CN103755375A - Binding agent used for carbon materials in high-temperature furnace and application method - Google Patents
Binding agent used for carbon materials in high-temperature furnace and application method Download PDFInfo
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Abstract
The invention provides a binding agent used for carbon materials in a high-temperature furnace and an application method. A preparation method of the binding agent comprises a step of evenly mixing carbonized materials, a dispersing agent, short or milled carbon fibers, short or milled graphite powder, silicon carbide powder and silica powder according to a certain proportion, so as to obtain the binding agent. The binding agent is particularly suitable for binding and surface treating of carbon fiber heat insulating materials in a polycrystalline silicon ingot casting funace, a single crystal silicon stretching furnace, a ceramic sintering furnace, a high temperature heat treatment furnace and other high-temperature furnaces. The binding agent is adopted to paste graphite paper or carbon cloth on a rigid carbon fiber heat insulation material; then curing treatment and carbonation treatment are performed to obtain the rigid carbon fiber heat insulating material pasted with graphite paper or carbon cloth; as the binding agent can prevent permeation of gas in furnaces and solves the problem of loss caused by reaction resulting from direct contact between the gas and the carbon fibers; the airflow washing resistance and certain oxidation resistance can be achieved; the service life of rigid carbon fiber heat insulating materials at a high-temperature environment is effectively prolonged; the energy-saving and cost-reducing effects are achieved; the production efficiency is improved; a great amount of cost is lowered for enterprises.
Description
Technical field
The present invention relates to carbon fiber thermal insulating material technical field, relate generally to carbon material in High Temperature Furnaces Heating Apparatus bonding making and using method with binding agent, particularly as stickup and the surface treatment binding agent of carbon fiber thermal insulating material in the High Temperature Furnaces Heating Apparatuss such as polycrystalline silicon ingot casting, silicon single crystal stretching, ceramic sintering furnace, high-temperature heat treatment stove.
Background technology
Along with scientific and technological progress, there is great demand in the fields such as photovoltaic solar, military affairs, national defence and scientific research to crystalline silicon, rare metal and magneticsubstance.And the production of these materials all has direct or indirect relation with High Temperature Furnaces Heating Apparatus, vacuum oven.In addition, in industrial technology field, workpiece or raw-material pyroprocessing are all completed in vacuum high temperature furnace or inert atmosphere furnace.In High Temperature Furnaces Heating Apparatus, temperature is generally all more than 1350 ℃, this has just proposed very harsh requirement to lagging material---not only required high insulating effect save the energy but also require high temperature resistant pollution-free, the life-span is long, carbon fiber thermal insulating material is because its superior insulative properties, lower volume, low volatile, high strength become the preferred material of soak.
Carbon fiber thermal insulating material, in rare gas element or vacuum, due to its high thermotolerance and extremely low vapour pressure, even can be used under the ultrahigh-temperature of 3000 ℃ of left and right.But, in practical service environment, because the metallic impurity reaction of the oxidizing gas in stove or gasification consumes, efflorescence, embrittlement and sex change.For example, in polycrystalline silicon ingot or purifying furnace, the SiO, the metal impurities gas reaction that in carbon fiber thermal insulating material and ingot furnace, produce, the constantly consumption of carbon fiber thermal insulating material surface, efflorescence, embrittlement, more seriously foreign gas is penetrated into that lagging material is inner to react and sex change with it, make carbon fiber thermal insulating material lose heat-insulating property, life-span reduces greatly, and the dust producing after lagging material efflorescence disperses in stove, polluted product workpiece, cause product foreign matter content to increase, have a strong impact on quality product.
In order to address the above problem, at present the habitual practice is to paste graphite paper at heat insulation material surface, prevents that surface from consuming, and this just needs adhibit quality good, the binding agent of high temperature resistant and good endurance.
Summary of the invention
The invention provides a kind of high-temperature agglomerant and using method thereof that is applicable to high-density rigid carbon-fiber lagging material, adopt the rigid carbon-fiber lagging material of adhesive treatment of the present invention, because it can prevent that furnace gas from permeating and completely cutting off gas, directly contact to react with carbon fiber and cause loss, make it have anti-airflow scouring and certain oxidation-resistance, can greatly improve the life-span of rigid carbon-fiber lagging material.And the graphite paper/carbon cloth Reusability that uses this binding agent to paste there will not be, and graphite paper/carbon cloth comes off, peeling.
In order to achieve the above object, the present invention realizes by the following technical solutions:
Carbon material binding agent in a kind of High Temperature Furnaces Heating Apparatus, by can char-forming material, dispersion agent, short cut or ground carbon fiber, Graphite Powder 99, carborundum powder, silica flour are mixed in proportion to stir and make, the weight ratio of each component is: can char-forming material 40-100 part, dispersion agent 40-160 part, short cutting or ground carbon fiber 5-20 part, Graphite Powder 99 25-50 part, carborundum powder 10-30 part, silica flour 5-20 part;
Described can char-forming material be a kind of, two or more combination of resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar;
Described dispersion agent is a kind of, two or more combination in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene or toluene;
Described short cut or ground carbon fiber is a kind of, two or more combination of asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber; Described short cut or ground carbon fiber mean length is 10-1200 μ m, more preferably mean length is 50-400 μ m;
Described Graphite Powder 99 is natural flake graphite; Described Graphite Powder 99 granularity is 10-600 μ m, and more preferably granularity is 30-300 μ m;
Described carborundum powder granularity is 200-1000 order, and more preferably granularity is at 300-800 order;
Described silicon particle size is 200-1000 order, and more preferably granularity is at 300-800 order.
In described High Temperature Furnaces Heating Apparatus, the using method of binding agent for carbon material, comprises the steps:
(1) rigid carbon-fiber lagging material is carried out to cut edge, Xiu Jiao, planing surface and machine and add processing, make goods reach surfacing, purge surperficial chip and make surface without tiny carbon fiber; Then with dehydrated alcohol, clean and skimming treatment, then in baking oven dry for standby at 110～130 ℃;
(2) according to the graphite paper using or carbon cloth size cutting graphite paper or carbon cloth; Graphite paper thickness is 0.1-5mm;
(3) the described binding agent of brush 1～4 time on the rigid carbon-fiber lagging material of drying and graphite paper or carbon cloth, its brushing method is: after front initial adhesion agent of once brushing is dried, then after brush once; After the rigid carbon-fiber lagging material of having brushed and graphite paper or carbon cloth dry, they are fit together, and roll extrusion discharge bubble, clamp then used; Described consumption of binder is according to 150-1300g/m
2.
(4) solidify, the rigid carbon-fiber lagging material of upper fixture and graphite paper or carbon cloth are put into baking oven, make binding agent at 150～350 ℃ of curing 1～5.5h, be formed with the solidifying product of certain bonding strength;
(5) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 ℃-1800 ℃ or vacuum atmosphere by solidifying product, can obtain the rigid carbon-fiber lagging material of surface label graphite paper or carbon cloth.
More preferably: as stated above, first paste one or more layers carbon cloth and paste graphite paper again on rigid carbon-fiber lagging material, effect is better.
Advantage of the present invention is according to requirements rigid carbon-fiber lagging material to be carried out the stickup of graphite paper/carbon cloth, preventing that furnace gas from permeating and completely cutting off gas directly contacts with carbon fiber and reacts and cause loss, anti-airflow scouring, there is certain oxidation-resistance, effectively extend the work-ing life of carbon fiber thermal insulating material under hot environment, energy-saving and cost-reducing, improved production efficiency, for enterprise can save great amount of cost.And the graphite paper/carbon cloth Reusability that uses this binding agent to paste there will not be, and graphite paper/carbon cloth comes off, peeling.
Embodiment
Below by embodiment, carbon material of the present invention is described in further detail with method of preparation and use and the example of binding agent.
Carbon material binding agent in High Temperature Furnaces Heating Apparatus, by material, dispersion agent, short cutting or ground carbon fiber that can carbonization, Graphite Powder 99, carborundum powder and silica flour mix and make, as described below:
(1) can char-forming material, as a kind of, two or more combination of resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch, tar;
(2) dispersion agent is as a kind of, two or more combination of methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene, toluene;
(3) carbon fiber, as a kind of, two or more combination of asphalt base carbon fiber, viscose-based carbon fiber, polypropylene cyano group carbon fiber, carbon fiber mean length is 10-1200 μ m, more preferably mean length is 50-400 μ m.
(4) crystalline graphite powder, particle diameter is 10-600 μ m, more preferably particle diameter is at 30-300 μ m.
(5) carborundum powder, granularity is 200-1000 order, more preferably granularity is at 300-800 order.
(6) silica flour, granularity is 200-1000 order, more preferably granularity is at 300-800 order.
Carbon material makes with the ratio mixing by weight of the above raw material of binding agent, 40-100 part can char-forming material, 40-160 part dispersion agent, 5-20 part is short cuts or ground carbon fiber, 25-50 part crystalline flake graphite, 10-30 part carborundum powder and 5-20 part silica flour, mixed according to the above ratio, can obtain carbon material binding agent.Above raw material all can obtain from commercially available prod.
Then use above-mentioned binding agent to paste graphite paper/carbon cloth to rigid carbon-fiber heat insulation material surface, graphite paper thickness is generally at 0.1-5mm, more preferably graphite paper thickness is at 0.2-1.5mm, more preferably graphite paper thickness is at 0.2-1.0mm, solidify again the rigid carbon-fiber lagging material that carbonizing treatment obtains surface label graphite paper/carbon cloth, because it can prevent that furnace gas from permeating and completely cutting off gas, directly contact to react with carbon fiber and cause loss, make it have anti-airflow scouring and certain oxidation-resistance, can greatly improve the life-span of rigid carbon-fiber lagging material.
The concrete steps of the rigid carbon-fiber lagging material of stickup graphite paper/carbon cloth are as follows:
(1) carbon material is prepared with binding agent: by above-mentioned raw materials and parts by weight of component, prepare described binding agent, and standby.
(2) rigid carbon-fiber lagging material is carried out to the processing such as cut edge, Xiu Jiao, planing surface and machine add, make goods reach surfacing, purge surperficial chip and make surface without tiny carbon fiber, rigid carbon-fiber lagging material density is 0.1～0.4g/cm
3; Then with dehydrated alcohol, clean and skimming treatment, then in baking oven dry for standby at 110～130 ℃.
(3) according to the graphite paper/carbon cloth size cutting graphite paper/carbon cloth using.Graphite paper thickness is generally at 0.1-5mm, and more preferably graphite paper thickness is at 0.2-1.5mm, and more preferably graphite paper thickness is at 0.2-1.0mm.
(4) on the rigid carbon-fiber lagging material of drying and graphite paper/carbon cloth, brush binding agent 1～4 time, its brushing method is: after front initial sizing agent of once brushing dries, then after brush once; After the sample of having brushed dries, they are bonded together, and roll extrusion discharge bubble, clamp then used.Consumption of binder is according to 150-1300g/m
2, 230-900g/m more preferably
2.
(5) solidify, the rigid carbon-fiber lagging material of upper fixture and graphite paper or carbon cloth are put into baking oven, make binding agent at 150～350 ℃ of curing 1～5.5h, be formed with the solidifying product of certain bonding strength.
(6) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 ℃-1800 ℃ or vacuum atmosphere by solidifying product, can obtain the rigid carbon-fiber lagging material of surface label graphite paper/carbon cloth.
More preferably: as stated above, first paste one or more layers carbon cloth and paste graphite paper again on rigid carbon-fiber lagging material, effect is better.Concrete using method is described below:
The using method of binding agent for carbon material in described High Temperature Furnaces Heating Apparatus, comprises the steps (take paste one deck carbon cloth and graphite paper is example narration):
(1) to density, be 0.1～0.4g/cm
3rigid carbon-fiber lagging material carry out cut edge, Xiu Jiao, planing surface and machine and add processing, make goods reach surfacing, purge surperficial chip and make surface without tiny carbon fiber; Then with dehydrated alcohol, clean and skimming treatment, then in baking oven dry for standby at 110～130 ℃;
(2) according to the graphite paper using, carbon cloth size cutting graphite paper or carbon cloth; Graphite paper thickness is 0.1-5mm, and more preferably graphite paper thickness is at 0.2-1.5mm, and more preferably graphite paper thickness is at 0.2-1.0mm;
(3) the described binding agent of brush 1～4 time on the rigid carbon-fiber lagging material of drying and graphite paper, carbon cloth, its brushing method is: after front initial adhesion agent of once brushing is dried, then after brush once; After the rigid carbon-fiber lagging material of having brushed and graphite paper, carbon cloth dry, rigid carbon-fiber lagging material, carbon cloth, graphite paper are fit together, and roll extrusion discharge bubble, clamp then used; Described consumption of binder is according to 150-1300g/m
2, 230-900g/m more preferably
2.
(4) solidify, the rigid carbon-fiber lagging material of upper fixture is put into baking oven, make binding agent at 150～350 ℃ of curing 1～5.5h, be formed with the solidifying product of certain bonding strength;
(5) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 ℃-1800 ℃ or vacuum atmosphere by solidifying product, can obtain the rigid carbon-fiber lagging material of surface label carbon cloth and graphite paper.
Example 1
(1) adopt isotropic asphalt base carbon fiber production inflexibility carbon fiber thermal insulating material, density 0.16g/cm
3, lagging material is carried out to machine and add, make its surfacing and it is purged, then use dehydrated alcohol clean surface, then it is standby in baking oven, at 110～130 ℃, to dry 2h.
(2) each components by weight of binding agent is resol: ethanol: asphalt base carbon fiber: Graphite Powder 99: carborundum powder: silica flour=55:45:10:25:10:10, mixes and make carbon material binding agent.
(3) according to the thick graphite paper of demand size cutting 0.5mm, by carbon material with binding agent with the even scrubbing brush of brush on rigid carbon-fiber lagging material and graphite paper, according to 500g/m
2, then graphite paper being adhered on rigid carbon-fiber heat insulation material surface, roll extrusion has prevented bubble, then uses clamp 200 ℃ of curing 2h in baking oven.
(4) carbonization, carbonization 2h in the vacuum oven of 1800 ℃, obtains the rigid carbon-fiber lagging material of surface label graphite paper.
Above-mentioned rigid carbon-fiber lagging material is used in polycrystalline silicon ingot or purifying furnace, use 4320h, heat insulation material surface is still better, there is not the phenomenons such as surperficial consumption, dry linting, embrittlement, graphite paper come off, and silicon ingot mass ratio is higher and more stable, greatly improved the work-ing life of lagging material.
Example 2
(1) adopt isotropic asphalt base carbon fiber production inflexibility carbon fiber thermal insulating material, density 0.18g/cm
3, lagging material is carried out to machine and add, make its surfacing and it is purged, then use dehydrated alcohol clean surface, then it is standby in baking oven, at 110～130 ℃, to dry 2h.
(2) each components by weight of binding agent is resol: ethanol: asphalt base carbon fiber: Graphite Powder 99: carborundum powder: silica flour=60:40:8:28:8:6, mixes and make carbon material binding agent.
(3) according to thick graphite paper and the carbon cloth of demand size cutting 0.5mm, by carbon material with binding agent with the even scrubbing brush of brush on rigid carbon-fiber lagging material and carbon cloth, according to 480g/m
2, then carbon cloth being adhered on rigid carbon-fiber heat insulation material surface, roll extrusion has prevented bubble; Brush coating on carbon cloth and graphite paper again, according to 400g/m
2, then graphite paper being adhered on carbon cloth, roll extrusion has prevented bubble, then by clamp, puts into 200 ℃ of curing 2h of baking oven.
(4) carbonization, carbonization 2h in the inert atmosphere furnace of 1200 ℃, obtains the rigid carbon-fiber lagging material of surface label one deck carbon cloth graphite paper.
Above-mentioned rigid carbon-fiber lagging material is used in quenching furnance, use 7200h, heat insulation material surface is still better, its anti-airflow scouring better performances, there is not the phenomenons such as surperficial consumption, dry linting, embrittlement, carbon cloth graphite paper come off, and the quality product of producing is higher, does not occur the phenomenons such as workpiece contamination, has greatly improved the work-ing life of lagging material.
Specific examples described in this specification sheets just illustrates the technical scheme of this patent but not restriction to this patent.Other technical scheme based on inventive concept, all within rights protection scope of the present invention.
Claims (3)
1. carbon material binding agent in a High Temperature Furnaces Heating Apparatus, it is characterized in that, by can char-forming material, dispersion agent, short cut or ground carbon fiber, Graphite Powder 99, carborundum powder, silica flour are mixed in proportion to stir and make, the weight ratio of each component is: can char-forming material 40-100 part, dispersion agent 40-160 part, short cutting or ground carbon fiber 5-20 part, Graphite Powder 99 25-50 part, carborundum powder 10-30 part, silica flour 5-20 part;
Described can char-forming material be a kind of, two or more combination of resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar;
Described dispersion agent is a kind of, two or more combination in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene or toluene;
Described short cut or ground carbon fiber is a kind of, two or more combination of asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber; Described short cut or ground carbon fiber mean length is 10-1200 μ m;
Described Graphite Powder 99 is natural flake graphite; Described Graphite Powder 99 granularity is 10-600 μ m;
Described carborundum powder granularity is 200-1000 order;
Described silicon particle size is 200-1000 order.
2. the using method of binding agent for carbon material in High Temperature Furnaces Heating Apparatus according to claim 1, is characterized in that, comprises the steps:
(1) rigid carbon-fiber lagging material is carried out to cut edge, Xiu Jiao, planing surface and machine and add processing, make goods reach surfacing, purge surperficial chip and make surface without tiny carbon fiber; Then with dehydrated alcohol, clean and skimming treatment, then in baking oven dry for standby at 110～130 ℃;
(2) according to the graphite paper using or carbon cloth size cutting graphite paper or carbon cloth; Graphite paper thickness is 0.1-5mm;
(3) the described binding agent of brush 1～4 time on the rigid carbon-fiber lagging material of drying and graphite paper or carbon cloth, its brushing method is: after front initial adhesion agent of once brushing is dried, then after brush once; After the rigid carbon-fiber lagging material of having brushed and graphite paper or carbon cloth dry, they are fit together, and roll extrusion discharge bubble, clamp then used; Described consumption of binder is according to 150-1300g/m
2.
(4) solidify, the rigid carbon-fiber lagging material of upper fixture and graphite paper or carbon cloth are put into baking oven, make binding agent at 150～350 ℃ of curing 1～5.5h, be formed with the solidifying product of certain bonding strength;
(5) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 ℃-1800 ℃ or vacuum atmosphere by solidifying product, can obtain the rigid carbon-fiber lagging material of surface label graphite paper or carbon cloth.
3. the using method of binding agent for carbon material in High Temperature Furnaces Heating Apparatus according to claim 2, is characterized in that, by described method, first paste one or more layers carbon cloth and paste graphite paper again on rigid carbon-fiber lagging material, effect is better.
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| CN104261853A (en) * | 2014-09-26 | 2015-01-07 | 辽宁奥亿达新材料有限公司 | Pitch-based carbon fiber non-woven felt heat-insulating cylinder and preparation method thereof |
| CN108218460A (en) * | 2018-01-24 | 2018-06-29 | 航天睿特碳材料有限公司 | A kind of middle low-density surface of carbon/carbon composite Enhancement Method |
| CN108558268A (en) * | 2018-06-22 | 2018-09-21 | 西南石油大学 | A kind of fibre reinforced high temperature resistant adhesive and preparation method thereof |
| CN114804926A (en) * | 2022-04-27 | 2022-07-29 | 辽宁金谷炭材料股份有限公司 | Repairing method of composite heat-insulating material |
| CN115368146A (en) * | 2022-10-24 | 2022-11-22 | 山东红点新材料有限公司 | Non-asphalt-based adhesive for producing carbon product and preparation method thereof |
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Address after: 114044 Liaoning city of Anshan province Anqian high tech Industrial Development Zone, Road No. 295 Patentee after: Anshan Senoda Technology Co.,Ltd. Address before: 114044 Liaoning city of Anshan province Anqian high tech Industrial Development Zone, Road No. 295 Patentee before: ANSHAN SINOCARB CARBON FIBERS CO.,LTD. |
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Effective date of registration: 20230228 Address after: 114000 Zhouzheng Street Office, Teng'ao Town, Haicheng City, Anshan City, Liaoning Province Patentee after: LIAONING AOYIDA ADVANCED MATERIAL Co.,Ltd. Address before: 114044 Liaoning city of Anshan province Anqian high tech Industrial Development Zone, Road No. 295 Patentee before: Anshan Senoda Technology Co.,Ltd. |
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Address after: 114000 Zhouzheng Street Office, Teng'ao Town, Haicheng City, Anshan City, Liaoning Province Patentee after: Liaoning Aoyida New Materials Co.,Ltd. Address before: 114000 Zhouzheng Street Office, Teng'ao Town, Haicheng City, Anshan City, Liaoning Province Patentee before: LIAONING AOYIDA ADVANCED MATERIAL Co.,Ltd. |