CN105218112A - A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof - Google Patents
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof Download PDFInfo
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- CN105218112A CN105218112A CN201510614217.6A CN201510614217A CN105218112A CN 105218112 A CN105218112 A CN 105218112A CN 201510614217 A CN201510614217 A CN 201510614217A CN 105218112 A CN105218112 A CN 105218112A
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Abstract
The invention discloses a kind of carbon containing refractory micro crystal graphite powder and preparation method thereof, preparation process comprises: the resol of 5 ~ 35wt% is dissolved in the alcohol of 10 ~ 35wt% by A., and adding the micro crystal graphite of 40 ~ 80wt%, magnetic agitation mixing 2 ~ 10 minutes, obtains thickener; B. thickener is put into baking oven low-temperature heat treatment 8 ~ 24 hours, after cooling, obtain cured article; C. cross 325 mesh sieves by after cured article ball milling, obtain ball milling powder; D. by ball milling powder high temperature cabonization 1 ~ 4 hour under the condition of isolated air, carbon containing refractory micro crystal graphite powder after cooling, is namely obtained.Present invention process is simple, with low cost, not only increase resource utilization and the added value of product of micro crystal graphite, alleviate the predicament of crystalline flake graphite resource exhaustion, and the carbon containing refractory of the micro crystal graphite power production utilizing the method to obtain has good thermal shock resistance and anti-scour property, can meet service requirements.
Description
Technical field
The invention belongs to graphite composite powder technical field, particularly relate to a kind of carbon containing refractory micro crystal graphite powder and preparation method.
Background technology
Carbon containing refractory refers to be made up of carbon or carbon compound, and main ingredient is the refractory product of carbon.Carbon containing refractory, with high temperature resistant, the anti-erosion of its excellence and thermal shock resistance, has a wide range of applications in Iron And Steel Industry.Current production carbon containing refractory is generally using the low crystalline flake graphite of foreign matter content as carbon source.But along with a large amount of consumption of crystalline flake graphite, crystalline flake graphite is faced with the problem of resource exhaustion.For another rich reserves domestic and cheap micro crystal graphite resource, if the carbon source into producing carbon containing refractory can be developed to, to solving the Resource Difficulties of crystalline flake graphite and improving the utilization ratio of micro crystal graphite and added value has realistic meaning.
But natural micro crystal graphite foreign matter content is higher, and these impurity can form a large amount of liquid phase under the high temperature conditions, the mechanical behavior under high temperature of refractory materials is caused to decline.In order to address this problem, the method of being calcined by high-temperature alkali in prior art is purified to micro crystal graphite, though this behave decreases the content of impurity in micro crystal graphite, but production stage is complicated, high-temperature alkali calcination process is high to equipment requirements, technique controlling difficulty is large, and considerably increases production cost.
Summary of the invention
The present invention is in order to overcome prior art deficiency, provide a kind of preparation technology carbon containing refractory micro crystal graphite powder simple and with low cost and preparation method, the carbon containing refractory micro crystal graphite powder body material prepared by the method can to reduce in micro crystal graphite impurity to the impact of refractory materials high-temperature behavior, make the refractory materials containing this micro crystal graphite powder have good thermal shock resistance and anti-scour property, this powder can meet carbon containing refractory and generates and use the requirement to graphite.
Concrete scheme is:
A kind of carbon containing refractory micro crystal graphite raw powder's production technology, comprises the following steps:
A. be dissolved in the alcohol of 10 ~ 35wt% by the resol of 5 ~ 35wt%, and add the micro crystal graphite of 40 ~ 80wt%, magnetic agitation mixing 2 ~ 10 minutes, obtains thickener;
B. thickener is put into baking oven low-temperature heat treatment 8 ~ 24 hours, after cooling, obtain cured article;
C. cross 325 mesh sieves by after cured article ball milling, obtain ball milling powder;
D. by ball milling powder high temperature cabonization 1 ~ 4 hour under the condition of isolated air, carbon containing refractory micro crystal graphite powder after cooling, is namely obtained.
Further, the alcohol described in steps A is raw spirit, and massfraction >=99.7% of wherein ethanol;
Further, the resol described in steps A is liquid ammonia resol, its carbon yield >=51.3%.
Further, the thermal treatment temp described in step B is 110 ~ 300 DEG C.
Further, the carbonization temperature described in step D is 600 ~ 1000 DEG C.
Further, the particle diameter of the carbon containing refractory micro crystal graphite powder obtained by aforesaid method is 3 ~ 500 μm,
Further, the carbon content >=90wt% of the carbon containing refractory micro crystal graphite powder obtained by aforesaid method.
Compared with prior art, useful point of the present invention is: wetting good in alcohol with micro crystal graphite powder under the resol normal temperature 1, in this programme, resol is made fully to be coated on micro crystal graphite powder surface, micro crystal graphite powder surface coated one deck resin RESEARCH OF PYROCARBON after high temperature cabonization, obtaining internal layer is micro crystal graphite, and skin is the micro crystal graphite powder of the nucleocapsid structure of resin RESEARCH OF PYROCARBON.Carbon containing refractory prepared by the present invention is with for micro crystal graphite powder is in applied at elevated temperature process, due to be distributed in micro crystal graphite surface or hole in impurity wrap up by resin RESEARCH OF PYROCARBON, low melting point is cut off by resin RESEARCH OF PYROCARBON, a large amount of successional liquid phase can not be formed, thus improve with micro crystal graphite the mechanical behavior under high temperature of the carbon containing refractory being carbon source production.
2, the preparation method of this programme only comprises pre-mixing, subzero treatment, ball milling and carburising step, technique is simple, with low cost, not only increase resource utilization and the added value of product of micro crystal graphite, alleviate the predicament of crystalline flake graphite resource exhaustion, and utilize the carbon containing refractory of this micro crystal graphite power production to have good thermal shock resistance and anti-scour property, can service requirements be met.The present invention, in the preparation of carbon containing refractory, especially has broad application prospects in magnesium carbon, aluminum-carbon refractory material preparation.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, the restriction not to its protection domain.
For avoiding repetition, existing by as follows for the technical parameter Unify legislation involved by this embodiment, do not repeating in enforcement:
Resol is liquid, wherein: resol is the ammonia resol of carbon yield >=51.3%.
Alcohol is raw spirit, wherein: massfraction >=99.7% of ethanol.
The particle diameter of micro crystal graphite powder is 3 ~ 500 μm, carbon content >=90wt% in micro crystal graphite powder.
Implementation column 1
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 20 ~ 25wt% resol is dissolved in 30 ~ 35wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 40 ~ 45wt%, put into baking oven, thermal treatment 8 ~ 12 hours at 110 ~ 150 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 1 ~ 2 hour at 600 ~ 700 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
Implementation column 2
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 15 ~ 20wt% resol is dissolved in 25 ~ 30wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 50 ~ 60wt%, put into baking oven, thermal treatment 12 ~ 16 hours at 150 ~ 200 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 2 ~ 3 hours at 700 ~ 800 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
Implementation column 3
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 10 ~ 15wt% resol is dissolved in 20 ~ 25wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 60 ~ 70wt%, put into baking oven, thermal treatment 16 ~ 20 hours at 200 ~ 250 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 3 ~ 4 hours at 800 ~ 900 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
Implementation column 4
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 5 ~ 10wt% resol is dissolved in 15 ~ 20wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 70 ~ 80wt%, put into baking oven, thermal treatment 20 ~ 24 hours at 250 ~ 300 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 4 ~ 5 hours at 900 ~ 1000 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
Implementation column 5
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 20 ~ 25wt% resol is dissolved in 10 ~ 15wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 60 ~ 70wt%, put into baking oven, thermal treatment 16 ~ 20 hours at 110 ~ 150 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 1 ~ 2 hour at 800 ~ 900 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
Implementation column 6
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 25 ~ 30wt% resol is dissolved in 15 ~ 20wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 50 ~ 60wt%, put into baking oven, thermal treatment 12 ~ 16 hours at 150 ~ 200 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 2 ~ 3 hours at 700 ~ 800 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
Implementation column 7
A kind of carbon containing refractory micro crystal graphite powder and preparation method thereof.First 30 ~ 35wt% resol is dissolved in 20 ~ 25wt% alcohol, 2 ~ 10 minutes are mixed with the micro crystal graphite magnetic agitation of 40 ~ 50wt%, put into baking oven, thermal treatment 8 ~ 12 hours at 250 ~ 300 DEG C, ball milling after cooling also crosses 325 mesh sieves, then isolated air, carbonizing treatment 3 ~ 4 hours at 600 ~ 700 DEG C, naturally cooling, both obtained carbon containing refractory micro crystal graphite powder.
This embodiment is pulverized after carrying out subzero treatment to pre-mixing raw material.Wetting good in alcohol with micro crystal graphite powder under resol normal temperature in raw material, resol is made to be coated on micro crystal graphite powder surface, after subzero treatment, micro crystal graphite powder surface coated one deck resin RESEARCH OF PYROCARBON, obtaining internal layer is micro crystal graphite, and skin is the micro crystal graphite powder of the nucleocapsid structure of resin RESEARCH OF PYROCARBON.Carbon containing refractory prepared by the present invention is with for micro crystal graphite powder is in applied at elevated temperature process, due to be distributed in micro crystal graphite surface or hole in impurity wrap up by resin RESEARCH OF PYROCARBON, low melting point is cut off by resin RESEARCH OF PYROCARBON, a large amount of successional liquid phase can not be formed, thus improve the mechanical behavior under high temperature containing micro crystal graphite refractory materials.
This embodiment adopts pre-mixing, Low temperature processing techniques and disintegrating process again, and generating process is simple, with low cost, not only increases resource utilization and the added value of product of micro crystal graphite, and alleviates the predicament of crystalline flake graphite resource exhaustion.This micro crystal graphite powder has broad application prospects in the preparation of carbon containing refractory, especially magnesium carbon, aluminum-carbon refractory material.
Therefore, the micro crystal graphite powder prepared by this embodiment can make the refractory materials containing this micro crystal graphite powder have good thermal shock resistance and anti-scour property, and this powder can meet carbon containing refractory and generates and use the requirement to graphite.
Claims (8)
1. a carbon containing refractory micro crystal graphite raw powder's production technology, is characterized in that, comprise the following steps:
A. be dissolved in the alcohol of 10 ~ 35wt% by the resol of 5 ~ 35wt%, and add the micro crystal graphite of 40 ~ 80wt%, magnetic agitation mixing 2 ~ 10 minutes, obtains thickener;
B. thickener is put into baking oven low-temperature heat treatment 8 ~ 24 hours, after cooling, obtain cured article;
C. cross 325 mesh sieves by after cured article ball milling, obtain ball milling powder;
D. by ball milling powder high temperature cabonization 1 ~ 4 hour under the condition of isolated air, carbon containing refractory micro crystal graphite powder after cooling, is namely obtained.
2. a kind of carbon containing refractory micro crystal graphite raw powder's production technology according to claim 1, is characterized in that: the alcohol described in steps A is raw spirit, and massfraction >=99.7% of wherein ethanol.
3. a kind of carbon containing refractory micro crystal graphite raw powder's production technology according to claim 1, is characterized in that: the resol described in steps A is liquid ammonia resol, its carbon yield >=51.3%.
4. a kind of carbon containing refractory micro crystal graphite raw powder's production technology according to claim 1, is characterized in that: the thermal treatment temp described in step B is 110 ~ 300 DEG C.
5. a kind of carbon containing refractory micro crystal graphite raw powder's production technology according to claim 1, is characterized in that: the carbonization temperature described in step D is 600 ~ 1000 DEG C.
6. the carbon containing refractory micro crystal graphite powder that a kind of carbon containing refractory micro crystal graphite raw powder's production technology as described in any one of claim 1-5 is obtained.
7. a kind of carbon containing refractory micro crystal graphite powder according to claim 6, is characterized in that: the particle diameter of described carbon containing refractory micro crystal graphite powder is 3 ~ 500 μm.
8. a kind of carbon containing refractory micro crystal graphite powder according to claim 6, is characterized in that: the carbon content >=90wt% of described carbon containing refractory micro crystal graphite powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111004042A (en) * | 2019-12-05 | 2020-04-14 | 江苏苏嘉集团新材料有限公司 | Magnesia carbon brick using microcrystalline graphite |
Citations (3)
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| CN101654239A (en) * | 2009-08-27 | 2010-02-24 | 清华大学 | Isotropic graphite product and preparation method thereof |
| CN101859893A (en) * | 2010-05-27 | 2010-10-13 | 深圳市德兴富电池材料有限公司 | Preparation method of lithium ion battery anode material |
| CN104600305A (en) * | 2013-10-31 | 2015-05-06 | 青岛泰浩达碳材料有限公司 | Modification method of carbon material used for lithium ion batteries |
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- 2015-09-24 CN CN201510614217.6A patent/CN105218112A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101654239A (en) * | 2009-08-27 | 2010-02-24 | 清华大学 | Isotropic graphite product and preparation method thereof |
| CN101859893A (en) * | 2010-05-27 | 2010-10-13 | 深圳市德兴富电池材料有限公司 | Preparation method of lithium ion battery anode material |
| CN104600305A (en) * | 2013-10-31 | 2015-05-06 | 青岛泰浩达碳材料有限公司 | Modification method of carbon material used for lithium ion batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111004042A (en) * | 2019-12-05 | 2020-04-14 | 江苏苏嘉集团新材料有限公司 | Magnesia carbon brick using microcrystalline graphite |
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Address after: Industrial agglomeration area in Henan province Jiaozuo city 454450 county (Guangxing Road No. 688) Jin Xin Jiaozuo hengtuo new materials Limited by Share Ltd Applicant after: Jiaozuo Jin Xin Heng Tuo new material Limited by Share Ltd Address before: Industrial agglomeration area in Henan province Jiaozuo city county 454450 (pine Avenue South East) Jiaozuo Jin Xin hengtuo high temperature materials Co. Ltd. Applicant before: Jiaozuo Jinxin Hengtuo Refractories Co., Ltd. |
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