to obtain a blank;
(5) roasting:
performing heat preservation on the green body obtained in the step (4) at the temperature of 750-1050 ℃ for roasting treatment for 10-100h to obtain a roasted green body;
(6) dipping:
preheating the roasted blank obtained in the step (5) at the temperature of 300-500 ℃ for 2-24h, and then carrying out impregnation treatment by using impregnating pitch under the pressure of 1.5-5Mpa for 1-5 h; and (5) further repeating the operation of the step (5) on the impregnated product, and performing graphitization treatment on the obtained product at the temperature of 2500-.
2. The preparation method of the microcrystalline graphite doped special isostatic pressing graphite according to claim 1, wherein the preparation method comprises the following steps: the mass percentage of the powder in the step (2) is 3-6%.
3. The preparation method of the microcrystalline graphite doped special isostatic pressing graphite according to claim 1, wherein the preparation method comprises the following steps: the modified asphalt in the step (2) is medium-temperature coal asphalt or high-temperature coal asphalt, the softening point of the modified asphalt is 100-250 ℃, the mass percentage of toluene insoluble substances is 30-60%, the mass percentage of quinoline insoluble substances is 2-30%, and the coking value is more than 50.
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| CN202210331033.9A CN114478011A (en) | 2022-03-30 | 2022-03-30 | Preparation method of microcrystalline graphite doped special isostatic pressing graphite |
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| CN202210331033.9A CN114478011A (en) | 2022-03-30 | 2022-03-30 | Preparation method of microcrystalline graphite doped special isostatic pressing graphite |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1510568A (en) * | 1975-06-24 | 1978-05-10 | Lorraine Carbone | Artificial graphite |
| CN101654239A (en) * | 2009-08-27 | 2010-02-24 | 清华大学 | Isotropic graphite product and preparation method thereof |
| CN101823707A (en) * | 2010-04-28 | 2010-09-08 | 四川广汉士达炭素股份有限公司 | Technical method for producing isostatic pressure graphite |
| CN102530933A (en) * | 2011-12-30 | 2012-07-04 | 清华大学 | Artificial graphite product taking emulsified asphalt as binder and preparation method thereof |
| CN103121671A (en) * | 2013-03-15 | 2013-05-29 | 四川广汉士达炭素股份有限公司 | Preparation method of isostatic pressing formed graphite |
| CN104016333A (en) * | 2014-05-25 | 2014-09-03 | 林前锋 | Preparation method of isostatic pressing microcrystalline graphite product |
| CN105174251A (en) * | 2015-09-22 | 2015-12-23 | 成都炭素有限责任公司 | Preparation method of isostatic pressing formed graphite of ultra-thin structure |
-
2022
- 2022-03-30 CN CN202210331033.9A patent/CN114478011A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1510568A (en) * | 1975-06-24 | 1978-05-10 | Lorraine Carbone | Artificial graphite |
| CN101654239A (en) * | 2009-08-27 | 2010-02-24 | 清华大学 | Isotropic graphite product and preparation method thereof |
| CN101823707A (en) * | 2010-04-28 | 2010-09-08 | 四川广汉士达炭素股份有限公司 | Technical method for producing isostatic pressure graphite |
| CN102530933A (en) * | 2011-12-30 | 2012-07-04 | 清华大学 | Artificial graphite product taking emulsified asphalt as binder and preparation method thereof |
| CN103121671A (en) * | 2013-03-15 | 2013-05-29 | 四川广汉士达炭素股份有限公司 | Preparation method of isostatic pressing formed graphite |
| CN104016333A (en) * | 2014-05-25 | 2014-09-03 | 林前锋 | Preparation method of isostatic pressing microcrystalline graphite product |
| CN105174251A (en) * | 2015-09-22 | 2015-12-23 | 成都炭素有限责任公司 | Preparation method of isostatic pressing formed graphite of ultra-thin structure |
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Application publication date: 20220513 |