CN103011148A - Method for preparing isotropical graphite - Google Patents
Method for preparing isotropical graphite Download PDFInfo
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Abstract
The invention discloses a method for preparing isotropical graphite, which is characterized by comprising the following steps: (1) mixing mesocarbon microbeads with asphalt to obtain a mixture; (2) carrying out thermal polymerization reaction to the mixture, and growing the mesocarbon microbeans for the second time to obtain intermediate phase raw material; (3) performing ball-milling treatment to the intermediate phase raw material to obtain ball-milled powder; (4) performing oxidization treatment to the ball-milled powder to obtain pre-treated powder; (5) performing iso-static compaction to the pre-treated powder; (6) sintering; and (7) graphitizing. The preparation method disclosed by the invention is short in process and easy to implement, and is beneficial for shortening the production cycle and reducing the manufacturing cost; in addition, the graphite material produced by the method disclosed by the invention has the characteristics of excellent homogeneity and high mechanical strength.
Description
Technical field
The present invention relates to a kind of method for preparing isotropic graphite.
Background technology
Isotropic graphite be a kind of graphite microcrystal disorderly orientations, have the special graphite material of isotropic structure, the incorgruous degree of its internal structure is generally between 1.0～1.1.Isotropic graphite possesses the multiple good characteristics such as stable performance under the high temperature, high-density, high strength, high thermal conductivity, be widely used in the various fields such as semi-conductor, photovoltaic solar, electrospark machining, nuclear energy, metallurgy, space flight, and along with the development of science and technology, its Application Areas is also in continuous expansion.
Mainly take coke or graphite as aggregate, coal-tar pitch is binding agent to traditional isotropic graphite, through batching, kneading, repeatedly roll sheet and grind after, adopt mold pressing or isostatic pressing, make through charing, dipping and graphite treatment again.In the charing stage, because the volumetric shrinkage of aggregate charcoal and Binder-based Carbon is different, thereby causes carbon graphite material generally to have the shortcomings such as void content is higher, homogeneity is poor, the interface is obvious, make the performances such as its density, intensity very low.For intensity and the density that improves goods, reduce void content, the way of generally taking is to utilize the technique of repeatedly dipping, roasting to reduce the porosity of material, but dipping repeatedly, calcination process have also been brought the problems such as the isotropic graphite material production cycle is tediously long, with high costs, and also there are gap in the final uniformity of material and physicochemical property and people's expection.
For improving the problem that exists in traditional isotropic graphite material produce, people have developed some novel procesies and novel method gradually, wherein prepare isotropic graphite take MCMB as raw material and have caused widely interest of people.MCMB possesses preferably spherical shapes, can realize between the bead in the sintering process merging, and therefore has the potentiality of the good isotropy carbon/graphite material of processability.But owing to there is the poor problems such as occurring easily crackle when large specification product, sintering motivating force do not cause sintering by force of can't suppressing of processability, therefore never accomplish scale production.
Summary of the invention
Problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of method for preparing isotropic graphite is provided.
The present invention has improved a kind of method for preparing isotropic graphite, it is characterized in that: it comprises following step:
1. MCMB is mixed with pitch, obtain compound;
2. described compound is carried out heat polymerization, MCMB diauxic growth, phase raw material in the middle of obtaining;
3. with phase raw material ball-milling processing in the middle of described, obtain the ball milling powder;
4. described ball milling powder is carried out oxide treatment, obtain the pre-treatment powder;
5. with described pre-treatment powder isostatic pressing;
6. sintering;
7. greying.
Step 1. described in the median size of MCMB be 3.0～15.0 μ m, consumption is 20%～80% of described compound gross weight.
Step 1. described in the quinoline insolubles mass content of pitch be that 0%～1.0%, β resin content is 10.0%～20.0%, softening temperature is 85.0～95.0 ℃.
Step 2. described in the temperature of reaction of heat polymerization be 370～460 ℃, reaction atmosphere is nitrogen or protection of inert gas atmosphere, the reaction times is 1～10 hour.
Step 3. described in the median size of ball milling powder be 1.0～20.0 μ m.
Step 4. described in the temperature of oxide treatment be 250～320 ℃, processing atmosphere is air atmosphere, the treatment time is 1～5 hour.
Step 5. described in the forming pressure of isostatic pressing be 50～100MPa, mold temperature is 20～500 ℃, molding time is 30～300 minutes.
Step 6. described in the top temperature of roasting be 800～1300 ℃, be 10～100 hours in the soaking time of top temperature point.
Step 7. described in graphited top temperature be 2000～3000 ℃.
The present invention makes MCMB carry out phase raw material in the middle of the diauxic growth preparation in pitch by the heat polymerization of step in 2., self-adhesive and the self sintering of MCMB have been improved, and in the middle of step is utilized in 4. the textural defect at phase feed particles edge, middle phase raw material is carried out oxide treatment, introduce oxygen-containing functional group in grain edges, further promoted the self sintering energy of pre-treatment powder.In step sintering process 6., the powder composition is single during owing to moulding, and the contraction that produces in the sintering process is even, can not be produced as tiny crack between particle, can form preferably microtexture, is conducive to improve volume density and physical strength.
Compared with prior art, the present invention possesses following advantage:
Powder is easy to moulding and sintering, can be used in to make large specification product;
Technique is brief, does not need to carry out kneading, rolls sheet and dipping/baking operation repeatedly, and the production cycle shortens dramatically;
The single-phase homogeneous of product, the isotropy degree that utilizes present method to prepare is good, physical strength is high.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, obviously, described embodiment is a part of embodiment of the present invention, rather than whole embodiment.Based on the embodiment among the present invention, the every other embodiment that those of ordinary skills obtain under the prerequisite of not making creative work belongs to the scope of protection of the invention.
Embodiment 1
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 4 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 7.9 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.87g/cm
3, folding strength is 62MPa, the structure anisotropic degree is 1.02.
Embodiment 2
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 88.6 ℃, quinoline insolubles content are 0.4%, β resin content be 16.3%) that with the 100g median size are 11.2 μ m mix, and obtain compound;
2. compound is carried out 4 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 8.4 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.82g/cm
3, folding strength is 47MPa, the structure anisotropic degree is 1.03.
Embodiment 3
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 400g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 4 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 7.7 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.75g/cm
3, folding strength is 16MPa, the structure anisotropic degree is 1.04.
Embodiment 4
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 10 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 8.0 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.91g/cm
3, folding strength is 75MPa, the structure anisotropic degree is 1.02.
Embodiment 5
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 10 hours heat polymerization under 450 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 8.2 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.84g/cm
3, folding strength is 43MPa, the structure anisotropic degree is 1.04.
Embodiment 6
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 10 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 7.9 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 300 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.79g/cm
3, folding strength is 33MPa, the structure anisotropic degree is 1.03.
Embodiment 7
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 10 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 8.3 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 50MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 1200 ℃ and carry out sintering, and soaking time 40 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.84g/cm
3, folding strength is 52MPa, the structure anisotropic degree is 1.02.
Embodiment 8
A kind of method for preparing isotropic graphite, it comprises following step:
1. MCMB and the 100g pitch (softening temperature is that 89.3 ℃, quinoline insolubles content are 0.6%, β resin content be 15.7%) that with the 100g median size are 4.7 μ m mix, and obtain compound;
2. compound is carried out 10 hours heat polymerization under 400 ℃, nitrogen atmosphere protection, phase raw material in the middle of obtaining;
3. with middle phase raw material ball-milling processing, obtaining median size is 8.4 μ m ball milling powders;
4. the ball milling powder is carried out oxide treatment 1 hour in 270 ℃, air atmosphere, obtain the pre-treatment powder;
5. with pre-treatment powder isostatic pressing, forming pressure is 80MPa, and mold temperature is 25 ℃, and molding time is 40 minutes;
6. be warming up to 900 ℃ and carry out sintering, and soaking time 80 hours;
7. be warming up to 2400 ℃, finish greying.
Result of implementation: the volume density of graphite material is 1.85g/cm
3, folding strength is 56MPa, the structure anisotropic degree is 1.03.
Claims (9)
1. method for preparing isotropic graphite, it is characterized in that: it comprises following step:
1. MCMB is mixed with pitch, obtain compound;
2. described compound is carried out heat polymerization, MCMB diauxic growth, phase raw material in the middle of obtaining;
3. with phase raw material ball-milling processing in the middle of described, obtain the ball milling powder;
4. described ball milling powder is carried out oxide treatment, obtain the pre-treatment powder;
5. with described pre-treatment powder isostatic pressing;
6. sintering;
7. greying.
2. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 1. described in the median size of MCMB be 3.0～15.0 μ m, consumption is 20%～80% of described compound gross weight.
3. a kind of method for preparing isotropic graphite as claimed in claim 1, it is characterized in that: step 1. described in the quinoline insolubles mass content of pitch be 0%～1.0%, the β resin content is 10.0%～20.0%, and softening temperature is 85.0～95.0 ℃.
4. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 2. described in the temperature of reaction of heat polymerization be 370～460 ℃, reaction atmosphere is nitrogen or protection of inert gas atmosphere, the reaction times is 1～10 hour.
5. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 3. described in the median size of ball milling powder be 1.0～20.0 μ m.
6. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 4. described in the temperature of oxide treatment be 250～320 ℃, processing atmosphere is air atmosphere, the treatment time is 1～5 hour.
7. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 5. described in the forming pressure of isostatic pressing be 50～100MPa, mold temperature is 20～500 ℃, molding time is 30～300 minutes.
8. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 6. described in the top temperature of roasting be 800～1300 ℃, be 10～100 hours in the soaking time of top temperature point.
9. a kind of method for preparing isotropic graphite as claimed in claim 1 is characterized in that: step 7. described in graphited top temperature be 2000～3000 ℃.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103849411A (en) * | 2014-03-11 | 2014-06-11 | 中钢集团鞍山热能研究院有限公司 | Method for preparing isotropic coke |
| CN103979930A (en) * | 2014-05-09 | 2014-08-13 | 湛江市聚鑫新能源有限公司 | High thermal conductivity of graphite material and preparation method and application thereof |
| CN104446646A (en) * | 2014-12-04 | 2015-03-25 | 大同新成新材料股份有限公司 | Impregnating method of preparing isostatic pressing graphite product |
| CN105271197A (en) * | 2015-11-04 | 2016-01-27 | 湖南大学 | Method for preparing high-strength high-density isotropic graphite material |
| CN105645960A (en) * | 2015-12-11 | 2016-06-08 | 天津工业大学 | Method for preparing isotropic graphite from isotropic asphalt with high softening point through self-sintering |
| CN105884357A (en) * | 2016-04-13 | 2016-08-24 | 湖南省长宇新型炭材料有限公司 | Graphite die material for hot-press molding and preparation method of graphite die material |
| CN107056300A (en) * | 2017-05-18 | 2017-08-18 | 天津工业大学 | A kind of preparation method of high-performance isotropic graphite material |
| CN108083806A (en) * | 2017-12-12 | 2018-05-29 | 中国平煤神马集团开封炭素有限公司 | A kind of hyperfine structure isotropic graphite and preparation method thereof |
| CN108610049A (en) * | 2016-12-09 | 2018-10-02 | 中国钢铁股份有限公司 | Isotropic graphite material, manufacturing method and its application |
| CN110655413A (en) * | 2019-09-18 | 2020-01-07 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849411A (en) * | 2014-03-11 | 2014-06-11 | 中钢集团鞍山热能研究院有限公司 | Method for preparing isotropic coke |
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| CN103979930A (en) * | 2014-05-09 | 2014-08-13 | 湛江市聚鑫新能源有限公司 | High thermal conductivity of graphite material and preparation method and application thereof |
| CN104446646A (en) * | 2014-12-04 | 2015-03-25 | 大同新成新材料股份有限公司 | Impregnating method of preparing isostatic pressing graphite product |
| CN104446646B (en) * | 2014-12-04 | 2016-05-11 | 大同新成新材料股份有限公司 | A kind of dipping method of preparing isostatic pressing formed graphite goods |
| CN105271197A (en) * | 2015-11-04 | 2016-01-27 | 湖南大学 | Method for preparing high-strength high-density isotropic graphite material |
| CN105645960A (en) * | 2015-12-11 | 2016-06-08 | 天津工业大学 | Method for preparing isotropic graphite from isotropic asphalt with high softening point through self-sintering |
| CN105884357A (en) * | 2016-04-13 | 2016-08-24 | 湖南省长宇新型炭材料有限公司 | Graphite die material for hot-press molding and preparation method of graphite die material |
| CN108610049A (en) * | 2016-12-09 | 2018-10-02 | 中国钢铁股份有限公司 | Isotropic graphite material, manufacturing method and its application |
| CN108610049B (en) * | 2016-12-09 | 2021-03-26 | 中国钢铁股份有限公司 | Isotropic graphite material, method for the production thereof and use thereof |
| CN107056300A (en) * | 2017-05-18 | 2017-08-18 | 天津工业大学 | A kind of preparation method of high-performance isotropic graphite material |
| CN108083806A (en) * | 2017-12-12 | 2018-05-29 | 中国平煤神马集团开封炭素有限公司 | A kind of hyperfine structure isotropic graphite and preparation method thereof |
| CN110655413A (en) * | 2019-09-18 | 2020-01-07 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
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Application publication date: 20130403 |