CN101628816B - Method for manufacturing high-density rigid carbon-fiber heat-insulation material - Google Patents
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Abstract
The invention relates to a method for manufacturing a high-density rigid carbon-fiber heat-insulation material. The method comprises the following steps: fully and evenly mixing ground or cut carbon fibers with a bonding agent and a dispersing agent, wherein the ground or cut carbon fiber accounts for 20 to 80 portions by weight, the bonding agent accounts for 80 to 20 portions by weight, and the weight ratio of the bonding agent to the dispersing agent is 1:0.4-1:1; carrying out pouring and compression molding on the mixture to obtain a prefab product made of rigid heat-insulation material of specified shape; and carrying out infusible treatment and carbonization treatment to manufacture rigid carbon-fiber heat-insulation material. The method has the advantages of simple process, high stability and convenient operation. Due to the characteristics of excellent heat insulation performance, low thermal capacity, low density, high strength, and the like, the high-density rigid carbon-fiber heat-insulation material is particularly suitable to be used as a heat-insulation material for high-temperature furnaces such as vacuum heat treatment furnaces, single crystal pulling furnace, ceramic sintering furnace and the like.
Description
Technical field
The present invention relates to the carbon-fiber heat-insulation material technical field, particularly as the manufacture method of the high-density rigid carbon-fiber heat-insulation material that uses in the stoves such as crystal growing furnace and crystal pulling apparatus, ceramic sintering furnace, vacuum high-temperature heat treatment furnace.
Background technology
The shortcomings such as employed heat-insulating heat-preserving material generally adopts soft carbon felt (Nomex) in the present domestic high-temperature vacuum furnace, and there is low, yielding, the easy efflorescence of intensity in the heat-insulating heat-preserving material of this structure, effect of heat insulation is poor and dismantle, installation is wasted time and energy.And rigid carbon-fiber heat-insulation material will overcome the existing shortcoming of this heat-insulation and heat-preservation of soft carbon felt, as crystal furnace, and ceramic sintering furnace, the high temperature furnace used heat-insulating heat-preserving material such as gaseous phase deposition stove will be widely used.
The hard felt of present domestic carbon fiber mainly adopts soft carbon felt dipping mold pressing or the layering of soft carbon felt dipping to paste the moulding process of (paste at graphite paper and carbon fiber interval).The shortcoming that the dipping former compression technology exists is that product strength is low, the easy delamination splitting of goods under the applied at elevated temperature condition, and work-ing life is short etc., because intensity is relatively low, it is convenient not to remove and install; The hard felt that adopts layering stickup shaping mode to make, although intensity increases, the thermal conductivity of goods increases, the heat-insulating property variation reduces effect of heat insulation.
Japanese Patent 29129/1983 discloses a kind of method of utilizing the hard felt of carbon fiber flexible felt production.Concrete grammar is that (1) becomes soft felt with carbon fiber acupuncture, and to the soft felt resin by injection of multilayer solution, compression and carbonization obtain the hard felt of carbon fiber; (2) with the carbon felt with roll together by binding agent less than the thick graphite flake of 1mm.This method requirement carbon fiber strength is higher and have better toughness, and this has limited the use of carbon fiber; Acupuncture and two step of injection cakingagent efficient and productivity are all very low; It is pouring-in that cakingagent adopts, and can cause its carbon felt internal bond agent skewness, after the carbonization so that carbon felt internal bond agent carbon residue skewness, thereby intensity is inhomogeneous, is restricted when causing it to use; And the carbon fiber thermal insulating material density that this method makes is all smaller, generally is lower than 0.1g/cm
3, so that its processing characteristics is poor.And whole production technique more complicated.
Summary of the invention
The problem that exists for solving prior art, the manufacture method that the purpose of this invention is to provide a kind of high-density rigid carbon-fiber heat-insulation material, the rigid carbon-fiber lagging material that adopts the method to make, because the characteristics such as its excellent heat-proof quality, low heat capacity, low density and high strength are specially adapted to the high temperature furnace used lagging materials such as vacuum heat treatment furnace, monocrystalline crystal pulling furnace, ceramic sintering furnace.
The present invention is achieved through the following technical solutions:
A kind of manufacture method of high-density rigid carbon-fiber heat-insulation material, the method comprises the steps:
1) ground carbon fiber, obtaining mean length is grinding of 0.2-30mm or chopped carbon fiber;
2) will grind or chopped carbon fiber and binding agent, dispersion agent fully mix, grind or chopped carbon fiber, weight of binder part ratio are: ground carbon fiber 20～80 weight parts, binding agent 80～20 weight parts, the part by weight of binding agent and dispersion agent is 1: (0.4～1);
3) said mixture is poured into a mould, compression molding, make the rigid heat insulating material prefabrication of regulation shape;
4) with the heating rate of 5～65 ℃/h above-mentioned rigid heat insulating material preform is heated to 180～350 ℃ and carries out not melt processed;
5) will be not preform carbonization under vacuum or inert atmosphere after the melt processed, temperature is 1000～1800 ℃;
Or graphitization processing, graphitization temperature is 1800～2500 ℃, produces the rigid carbon-fiber lagging material.
Described carbon fiber is selected from a kind of in asphalt base carbon fiber, PAN base carbon fibre, the viscose-based carbon fiber.
Described binding agent is selected from one or more in pitch fibers or powdered asphalt, tar, thermosetting resin resol, urea-formaldehyde resin, Resins, epoxy, furane resin, vinyl ester resin, red shortness's resin polyethylene, polypropylene, ethylene propylene copolymer, polymeric amide, polystyrene, the acrylic resin.
Described dispersion agent is selected one or more of methyl alcohol, ethanol, butanols, acetone, diacetone alcohol, pimelinketone, methylethylketone, vinyl acetic monomer, N-BUTYL ACETATE organic thinner.
For increasing the surface property of rigid carbon-fiber lagging material, need to carry out surface treatment to it, its surface treatment method comprises the steps:
1) carbonization/graphited rigid carbon-fiber lagging material is carried out surface grinding and process, make surfacing;
2) the rigid carbon-fiber lagging material brushing binding agent after smooth forms adhesive layer, pastes graphite paper, Graphite cloth, carbon cloth at adhesive layer; Ratio is formulated by weight by resin and norbide for described binding agent, and the part by weight of resin and norbide is 100: (40～160), according to the above ratio resin and norbide are mixed, namely obtain high-temperature agglomerant; Described resin is selected from one or more in resol, Resins, epoxy or the urea aldehyde;
3) temperature rise rate with 1～15 ℃/min is warmed up to 150～350 ℃, constant temperature 1～5.5h under this temperature, and the cured binders layer is made preform;
4) with preform carbonization under inert atmosphere under 1000 ℃～1800 ℃, make pad pasting/coating rigid carbon-fiber lagging material.
For increasing the surface property of rigid carbon-fiber lagging material, need to carry out surface treatment to it, its surface treatment method comprises the steps:
1) carbonization/graphited rigid carbon-fiber lagging material is carried out surface grinding and process, make surfacing;
2) direct coating on the surface of the rigid carbon-fiber lagging material after smooth; Directly ratio is formulated by weight by organic binder bond resin, dispersion agent, crystalline graphite powder for the high-temperature material of coating, the portions of resin dispersion agent: the part by weight of crystalline flake graphite is 100: (40～160): (40～100), according to the above ratio resin, dispersion agent and crystalline flake graphite are mixed, namely obtain high temperature coating; Described resin is selected from one or more in resol, Resins, epoxy, the urea-formaldehyde resin; Described dispersion agent is selected from ethanol, propyl alcohol or acetone;
3) temperature rise rate with 1～15 ℃/min is warmed up to 150～350 ℃, constant temperature 1～5.5h under this temperature, and the cured binders layer is made preform;
4) with preform carbonization under inert atmosphere under 1000 ℃～1800 ℃, make pad pasting/coating rigid carbon-fiber lagging material.
Asphaltic base ground carbon fiber of the present invention and organic binder bond, dispersant.The dispersion agent Main Function is to disperse binding agent to increase its flowability; Increase the dispersiveness of carbon fiber, make it reach desirable dispersion effect.Adopt cast, die press technology for forming to make preform, again preform is not melted and high temperature cabonization is processed and namely obtained high-density rigid carbon-fiber heat-insulation material.Its goods form randomness is good, can be made into plate, cylinder, dish or obform body.
According to the present invention, can be made into the high-density insulation product.This product is mixed with organic binder bond by the asphaltic base ground carbon fiber, and the cast compression molding makes through high temperature cabonization again, and density is 0.1～0.5g/cm
3
According to requirements rigid heat insulating material is carried out surface treatment, comprise and paste skim flexible graphite paper, Graphite cloth, carbon cloth, graphite thin plate or carry out the top coat hardening treatment, prevent that furnace gas from directly directly contacting with rigid heat insulating material, anti-airflow scouring, and have certain antioxidant property, further improve its work-ing life.
Advantage of the present invention is to make high-density, lower thermal conductivity and high-intensity rigid heat insulating material; Can be by the ratio of change binding agent, ground carbon fiber length, the techniques such as forming pressure are adjusted the density of lagging material; Technique is simple, and stability is high, and is easy to operate.
Embodiment
1. the feed composition, the proportioning that prepare high-density rigid carbon-fiber heat-insulation material.
(1) carbon fiber: comprise asphalt base carbon fiber, polyacrylonitrile (PAN) base carbon fibre, viscose-based carbon fiber etc.Carry out carbon fiber chopped or grind, require carbon fiber diameter 5-21 μ m, length 0.2-30mm, length-to-diameter ratio is greater than 20; The carbon fiber that adds 20～80% weight percents can be given full play to the thermal and insulating performance of carbon fiber.
(2) organic binder bond: be selected from pitch fibers or powdered asphalt, tar, thermosetting resin resol, urea-formaldehyde resin, Resins, epoxy, furane resin, vinyl ester resin, red shortness's resin polyethylene, polypropylene, ethylene propylene copolymer, polymeric amide, polystyrene, the acrylic resin one or more.The organic binder bond that adds 20～80% weight percents.For reducing the viscosity of organic binder bond, increase the dispersiveness of fiber, can add an amount of dispersion agent it is diluted, the part by weight of organic binder bond and dispersion agent is 1: (0.4～1).Dispersion agent is selected from one or more of the organic thinners such as methyl alcohol, ethanol, butanols, acetone, diacetone alcohol, pimelinketone, methylethylketone, vinyl acetic monomer, N-BUTYL ACETATE.
(3) releasing agent: Graphite Powder 99.
2. do not melt with carbonization (greying) and process: with the ratio batching of material in (1) and (2) in advance design, mix, be coated with equably one deck Graphite Powder 99 as releasing agent at mould inner surface, then cast, compression molding, the demoulding.
(1) with the heating rate of 5～65 ℃/h above-mentioned rigid heat insulating material preform is heated to 180～350 ℃ and carries out not melt processed;
(2) will be not preform carbonization under vacuum or inert atmosphere after the melt processed, temperature is 1000～1800 ℃; Or graphitization processing, graphitization temperature is 1800～2500 ℃, produces rigid carbon-fiber heat-insulation material.
For increasing the surface property of rigid carbon-fiber lagging material, need to carry out surface treatment to the rigid carbon-fiber heat-insulation material after above-mentioned carbonization/greying, rigid carbon-fiber heat-insulation material surface after carbonization/greying is pasted skim flexible graphite paper, Graphite cloth, carbon cloth, graphite thin plate or is carried out the top coat hardening treatment, can prevent that furnace gas from directly directly contacting with rigid heat insulating material, anti-airflow scouring, and have certain antioxidant property, further improve its work-ing life.
Surface treatment method comprises the steps:
1) carbonization/graphited rigid carbon-fiber lagging material is carried out surface grinding and process, make surfacing;
2) the rigid carbon-fiber lagging material brushing binding agent after smooth forms adhesive layer, pastes graphite paper, Graphite cloth, carbon cloth at adhesive layer; Ratio is formulated by weight by resin and norbide for described binding agent, and the part by weight of resin and norbide is 100: (40～160), according to the above ratio resin and norbide are mixed, namely obtain high-temperature agglomerant; Described resin is selected from one or more in resol, Resins, epoxy or the urea aldehyde;
4) temperature rise rate with 1～15 ℃/min is warmed up to 150～350 ℃, constant temperature 1～5.5h under this temperature, and the cured binders layer is made preform;
4) with preform carbonization under inert atmosphere under 1000 ℃～1800 ℃, make pad pasting/coating rigid carbon-fiber lagging material.
Surface treatment method also can be following steps:
1) carbonization/graphited rigid carbon-fiber lagging material is carried out surface grinding and process, make surfacing;
2) direct coating on the surface of the rigid carbon-fiber lagging material after smooth; Directly ratio is formulated by weight by organic binder bond resin, dispersion agent, crystalline graphite powder for the high-temperature material of coating, the portions of resin dispersion agent: the part by weight of crystalline flake graphite is 100: (40～160): (40～100), according to the above ratio resin, dispersion agent and crystalline flake graphite are mixed, namely obtain high temperature coating; Described resin is selected from one or more in resol, Resins, epoxy, the urea-formaldehyde resin; Described dispersion agent is selected from ethanol, propyl alcohol or acetone;
3) temperature rise rate with 1～15 ℃/min is warmed up to 150～350 ℃, constant temperature 1～5.5h under this temperature, and the cured binders layer is made preform;
4) with preform carbonization under inert atmosphere under 1000 ℃～1800 ℃, make pad pasting/coating rigid carbon-fiber lagging material.
The below exemplifies two specific exampless, but not as to concrete restriction of the present invention.
Embodiment 1
Adopt isotropic pitch base carbon fibre P-800, numerical value represents staple length, the unit micron, and P represents grated product.50 parts of ground carbon fibers and 50 parts of resol (add 40 parts of alcohol dilution resol and reduce its viscosity) are through stirring abundant mixing.Mixture is added in the forming mould, apply the certain pressure moulding, the demoulding is heated to 200 ℃ with the heating rate of 15 ℃/h with preform, carries out not melt processed.Temperature rise rate with 100 ℃/h is heated to 1000 ℃, carries out carbonizing treatment and obtains rigid heat insulating material.The density of carbon fiber thermal insulating material is 0.19g/cm
3
Embodiment 2
Adopt isotropic pitch base carbon fibre P-800, numerical value represents staple length, the unit micron, and P represents grated product.50 parts of ground carbon fibers and 50 parts of resol (add 40 parts of alcohol dilution resol and reduce its viscosity) are through stirring abundant mixing.Mixture is added in the forming mould, apply the certain pressure moulding, the demoulding is heated to 200 ℃ with the heating rate of 15 ℃/h with preform, carries out not melt processed.Temperature rise rate with 100 ℃/h is heated to 1000 ℃, carries out carbonizing treatment and obtains rigid heat insulating material.The density of carbon fiber thermal insulating material is 0.19g/cm
3The rigid heat insulating material of carbonization is carried out surface grinding process, make surfacing.
High temperature coating each component part by weight is resol: ethanol: Graphite Powder 99=100: 60: 60, according to the above ratio resol, ethanol and Graphite Powder 99 are mixed, and can obtain high temperature coating.Must be coated in the rigid heat insulating material surface with hairbrush or spray gun with high temperature coating is even, be raised to 200 ℃ with the temperature rise rate of 2 ℃/h, under this temperature, solidify 2h, solidify high temperature coating.Preform in the lower carbonization of rare gas element (nitrogen, argon gas etc.), 1000 ℃ of lower carbonizations, is produced top coat rigid carbon-fiber lagging material with 150 ℃/h temperature rise rate.This kind lagging material can prevent that furnace gas from directly directly contacting with rigid heat insulating material, anti-airflow scouring, and have certain antioxidant property, further improve its work-ing life.
Claims (3)
1. the manufacture method of a rigid carbon-fiber heat-insulation material is characterized in that the method comprises the steps:
1) ground carbon fiber, obtaining mean length is grinding of 0.2-30mm or chopped carbon fiber;
2) will grind or chopped carbon fiber and binding agent, dispersion agent fully mix, grind or chopped carbon fiber, weight of binder part ratio are: grind or chopped carbon fiber 20～80 weight parts, binding agent 80～20 weight parts, the part by weight of binding agent and dispersion agent is 1:(0.4～1);
3) said mixture is poured into a mould, compression molding, make the rigid heat insulating material prefabrication of regulation shape;
4) with the heating rate of 5～65 ℃/h above-mentioned rigid heat insulating material preform is heated to 180～350 ℃ and carries out not melt processed;
5) will be not preform carbonization under vacuum or inert atmosphere after the melt processed, temperature is 1000～1800 ℃; Or graphitization processing, graphitization temperature is 1800～2500 ℃, produces the rigid carbon-fiber lagging material;
Described carbon fiber is selected from a kind of in asphalt base carbon fiber, PAN base carbon fibre, the viscose-based carbon fiber;
Described binding agent is selected from one or more in pitch fibers or powdered asphalt, tar, thermosetting resin resol, urea-formaldehyde resin, Resins, epoxy, furane resin, vinyl ester resin, red shortness's resin polyethylene, polypropylene, ethylene propylene copolymer, polymeric amide, polystyrene, the acrylic resin;
Described dispersion agent is selected one or more of methyl alcohol, ethanol, butanols, acetone, diacetone alcohol, pimelinketone, methylethylketone, vinyl acetic monomer, N-BUTYL ACETATE organic thinner.
2. the manufacture method of rigid carbon-fiber heat-insulation material according to claim 1 is characterized in that need to carrying out surface treatment to it for increasing the surface property of rigid carbon-fiber lagging material, and its surface treatment method comprises the steps:
1) carbonization/graphited rigid carbon-fiber lagging material is carried out surface grinding and process, make surfacing;
2) the rigid carbon-fiber lagging material brushing binding agent after smooth forms adhesive layer, pastes graphite paper or Graphite cloth or carbon cloth at adhesive layer; Ratio is formulated by weight by resin and norbide for described binding agent, and the part by weight of resin and norbide is 100:(40～160), according to the above ratio resin and norbide are mixed, namely obtain high-temperature agglomerant; Described resin is selected from one or more in resol, Resins, epoxy or the urea aldehyde;
3) temperature rise rate with 1～15 ℃/min is warmed up to 150～350 ℃, constant temperature 1～5.5h under this temperature, and the cured binders layer is made preform;
4) with preform carbonization under inert atmosphere under 1000 ℃～1800 ℃, make lagging material.
3. the manufacture method of rigid carbon-fiber heat-insulation material according to claim 1 is characterized in that need to carrying out surface treatment to it for increasing the surface property of rigid carbon-fiber lagging material, and its surface treatment method comprises the steps:
1) carbonization/graphited rigid carbon-fiber lagging material is carried out surface grinding and process, make surfacing;
2) direct coating on the surface of the rigid carbon-fiber lagging material after smooth; Directly ratio is formulated by weight by organic binder bond resin, dispersion agent, crystalline graphite powder for the high-temperature material of coating, resin: dispersion agent: the part by weight of crystalline graphite powder is 100:(40～160): (40～100), according to the above ratio resin, dispersion agent and crystalline graphite powder are mixed, namely obtain high temperature coating; Described resin is selected from one or more in resol, Resins, epoxy, the urea-formaldehyde resin; Described dispersion agent is selected from ethanol, propyl alcohol or acetone;
3) temperature rise rate with 1～15 ℃/min is warmed up to 150～350 ℃, constant temperature 1～5.5h under this temperature, and the cured binders layer is made preform;
4) with preform carbonization under inert atmosphere under 1000 ℃～1800 ℃, make lagging material.
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