CN106747552A - A kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance - Google Patents

A kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance Download PDF

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CN106747552A
CN106747552A CN201710102921.2A CN201710102921A CN106747552A CN 106747552 A CN106747552 A CN 106747552A CN 201710102921 A CN201710102921 A CN 201710102921A CN 106747552 A CN106747552 A CN 106747552A
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carbon fiber
thermal insulation
insulation cylinder
compound
fiber thermal
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CN106747552B (en
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王红伟
郑淑云
陈惠龙
朴成军
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Liaoning Aoyida New Materials Co ltd
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LIAONING AOYIDA ADVANCED MATERIAL Co Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/526—Fibers characterised by the length of the fibers
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5272—Fibers of the same material with different length or diameter
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The present invention relates to a kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance, after the mixed carbon fibre that chopped carbon fiber and ground carbon fiber are constituted is mixed with organic binder bond, solvent, remove solvent therein, the compound carbon fiber of Surface coating organic binder bond and water, dispersant are formed into carbon fiber mixed slurry, compound Carbon fiber thermal insulation cylinder prefabrication is made through being sucked by vacuum shaping；It is dehydrated it by the way of vapours or hot air and completes non-fusible, insoluble treatment；Then through carbonization or graphitization processing, compound Carbon fiber thermal insulation cylinder finished product is obtained.Compound Carbon fiber thermal insulation cylinder made by the present invention has good heat-proof quality, good in oxidation resistance, the characteristic that thermal capacity is low, intensity is high, and manufacture craft is simple, and low cost, finished form and size are controllable, and density is adjustable；Finished product is not easy to crack, and self-supporting is good, long service life；Can also have excellent antioxygenic property after surface treated, and further improve service life.

Description

A kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance
Technical field
Protected the present invention relates to high temperature furnace used heat-preservation cylinder manufacture technology field, more particularly to a kind of high performance compound carbon fiber The manufacture method of warm cylinder.
Background technology
With the progress of science and technology, the field such as military affairs, national defence, solar energy, semiconductor, heat treatment all in fast development, The development in these fields is directed to the use of insulation material；Especially solar energy, semiconductor are developed rapidly in recent years, to thermal insulating material The demand of material seems more prominent, and the requirement more and more higher to insulation material, does not require nothing more than energy-saving, and requires anti- Oxidation susceptibility is high, and these requirements also constantly promote the fast development of field of heat insulating materials.
The carbon fiber thermal insulating material for once being commonly used on vacuum high temperature furnace at home is soft carbon felt (Nomex), soft carbon felt There is low intensity, yielding, easy efflorescence, effect of heat insulation difference and dismounting, installation when being used as heat-insulating heat-preserving material wastes time and energy The shortcomings of.The hard felt heat-insulating heat-preserving material of carbon fiber newly developed can overcome the disadvantages mentioned above of soft carbon felt, thus as crystal oven, The high temperature furnace used heat-insulating heat-preserving material such as ceramic sintering furnace, gaseous phase deposition stove is increasingly used.
At present, the domestic hard felt of carbon fiber for using is mainly using the moulding process of PAN base soft carbons felt dipping molding.Dipping former Pressure technique makes the hard felt of carbon fiber and there is low intensity between high energy consumption, carbon fiber hard carpet veneer, easy to crack, and the life-span is low, binder content The shortcomings of height, antioxygenic property difference.
The content of the invention
The invention provides a kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance, made compound carbon fiber is protected Warm cylinder has good heat-proof quality, good in oxidation resistance, the characteristic that thermal capacity is low, intensity is high, and manufacture craft is simple, low cost, into Product shape and size are controllable, and density is adjustable；Finished product is not easy to crack, and self-supporting is good, long service life；May be used also after surface treated With excellent antioxygenic property, and further improve service life.
In order to achieve the above object, the present invention is realized using following technical scheme：
A kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance, comprises the following steps：
1) chopped carbon fiber is prepared；Carbon fiber is chopped, the chopped carbon fiber that average length is 1~80mm is obtained；
2) ground carbon fiber is prepared；Carbon fiber is ground, the ground carbon fiber that average length is 100~800 μm is obtained；
3) by chopped carbon fiber and ground carbon fiber according to 10~90 ﹕ 90~10 weight ratio, using cyclonic separation Device is sufficiently mixed uniformly, obtains mixed carbon fibre；
4) mixed carbon fibre is mixed with organic binder bond, solvent by the weight ratio of the ﹕ 3~920 of 100 ﹕ 20~230, Obtain carbon fiber mixed liquor；Carbon fiber mixed liquor is put into mesh bag, through the mesh bag initial filter that mesh aperture is 1~50 μm after, then Using 50~60 DEG C of hot-airs to 10~30min of blow-through in mesh bag, the solvent in carbon fiber mixed liquor is volatilized completely, obtain The compound carbon fiber of Surface coating organic binder bond；
5) by the compound carbon fiber of Surface coating organic binder bond and water, dispersant according to the ﹕' 0.1~2 of 0.3~6 ﹕ 100 Weight ratio is sufficiently mixed, and forms uniform carbon fiber mixed slurry；
6) carbon fiber mixed slurry is molded using vacuum suction；By the heat-preservation cylinder mould immersion used by vacuum suction In shaping pond, heat-preservation cylinder mould is made up of the inner mold that is set in together, outer mold, and inside and outside mould is cylindrical shape knot Structure；Wherein inner mold is made up of sieve plate, and its outer surface is fixed with screen cloth, and the aperture of screen cloth is 30~200 μm, and outer mold is grid Shape structure, the unilateral or radial dimension of grid hole is 30~100mm；
The heat-preservation cylinder mould is placed in shaping pond with axis in vertical state, and its upper end is provided with suspender for soaking It is adjusted when entering to be molded pond highly；
Vacuum forming chamber is formed between the inner mold, outer mold and upper and lower end plate, and vacuum forming chamber has and is combined The shape and size that Carbon fiber thermal insulation cylinder is engaged；Suction tube is along the elongated setting of inner mold longitudinal center；In the effect of suction tube Under, carbon fiber mixed slurry is molded between inside and outside mould by aligned transfer, is made compound Carbon fiber thermal insulation cylinder prefabrication；
7) compound Carbon fiber thermal insulation cylinder prefabrication is taken out together with heat-preservation cylinder mould from shaping pond, is used 100~240 DEG C of vapours or hot air 2~5 hours, make compound Carbon fiber thermal insulation cylinder prefabrication be dehydrated and complete not melt Change, insoluble treatment；
8) through the compound Carbon fiber thermal insulation cylinder prefabrication demoulding after dehydration and non-fusible, insoluble treatment, it is then placed in true It is carbonized in empty stove or under an inert atmosphere, carburizing temperature is 800~1800 DEG C；Carried out at graphitization also dependent on use requirement Reason, graphitization temperature is 1800~2500 DEG C；High performance compound Carbon fiber thermal insulation is obtained after carbonization or graphitization processing Cylinder；
9) density of the compound Carbon fiber thermal insulation cylinder obtained by is 0.1~0.35g/cm3, thermal conductivity factor is less than 0.35W/ m·K；
10) selectively compound Carbon fiber thermal insulation cylinder is surface-treated as needed；To increase its anti-airflow scouring And antioxygenic property, improve its service life；What is be surface-treated concretely comprises the following steps：
A. it is machined to compound Carbon fiber thermal insulation cylinder to carry out surface grinding；
B. in the inside/outside or inner and outer surfaces brushing adhesive layer of compound Carbon fiber thermal insulation cylinder, can further exist as needed Adhesive layer external pasting overcoat, overcoat is flexible graphite paper/carbon cloth, carbon cloth or graphitic sheet, it is also possible to do not pasted Overcoat；
C. to being processed through b step after compound Carbon fiber thermal insulation cylinder carry out curing process, then be carbonized/graphitization at Reason, obtains surface treated compound Carbon fiber thermal insulation cylinder.
It is described to prepare carbon fiber used when chopped carbon fiber or ground carbon fiber for asphalt base carbon fiber, viscose base carbon are fine Dimension, one or more in PAN base carbon fibres, be preferably chopped asphalt base carbon fiber, by any during from more than one carbon fibers Ratio mixes.
The mesh bag is made up of non-woven fabrics, synthetic cotton, polypropylene, Teflon or polyester material, and the aperture of mesh bag is 1~50 μm, preferably 5~30 μm.
The grid hole of the outer mold is shaped as triangle, circle, square, rectangle, rhombus, regular polygon or does not advise Then one kind in polygon.
The organic binder bond is selected from phenolic resin, epoxy resin, furane resins, Lauxite, vinyl ester resin, poly- In acid amides, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, monose, polysaccharide, pitch, tar One or more arbitrarily mix.
The solvent be selected from methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propane diols, glycerine, ether, furfuryl alcohol, furfural, acetone, One or more any mixing in benzene, toluene, furancarbinol, furtural.
The dispersant is selected from methylcellulose, carboxymethylcellulose calcium, hydroxypropyl methyl cellulose, hydroxyethyl methyl fiber Element, hydroxymethyl cellulose, ethyl cellulose, cellulose ether, methylethylcellulose, Hydroxypropyl ethyl cellulose, hydroxyl second One kind in base ethyl cellulose, hydroxymethyl ethylcellulose, polyvinyl alcohol, Pioloform, polyvinyl acetal, starch, modified starch or one Plant any of the above mixing.
Compared with prior art, the beneficial effects of the invention are as follows：
1) can produce higher density, lower thermal conductivity and high intensity compound Carbon fiber thermal insulation cylinder, and finished product have it is excellent Good cracking resistance；
Chopped carbon fiber of the present invention can not only increase the intensity of compound Carbon fiber thermal insulation cylinder, and can increase Plus its toughness, can shock resistance, so as to make it have excellent cracking resistance；The ground carbon fiber for being used not only may be used To play a part of the compound Carbon fiber thermal insulation cylinder density of appropriate adjustment, the content of carbon fiber in finished product can also be increased；And carbon is fine The content of dimension can not only influence the thermal conductivity factor of compound Carbon fiber thermal insulation cylinder, can also influence its antioxygenic property；Carbon fiber content More arrangements are better, and the thermal conductivity factor for being combined Carbon fiber thermal insulation cylinder is smaller；Carbon fiber content is more, and its inoxidizability is better；
The present invention is taken out by changing organic binder bond, chopped carbon fiber and the mixed proportion of ground carbon fiber, adjustment vacuum The vacuum in moulding process is inhaled, the density of compound Carbon fiber thermal insulation cylinder can be adjusted；Made compound Carbon fiber thermal insulation cylinder Density be 0.1~0.35g/cm3, thermal conductivity factor is less than 0.35W/mK；
2) low production cost of the invention, process is simple, stability is high, easy to operate；
The present invention is dehydrated and non-fusible, insoluble using vapours or hot-air to compound Carbon fiber thermal insulation cylinder prefabrication Change is processed, and can greatly improve production efficiency, reduces production cost, saving energy consumption；It is dehydrated using the method for the invention And non-fusible, insoluble treatment only needs to complete for 2~5 hours, and use conventional baking oven or heating furnace carry out it is non-fusible, Insoluble treatment needs to complete for 80~120 hours, therefore efficiency of the invention improves tens times；And the operation link Energy consumption be also down to below 3 yuan/kilogram from yuan/kilogram of unit consumption 11, energy conservation and consumption reduction effects are obvious；
3) the compound Carbon fiber thermal insulation cylinder made by the present invention has good effect of heat insulation；
In compound Carbon fiber thermal insulation cylinder prefabrication of the present invention, carbon fiber orientation meets two-dimensional arrangements, and with Direction of heat flow is vertical, is heat-insulated optimum orientation；Product is not easy to crack, and self-supporting is good, long service life；Especially making big It is more advantageous in technique during sized products；
4) present invention is coordinated using inside and outside mould, can be with the shape of one-step building product and size, finished product through vacuum suction It is that can obtain scale product only to need slightly processed, and stock utilization can reach more than 90%；And use common die shaping Product size is unable to precise control, and Surface Machining amount is big, and product utilization rate most multipotency reaches 75~80%；Therefore the present invention is significantly The utilization rate of material is improve, the generation of waste material is reduced, so as to considerably reduce production cost；
5) according to requirements, further surface can be done to it on the basis of obtained compound Carbon fiber thermal insulation cylinder Treatment, can prevent high temperature furnace gas and compound Carbon fiber thermal insulation cylinder directly contact, improve the ability of its anti-airflow scouring, make It has excellent antioxygenic property, and further improves the service life of compound Carbon fiber thermal insulation cylinder.
Brief description of the drawings
Fig. 1 is the process diagram of vacuum suction shaping of the present invention.
The structural representation of heat-preservation cylinder mould used when Fig. 2 is vacuum suction shaping of the present invention；
Fig. 3 is the cross-sectional view in Fig. 2.
Fig. 4 is the structural representation (by taking network as an example) of the outer mold of heat-preservation cylinder mould of the present invention.
Fig. 5 is the structural representation after compound Carbon fiber thermal insulation tube inner surface surface treated of the present invention.
Fig. 6 is the structural representation after compound Carbon fiber thermal insulation cylinder inner and outer surfaces surface treated of the present invention.
In figure：1. the internal model of 5. suction tube of shaping pond 2. heat-preservation cylinder mould, 3. vacuum tank, 4. water ring vacuum pump 6. The compound Carbon fiber thermal insulation cylinder outer mold 9. of prefabrication 8. of tool 7. is combined the Carbon fiber thermal insulation cylinder overcoat of 10. bond layer 11. The 12. shaping suspenders of dolly 13.
Specific embodiment
Specific embodiment of the invention is described further below in conjunction with the accompanying drawings：
A kind of manufacture method of the compound Carbon fiber thermal insulation cylinder of high-performance of the present invention, comprises the following steps：
1) chopped carbon fiber is prepared；Carbon fiber is chopped, the chopped carbon fiber that average length is 1~80mm is obtained；
2) ground carbon fiber is prepared；Carbon fiber is ground, the ground carbon fiber that average length is 100~800 μm is obtained；
3) by chopped carbon fiber and ground carbon fiber according to 10~90 ﹕ 90~10 weight ratio, using cyclonic separation Device is sufficiently mixed uniformly, obtains mixed carbon fibre；
4) mixed carbon fibre is mixed with organic binder bond, solvent by the weight ratio of the ﹕ 3~920 of 100 ﹕ 20~230, Obtain carbon fiber mixed liquor；Carbon fiber mixed liquor is put into mesh bag, through the mesh bag initial filter that mesh aperture is 1~50 μm after, then Using 50~60 DEG C of hot-airs to 10~30min of blow-through in mesh bag, the solvent in carbon fiber mixed liquor is volatilized completely, obtain The compound carbon fiber of Surface coating organic binder bond；
5) by the compound carbon fiber of Surface coating organic binder bond and water, dispersant according to the ﹕' 0.1~2 of 0.3~6 ﹕ 100 Weight ratio is sufficiently mixed, and forms uniform carbon fiber mixed slurry；
6) carbon fiber mixed slurry is molded using vacuum suction；As shown in figure 1, by the heat-preservation cylinder used by vacuum suction into In the immersion shaping ponds 1 of pattern tool 2, as shown in Figure 2 and Figure 3, heat-preservation cylinder mould 2 is by the inner mold 6, external mold that is set in together Tool 8 is constituted, and inside and outside mould is columnar structured；Wherein inner mold is made up of sieve plate, and its outer surface is fixed with screen cloth, screen cloth Aperture be 30~200 μm, outer mold is fenestral fabric, and the unilateral or radial dimension of grid hole is 30~100mm；(such as Fig. 4 It is shown)
The heat-preservation cylinder mould is placed in shaping pond with axis in vertical state, and its upper end is provided with suspender 13 to be used for It is adjusted during immersion shaping pond highly；
Vacuum forming chamber is formed between the inner mold, outer mold and upper and lower end plate, and vacuum forming chamber has and is combined The shape and size that Carbon fiber thermal insulation cylinder is engaged；Suction tube 5 is along the elongated setting of the longitudinal center of inner mold 6；In the work of suction tube 5 Under, carbon fiber mixed slurry is molded between inside and outside mould 6,8 by aligned transfer, is made compound Carbon fiber thermal insulation cylinder prefabricated Product 7；
7) compound Carbon fiber thermal insulation cylinder prefabrication 7 is taken out together with heat-preservation cylinder mould 2 from shaping pond 1, is adopted With 100~240 DEG C of vapours or hot air 2~5 hours, compound Carbon fiber thermal insulation cylinder prefabrication 7 is set to be dehydrated and complete Non-fusible, insoluble treatment；
8) through the compound Carbon fiber thermal insulation cylinder demoulding of prefabrication 7 after dehydration and non-fusible, insoluble treatment, it is then placed in true It is carbonized in empty stove or under an inert atmosphere, carburizing temperature is 800~1800 DEG C；Carried out at graphitization also dependent on use requirement Reason, graphitization temperature is 1800~2500 DEG C；High performance compound Carbon fiber thermal insulation is obtained after carbonization or graphitization processing Cylinder 9；
9) density of the compound Carbon fiber thermal insulation cylinder 9 obtained by is 0.1~0.35g/cm3, thermal conductivity factor is less than 0.35W/ m·K；
10) selectively compound Carbon fiber thermal insulation cylinder 9 is surface-treated as needed；To increase its anti-airflow scouring And antioxygenic property, improve its service life；What is be surface-treated concretely comprises the following steps：
A. it is machined to compound Carbon fiber thermal insulation cylinder 9 to carry out surface grinding；
B. as shown in Figure 5, Figure 6, in the inside/outside or inner and outer surfaces brushing adhesive layer 10 of compound Carbon fiber thermal insulation cylinder 9, As needed can further in the external pasting overcoat 11 of adhesive layer 10, overcoat 11 is flexible graphite paper/carbon cloth, carbon cloth Or graphitic sheet, it is also possible to overcoat 11 is not pasted；
C. to being processed through b step after compound Carbon fiber thermal insulation cylinder carry out curing process, then be carbonized/graphitization at Reason, obtains surface treated compound Carbon fiber thermal insulation cylinder.
It is described to prepare carbon fiber used when chopped carbon fiber or ground carbon fiber for asphalt base carbon fiber, viscose base carbon are fine Dimension, one or more in PAN base carbon fibres, be preferably chopped asphalt base carbon fiber, by any during from more than one carbon fibers Ratio mixes.
The mesh bag is made up of non-woven fabrics, synthetic cotton, polypropylene, Teflon or polyester material, and the aperture of mesh bag is 1~50 μm, preferably 5~30 μm.
The grid hole of the outer mold is shaped as triangle, circle, square, rectangle, rhombus, regular polygon or does not advise Then one kind in polygon.
The organic binder bond is selected from phenolic resin, epoxy resin, furane resins, Lauxite, vinyl ester resin, poly- In acid amides, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, monose, polysaccharide, pitch, tar One or more arbitrarily mix.
The solvent be selected from methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propane diols, glycerine, ether, furfuryl alcohol, furfural, acetone, One or more any mixing in benzene, toluene, furancarbinol, furtural.
The dispersant is selected from methylcellulose, carboxymethylcellulose calcium, hydroxypropyl methyl cellulose, hydroxyethyl methyl fiber Element, hydroxymethyl cellulose, ethyl cellulose, cellulose ether, methylethylcellulose, Hydroxypropyl ethyl cellulose, hydroxyl second One kind in base ethyl cellulose, hydroxymethyl ethylcellulose, polyvinyl alcohol, Pioloform, polyvinyl acetal, starch, modified starch or one Plant any of the above mixing.
Following examples are implemented under premised on technical solution of the present invention, give detailed implementation method and tool The operating process of body, but protection scope of the present invention is not limited to following embodiments.Method therefor and material in following embodiments Conventional method and material are unless otherwise instructed.
【Embodiment 1】
In the present embodiment, the manufacture method of high performance compound Carbon fiber thermal insulation cylinder is as follows：
1) chopped carbon fiber is prepared；Asphalt base carbon fiber is chopped, the chopped carbon fiber that average length is 40mm is obtained；
2) ground carbon fiber is prepared；Asphalt base carbon fiber is ground, the ground carbon fiber that average length is 100 μm is obtained；
3) by chopped carbon fiber and ground carbon fiber according to 60：40 weight ratio, is fully mixed using cyclone separator Close uniform, obtain mixed carbon fibre；
4) mixed carbon fibre and organic binder bond phenolic resin, etoh solvent are pressed 100：30：70 weight ratio is mixed Close, obtain carbon fiber mixed liquor；Carbon fiber mixed liquor is put into mesh bag, through the mesh bag initial filter that mesh aperture is 30 μm after, then Using 50 DEG C of hot-airs to blow-through 30min in mesh bag, the solvent in carbon fiber mixed liquor is volatilized completely, obtain Surface coating The compound carbon fiber of organic binder bond；
5) by the compound carbon fiber of Surface coating organic binder bond and water, methylcellulose according to the ﹕ 1 of 3 ﹕ 100 weight portion Ratio is sufficiently mixed, and forms uniform carbon fiber mixed slurry；
6) carbon fiber mixed slurry is molded using vacuum suction；Heat-preservation cylinder mould 2 used by vacuum suction is soaked Enter to be molded in pond 1, shaping pond 1 is arranged on shaping dolly 12, facilitates finishing type to finish the transport of rear material；Heat-preservation cylinder shaping mould Tool 2 is made up of the inner mold 6 that is set in together, outer mold 8, and inner mold 6 is made up of sieve plate, and its outer surface is fixed with screen cloth, sieve The aperture of net is 50 μm, and outer mold 8 is fenestral fabric, and the unilateral or radial dimension of grid hole is 60mm；
The heat-preservation cylinder mould 2 is placed in shaping pond 1 with axis in vertical state, and its upper end is provided with suspender 13 and uses It is adjusted when immersion shaping pond 1 highly.
The inner mold 6 and outer mold 8 are columnar structured, and are coaxially disposed, the two ends difference of inside and outside mould 6,8 Fit together with upper and lower end plate, the annular space for being formed i.e. vacuum forming chamber, the unilateral section of vacuum forming chamber radial direction is Rectangle；Vacuum forming chamber has the shape and size being engaged with compound Carbon fiber thermal insulation cylinder；Suction tube 5 is along the longitudinal direction of inner mold 6 The elongated setting in center；SS is densely covered with suction tube 5, suction tube 5 connects vacuum tank 3 by connecting flexible pipe, and vacuum tank 3 connects again Water receiving ring vacuum pump 4 forms vacuum suction apparatus；After opening vacuum suction apparatus, in the presence of suction tube 5, carbon fiber mixing Slurry is molded in vacuum forming room by aligned transfer, is made compound Carbon fiber thermal insulation cylinder prefabrication 7；
7) compound Carbon fiber thermal insulation cylinder prefabrication 7 is taken out together with heat-preservation cylinder mould 2 from shaping pond 1, is adopted With 150 DEG C of vapours or hot air 3 hours, it is dehydrated compound Carbon fiber thermal insulation cylinder prefabrication 7 and completes non-fusible, no Dissolve treatment；
8) through the compound Carbon fiber thermal insulation cylinder demoulding of prefabrication 7 after dehydration and non-fusible, insoluble treatment, it is then placed in true It is carbonized in empty stove or under an inert atmosphere, carburizing temperature is 1200 DEG C；Then graphitization processing is carried out, graphitization temperature is 2100 ℃；High performance compound Carbon fiber thermal insulation cylinder 9 is obtained after carbonization or graphitization processing；
9) density of the compound Carbon fiber thermal insulation cylinder 9 obtained by is 0.16g/cm3, thermal conductivity factor 0.22W/mK；Carbon contains Amount 99.6%, ash content 0.01%；(sample thickness is 45mm, under nitrogen protection, detection data at 1500 DEG C).
【Embodiment 2】
To increase the anti-airflow scouring and antioxygenic property of compound Carbon fiber thermal insulation cylinder 9, its service life is further improved； It is right【Embodiment 1】Obtained compound Carbon fiber thermal insulation cylinder 9 is surface-treated, and surface treatment is comprised the following steps that：
1) by compound Carbon fiber thermal insulation cylinder 9 it is machined carry out surface grinding treatment, make surfacing；
2) compound Carbon fiber thermal insulation 9 inner and outer surfaces of cylinder after surface is processed through polishing brush 3~6 times binding agents respectively, Adhesive layer 10 is formed, binding agent uses conventional use of bonding agent；
3) the compound Carbon fiber thermal insulation cylinder 9 of brushing adhesive layer 10 is put into heating furnace, with the heating rate of 5 DEG C/min 240 DEG C are warmed up to, at this temperature constant temperature 1h, solidify adhesive layer 10；Then it is placed in again at 1700 DEG C, enters under an inert atmosphere Row carbonization treatment, is made the compound Carbon fiber thermal insulation cylinder of band coating.
The compound Carbon fiber thermal insulation cylinder of the band coating obtained by the present embodiment is used 100 times on monocrystalline silicon stretching furnace, is not had The phenomenons such as coating stripping, cracking, foaming are occurred, the compound Carbon fiber thermal insulation corrosion-free phenomenon of cylinder inside coating.
【Embodiment 3】
In the present embodiment, the manufacture method of high performance compound Carbon fiber thermal insulation cylinder is as follows：
1) chopped carbon fiber is prepared；Asphalt base carbon fiber is chopped, the chopped carbon fiber that average length is 80mm is obtained；
2) ground carbon fiber is prepared；Asphalt base carbon fiber is ground, the ground carbon fiber that average length is 180 μm is obtained；
3) by chopped carbon fiber and ground carbon fiber according to 50：50 weight ratio, is fully mixed using cyclone separator Close uniform, obtain mixed carbon fibre；
4) mixed carbon fibre and organic binder bond phenolic resin, etoh solvent are pressed 100：55：75 weight ratio is mixed Close, obtain carbon fiber mixed liquor；Carbon fiber mixed liquor is put into mesh bag, through the mesh bag initial filter that mesh aperture is 30 μm after, then Using 60 DEG C of hot-airs to blow-through 30min in mesh bag, the solvent in carbon fiber mixed liquor is volatilized completely, obtain Surface coating The compound carbon fiber of organic binder bond；
5) by the compound carbon fiber of Surface coating organic binder bond and water, methylcellulose according to the ﹕ 1 of 6 ﹕ 100 weight portion Ratio is sufficiently mixed, and forms uniform carbon fiber mixed slurry；
6) carbon fiber mixed slurry is molded using vacuum suction；Heat-preservation cylinder mould 2 used by vacuum suction is soaked In entering to be molded pond 1；Heat-preservation cylinder mould 2 is made up of the inner mold 6 that is set in together, outer mold 8, and inner mold 6 is by sieve plate system Into its outer surface is fixed with screen cloth, and the aperture of screen cloth is 70 μm, and outer mold 8 is fenestral fabric, the unilateral or radial direction of grid hole Size is 10mm；
In the presence of suction tube 5, carbon fiber mixed slurry is molded in vacuum forming room by aligned transfer, is made compound Carbon fiber thermal insulation cylinder prefabrication 7；
7) compound Carbon fiber thermal insulation cylinder prefabrication 7 is taken out together with heat-preservation cylinder mould 2 from shaping pond 1, is adopted With 180 DEG C of vapours or hot air 2.5 hours, make compound Carbon fiber thermal insulation cylinder prefabrication 7 be dehydrated and complete it is non-fusible, Insoluble treatment；
8) through the compound Carbon fiber thermal insulation cylinder demoulding of prefabrication 7 after dehydration and non-fusible, insoluble treatment, it is then placed in true It is carbonized in empty stove or under an inert atmosphere, carburizing temperature is 1500 DEG C；Then graphitization processing is carried out, graphitization temperature is 2000 ℃；High performance compound Carbon fiber thermal insulation cylinder 9 is obtained after carbonization or graphitization processing；
9) density of the compound Carbon fiber thermal insulation cylinder 9 obtained by is 0.19g/cm3, thermal conductivity factor 0.20W/mK；Carbon contains Amount 99.7%, ash content 0.01%；(sample thickness is 45mm, under nitrogen protection, detection data at 1500 DEG C).
To increase the anti-airflow scouring and antioxygenic property of compound Carbon fiber thermal insulation cylinder 9, its service life is further improved； Obtained compound Carbon fiber thermal insulation cylinder 9 is further surface-treated, surface treatment is comprised the following steps that：
1) by compound Carbon fiber thermal insulation cylinder 9 it is machined carry out surface grinding treatment, make surfacing；
2) compound Carbon fiber thermal insulation 9 inner and outer surfaces of cylinder after surface is processed through polishing brush 3~6 times binding agents respectively, Adhesive layer 10 is formed, binding agent uses conventional use of bonding agent；In the external pasting overcoat 11 of adhesive layer 10, protection Layer 11 is flexible graphite paper；
3) by brushing adhesive layer 10 and paste the compound Carbon fiber thermal insulation cylinder of overcoat 11 and 9 be put into heating furnace, with 8 DEG C/heating rate of min is warmed up to 300 DEG C, constant temperature 1h, solidifies adhesive layer 10 at this temperature；Then 1800 DEG C are placed in again Under, carbonization treatment is carried out under an inert atmosphere, it is made the compound Carbon fiber thermal insulation cylinder with overcoat.
The cylinder of the compound Carbon fiber thermal insulation with overcoat obtained by the present embodiment is used 100 times on monocrystalline silicon stretching furnace, There are not the phenomenons such as overcoat stripping, cracking, foaming, the compound Carbon fiber thermal insulation corrosion-free phenomenon of cylinder inside overcoat.
Be may certify that through above example, band coating or the cylinder of the compound Carbon fiber thermal insulation with overcoat can prevent miscellaneous in stove Matter gas is directly contacted with compound Carbon fiber thermal insulation cylinder surface, prevents it from corroding and anti-airflow scouring, is made with excellent antioxygen Change and corrosion resistance, the service life of compound Carbon fiber thermal insulation cylinder can be significantly improved.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.

Claims (8)

1. a kind of high-performance is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that comprise the following steps：
1) chopped carbon fiber is prepared；Carbon fiber is chopped, the chopped carbon fiber that average length is 1~80mm is obtained；
2) ground carbon fiber is prepared；Carbon fiber is ground, the ground carbon fiber that average length is 100~800 μm is obtained；
3) chopped carbon fiber and ground carbon fiber are filled according to the weight ratio of 10~90 ﹕ 90~10 using cyclone separator Divide well mixed, obtain mixed carbon fibre；
4) mixed carbon fibre is mixed with organic binder bond, solvent by the weight ratio of the ﹕ 3~920 of 100 ﹕ 20~230, is obtained Carbon fiber mixed liquor；Carbon fiber mixed liquor is put into mesh bag, through the mesh bag initial filter that mesh aperture is 1~50 μm after, then use 50~60 DEG C of hot-air makes the solvent in carbon fiber mixed liquor volatilize completely to 10~30min of blow-through in mesh bag, obtains surface Coat the compound carbon fiber of organic binder bond；
5) by the compound carbon fiber of Surface coating organic binder bond and water, dispersant according to the ﹕ 0.1~2 of 0.3~6 ﹕ 100 weight Part ratio is sufficiently mixed, and forms uniform carbon fiber mixed slurry；
6) carbon fiber mixed slurry is molded using vacuum suction；Heat-preservation cylinder mould used by vacuum suction is immersed into shaping Chi Zhong, heat-preservation cylinder mould is made up of the inner mold that is set in together, outer mold, and inside and outside mould is columnar structured；Its Middle inner mold is made up of sieve plate, and its outer surface is fixed with screen cloth, and the aperture of screen cloth is 30~200 μm, and outer mold is latticed knot Structure, the unilateral or radial dimension of grid hole is 30~100mm；
The heat-preservation cylinder mould is placed in shaping pond with axis in vertical state, and its upper end is provided with suspender for immersing into It is adjusted during type pond highly；
Vacuum forming chamber is formed between the inner mold, outer mold and upper and lower end plate, and vacuum forming chamber has and composite carbon fibre The shape and size that dimension heat-preservation cylinder is engaged；Suction tube is along the elongated setting of inner mold longitudinal center；In the presence of suction tube, carbon Fiber-incorporated slurry is molded between inside and outside mould by aligned transfer, is made compound Carbon fiber thermal insulation cylinder prefabrication；
7) compound Carbon fiber thermal insulation cylinder prefabrication is taken out together with heat-preservation cylinder mould from shaping pond, using 100~ 240 DEG C of vapours or hot air 2~5 hours, are dehydrated compound Carbon fiber thermal insulation cylinder prefabrication and complete non-fusible, no Dissolve treatment；
8) through the compound Carbon fiber thermal insulation cylinder prefabrication demoulding after dehydration and non-fusible, insoluble treatment, it is then placed in vacuum drying oven In or be carbonized under an inert atmosphere, carburizing temperature be 800~1800 DEG C；Graphitization processing, stone are carried out also dependent on use requirement Inkization temperature is 1800~2500 DEG C；High performance compound Carbon fiber thermal insulation cylinder is obtained after carbonization or graphitization processing；
9) density of the compound Carbon fiber thermal insulation cylinder obtained by is 0.1~0.35g/cm3, thermal conductivity factor is less than 0.35W/mK；
10) selectively compound Carbon fiber thermal insulation cylinder is surface-treated as needed；To increase its anti-airflow scouring and resist Oxidation susceptibility, improves its service life；What is be surface-treated concretely comprises the following steps：
A. it is machined to compound Carbon fiber thermal insulation cylinder to carry out surface grinding；
B. in the inside/outside or inner and outer surfaces brushing adhesive layer of compound Carbon fiber thermal insulation cylinder, can further bond as needed Oxidant layer external pasting overcoat, overcoat is flexible graphite paper/carbon cloth, carbon cloth or graphitic sheet, it is also possible to do not paste protection Layer；
C. to being processed through b step after compound Carbon fiber thermal insulation cylinder carry out curing process, then carry out the/graphitization processing that is carbonized, obtain To surface treated compound Carbon fiber thermal insulation cylinder.
2. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that pass through Change the mixed proportion of organic binder bond, chopped carbon fiber and ground carbon fiber, and vacuum during vacuum suction shaping, can Density to being combined Carbon fiber thermal insulation cylinder is accurately adjusted, to meet the use requirement under different condition.
3. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that described Carbon fiber used when chopped carbon fiber or ground carbon fiber is prepared for asphalt base carbon fiber, viscose base carbon fibre, PAN bases carbon are fine One or more in dimension, be preferably chopped asphalt base carbon fiber, mixes in any proportion during from more than one carbon fibers.
4. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that described Mesh bag is made up of non-woven fabrics, synthetic cotton, polypropylene, Teflon or polyester material, and the aperture of mesh bag is 1~50 μm, preferably 5~30 μm。
5. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that described The grid hole of outer mold is shaped as in triangle, circle, square, rectangle, rhombus, regular polygon or irregular polygon It is a kind of.
6. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that described Organic binder bond is selected from phenolic resin, epoxy resin, furane resins, Lauxite, vinyl ester resin, polyamide, acrylic acid One kind or one kind in resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, monose, polysaccharide, pitch, tar Any of the above mixes.
7. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that described Solvent is selected from methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propane diols, glycerine, ether, furfuryl alcohol, furfural, acetone, benzene, toluene, furans One or more any mixing in methyl alcohol, furtural.
8. a kind of high-performance according to claim 1 is combined the manufacture method of Carbon fiber thermal insulation cylinder, it is characterised in that described It is fine that dispersant is selected from methylcellulose, carboxymethylcellulose calcium, hydroxypropyl methyl cellulose, HEMC, methylol Dimension element, ethyl cellulose, cellulose ether, methylethylcellulose, Hydroxypropyl ethyl cellulose, Hydroxyethylethyl fiber One or more in element, hydroxymethyl ethylcellulose, polyvinyl alcohol, Pioloform, polyvinyl acetal, starch, modified starch are any Mixing.
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CN108144584A (en) * 2018-01-03 2018-06-12 岐北通用净水技术（厦门）有限公司 A kind of Carbon fibe stick moulding technique and its device
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CN116084006A (en) * 2022-07-18 2023-05-09 浙江星辉新材料科技有限公司 Method for preparing spliced thermal insulation cylinder by using carbon-carbon composite material
CN116621595A (en) * 2023-07-21 2023-08-22 浙江德鸿碳纤维复合材料有限公司 Carbon fiber reinforced graphite ring and preparation method thereof
CN116655397A (en) * 2023-07-28 2023-08-29 浙江德鸿碳纤维复合材料有限公司 Carbon/carbon composite material based on short carbon fibers and preparation method thereof

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CN108129159A (en) * 2017-12-29 2018-06-08 湖南省鑫源新材料股份有限公司 A kind of Carbon fiber thermal insulation cylinder and preparation method thereof
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CN116621595B (en) * 2023-07-21 2023-10-27 浙江德鸿碳纤维复合材料有限公司 Carbon fiber reinforced graphite ring and preparation method thereof
CN116655397A (en) * 2023-07-28 2023-08-29 浙江德鸿碳纤维复合材料有限公司 Carbon/carbon composite material based on short carbon fibers and preparation method thereof
CN116655397B (en) * 2023-07-28 2023-10-27 浙江德鸿碳纤维复合材料有限公司 Carbon/carbon composite material based on short carbon fibers and preparation method thereof

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