CN106904986B - Manufacturing method of high-performance composite carbon fiber insulation board - Google Patents

Manufacturing method of high-performance composite carbon fiber insulation board Download PDF

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CN106904986B
CN106904986B CN201710098358.6A CN201710098358A CN106904986B CN 106904986 B CN106904986 B CN 106904986B CN 201710098358 A CN201710098358 A CN 201710098358A CN 106904986 B CN106904986 B CN 106904986B
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carbon fiber
insulation board
composite carbon
carbon fibers
heat
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CN106904986A (en
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陈惠龙
郑淑云
王红伟
张作桢
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Liaoning Aoyida New Materials Co.,Ltd.
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Liaoning Aoyida Advanced Material Co ltd
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Abstract

The invention relates to a method for manufacturing a high-performance composite carbon fiber heat-insulation board, which comprises the steps of mixing mixed carbon fibers consisting of chopped carbon fibers and ground carbon fibers with an organic binder and a solvent, removing the solvent, mixing the composite carbon fibers coated with the organic binder on the surface with water and a dispersing agent to form carbon fiber mixed slurry, and carrying out vacuum suction molding to prepare a prefabricated product of the composite carbon fiber heat-insulation board; dehydrating the mixture by adopting a hot steam or hot air heating mode and completing infusible and insoluble treatment; and then carrying out carbonization or graphitization treatment to obtain a finished product of the composite carbon fiber insulation board. The composite carbon fiber insulation board manufactured by the invention has the characteristics of good heat insulation performance, good oxidation resistance, low thermal capacity and high strength, and has the advantages of simple manufacturing process, low cost, controllable shape and size of a finished product and adjustable density; the finished product is not easy to crack, has good self-supporting property and long service life; after surface treatment, the paint also has excellent oxidation resistance and further prolongs the service life.

Description

Manufacturing method of high-performance composite carbon fiber insulation board
Technical Field
The invention relates to the technical field of manufacturing of insulation boards for high-temperature furnaces, in particular to a manufacturing method of a high-performance composite carbon fiber insulation board.
Background
With the progress of science and technology, the fields of military affairs, national defense, solar energy, semiconductors, heat treatment and the like are rapidly developed, and the development of the fields relates to the use of heat insulation materials; especially, in recent years, the rapid development of solar energy and semiconductors makes the demand for thermal insulation materials more prominent, and the demand for thermal insulation materials is higher and higher, so that not only energy conservation and consumption reduction are required, but also high oxidation resistance is required, and the requirements also continuously promote the rapid development of the field of thermal insulation materials.
The carbon fiber heat preservation material which is commonly used in domestic high-temperature vacuum furnaces is soft carbon felt (needle felt), and when the soft carbon felt is used as a heat insulation material, the soft carbon felt has the defects of low strength, easy deformation, easy pulverization, poor heat insulation effect, time and labor waste in disassembly and assembly and the like. The newly developed carbon fiber hard felt heat insulation material can overcome the defects of the soft carbon felt, and therefore, the carbon fiber hard felt heat insulation material is increasingly widely used as a heat insulation material for high temperature furnaces such as crystal furnaces, ceramic sintering furnaces, vapor deposition furnaces and the like.
At present, the domestic carbon fiber hard felt mainly adopts a PAN-based soft carbon felt impregnation molding process. The carbon fiber hard felt manufactured by the impregnation die pressing process has the defects of high energy consumption, low interlaminar strength of the carbon fiber hard felt, easiness in cracking, short service life, high binder content, poor oxidation resistance and the like.
Disclosure of Invention
The invention provides a manufacturing method of a high-performance composite carbon fiber insulation board, and the manufactured composite carbon fiber insulation board has the characteristics of good heat insulation performance, good oxidation resistance, low thermal capacity and high strength, and is simple in manufacturing process, low in cost, controllable in shape and size of a finished product and adjustable in density; the finished product is not easy to crack, has good self-supporting property and long service life; the surface treated product has excellent antioxidant performance and long service life.
In order to achieve the purpose, the invention adopts the following technical scheme:
a manufacturing method of a high-performance composite carbon fiber insulation board comprises the following steps:
1) preparing short carbon fibers; chopping the carbon fibers to obtain chopped carbon fibers with the average length of 1-80 mm;
2) preparing ground carbon fibers; grinding carbon fibers to obtain ground carbon fibers with the average length of 100-800 mu m;
3) fully and uniformly mixing the chopped carbon fibers and the ground carbon fibers by a cyclone separator according to the weight ratio of 10-90: 90-10 to obtain mixed carbon fibers;
4) mixing the mixed carbon fibers with an organic binder and a solvent according to a weight part ratio of 100: 20-230: 3-920 to obtain a carbon fiber mixed solution; putting the carbon fiber mixed solution into a mesh bag, primarily filtering the carbon fiber mixed solution by using the mesh bag with the mesh aperture of 1-50 mu m, and then directly blowing hot air at 50-60 ℃ into the mesh bag for 10-30 min to completely volatilize a solvent in the carbon fiber mixed solution to obtain the composite carbon fiber with the surface coated with the organic binder;
5) fully mixing the composite carbon fibers coated with the organic binder on the surfaces with water and a dispersing agent according to a weight part ratio of 0.3-6: 100: 0.1-2 to form uniform carbon fiber mixed slurry;
6) vacuum suction molding is adopted for the carbon fiber mixed slurry; immersing a heat insulation board forming die for vacuum suction into a forming pool, wherein the heat insulation board forming die consists of an upper die and a lower die which are arranged in a forming die body in parallel, and the upper die and the lower die are both of flat plate structures; wherein the lower die is made of a sieve plate, a screen is fixed on the upper surface of the lower die, and the aperture of the screen is 30-200 mu m; the upper die is a grid plate, and the unilateral or radial size of grid holes is 30-100 mm;
the upper die and the lower die of the insulation board forming die are horizontally placed in the forming pool, and the bottom of the forming pool is provided with a conical structure matched with the forming die body; a vacuum forming chamber is formed among the upper die, the lower die and the enclosing plate of the forming die body, and the vacuum forming chamber has the shape and the size matched with the composite carbon fiber heat-insulation plate; a suction pipe is arranged at the bottom of the forming die body, and carbon fiber mixed slurry is regularly arranged and formed in a vacuum forming chamber under the action of the suction pipe to form a composite carbon fiber heat-insulation board prefabricated product;
7) taking out the composite carbon fiber heat-insulation board prefabricated product together with the heat-insulation board forming die from the forming pool, and heating the composite carbon fiber heat-insulation board prefabricated product for 2-5 hours by adopting hot steam or hot air at the temperature of 100-240 ℃ to dehydrate the composite carbon fiber heat-insulation board prefabricated product and finish non-melting and non-dissolving treatment;
8) demoulding the prefabricated product of the composite carbon fiber heat-insulating board subjected to dehydration, non-melting and non-dissolving treatment, and then putting the prefabricated product into a vacuum furnace or carbonizing the prefabricated product in an inert atmosphere, wherein the carbonization temperature is 800-1800 ℃; graphitization treatment can be carried out according to the use requirement, and the graphitization temperature is 1800-2500 ℃; carbonizing or graphitizing to obtain the high-performance composite carbon fiber insulation board;
9) the density of the prepared composite carbon fiber heat-insulation board is 0.1-0.35 g/cm 3 The heat conductivity coefficient is less than 0.35W/m.K;
10) optionally carrying out surface treatment on the composite carbon fiber heat-insulation board according to the requirement; so as to increase the airflow scouring resistance and the oxidation resistance of the composite material and prolong the service life of the composite material; the surface treatment comprises the following specific steps:
a. performing surface polishing on the composite carbon fiber heat-insulation board through mechanical processing;
b. coating a binder layer on the surface of one side or two sides of the composite carbon fiber heat-insulation board, and further pasting a protective layer outside the binder layer according to needs, wherein the protective layer is flexible graphite paper/carbon fiber cloth, carbon cloth or a graphite sheet, or the protective layer can not be pasted;
c. and c, curing the composite carbon fiber insulation board treated in the step b, and then carbonizing/graphitizing to obtain the surface-treated composite carbon fiber insulation board.
The density of the composite carbon fiber insulation board can be accurately adjusted by changing the mixing proportion of the organic binder, the chopped carbon fibers and the ground carbon fibers and the vacuum degree during vacuum suction molding so as to meet the use requirements under different conditions.
The carbon fiber used in the preparation of the chopped carbon fiber or the ground carbon fiber is one or more of pitch-based carbon fiber, viscose-based carbon fiber and PAN-based carbon fiber, preferably the chopped pitch-based carbon fiber, and is mixed according to any proportion when more than one carbon fiber is selected.
The mesh bag is made of non-woven fabrics, artificial cotton, polypropylene, Teflon or polyester materials, and the aperture of the mesh bag is 1-50 microns, preferably 5-30 microns.
The shape of the grid holes of the upper die is one of a triangle, a circle, a square, a rectangle, a diamond, a regular polygon or an irregular polygon.
The organic binder is selected from one or more of phenolic resin, epoxy resin, furan resin, urea resin, vinyl ester resin, polyamide, acrylic resin, polyethylene, polypropylene, ethylene-propylene copolymer, polystyrene, monosaccharide, polysaccharide, asphalt and tar which are randomly mixed.
The solvent is one or more of methanol, ethanol, propanol, ethylene glycol, propylene glycol, glycerol, diethyl ether, furfuryl alcohol, furfural, acetone, benzene, toluene, furfuryl alcohol and furfural.
The dispersing agent is one or more of methylcellulose, carboxymethyl cellulose, hydroxypropyl methylcellulose, hydroxyethyl methylcellulose, hydroxymethyl cellulose, ethyl cellulose ether, methyl ethyl cellulose, hydroxypropyl ethyl cellulose, hydroxyethyl ethyl cellulose, hydroxymethyl ethyl cellulose, polyvinyl alcohol, polyvinyl acetal, starch and modified starch.
Compared with the prior art, the invention has the beneficial effects that:
1) the composite carbon fiber insulation board with higher density, low thermal conductivity and high strength can be manufactured, and the finished product has excellent crack resistance;
the chopped carbon fibers adopted by the invention not only can increase the strength of the composite carbon fiber heat-insulation board, but also can increase the toughness of the composite carbon fiber heat-insulation board, so that the composite carbon fiber heat-insulation board can resist impact, and has excellent crack resistance; the adopted ground carbon fibers not only can play a role in properly adjusting the density of the composite carbon fiber heat-insulation board, but also can increase the content of carbon fibers in a finished product; the content of the carbon fibers not only can influence the heat conductivity coefficient of the composite carbon fiber insulation board, but also can influence the oxidation resistance of the composite carbon fiber insulation board; the more the carbon fiber content is, the better the carbon fiber content is, the smaller the heat conductivity coefficient of the composite carbon fiber heat-insulation board is; the more the carbon fiber content is, the better the oxidation resistance is;
according to the invention, the density of the composite carbon fiber insulation board can be adjusted by changing the mixing proportion of the organic binder, the chopped carbon fibers and the ground carbon fibers and adjusting the vacuum degree in the vacuum suction forming process; the density of the prepared composite carbon fiber heat-insulation board is 0.1-0.35 g/cm 3 The heat conductivity coefficient is lower than 0.35W/m.K;
2) the invention has the advantages of low production cost, simple process, high stability and convenient operation;
according to the invention, hot steam or hot air is adopted to carry out dehydration, non-melting and insolubilization treatment on the composite carbon fiber heat-insulation board prefabricated product, so that the production efficiency can be greatly improved, the production cost is reduced, and the energy consumption is saved; the dehydration, the non-melting and the insolubilization treatment by adopting the method can be completed only in 2-5 hours, and the non-melting and the insolubilization treatment by adopting a conventional oven or a heating furnace can be completed in 80-120 hours, so the efficiency of the method is improved by dozens of times; the energy consumption of the operation link is reduced from the unit consumption of 11 yuan/kg to less than 3 yuan/kg, and the effects of energy conservation and consumption reduction are obvious;
3) the composite carbon fiber insulation board has a good heat insulation effect;
in the prefabricated product of the composite carbon fiber heat-insulation board, the arrangement direction of carbon fibers accords with two-dimensional arrangement and is vertical to the heat flow direction, so that the prefabricated product is the optimal heat-insulation direction; the product is not easy to crack, has good self-supporting property and long service life; particularly, the method has process advantages when large-size products are manufactured;
4) the invention adopts the matching of the upper die and the lower die, the shape and the size of the product can be shaped at one time through vacuum suction, the finished product can be processed slightly to obtain a fixed-size product, and the material utilization rate can reach more than 90%; the size of a product formed by adopting a common die cannot be accurately controlled, the surface processing amount is large, and the product utilization rate can reach 75-80% at most; therefore, the invention greatly improves the utilization rate of materials and reduces the generation of waste materials, thereby greatly reducing the production cost;
5) according to the use requirements, the composite carbon fiber insulation board can be further subjected to surface treatment on the basis of the prepared composite carbon fiber insulation board, so that the direct contact between the gas in the high-temperature furnace and the composite carbon fiber insulation board can be prevented, the airflow scouring resistance of the composite carbon fiber insulation board is improved, the composite carbon fiber insulation board has excellent oxidation resistance, and the service life of the composite carbon fiber insulation board is further prolonged.
Drawings
FIG. 1 is a schematic view of a vacuum suction forming process according to the present invention.
FIG. 2 is a schematic structural diagram of a heated board forming mold used in the vacuum suction forming of the invention;
fig. 3 is a schematic structural view of an upper die of the insulation board forming die of the present invention. (taking diamond grid holes as an example)
FIG. 4 is a schematic structural diagram of the composite carbon fiber insulation board of the present invention after surface treatment of the upper surface thereof.
FIG. 5 is a schematic structural view of the composite carbon fiber insulation board according to the present invention after surface treatment of the upper and lower surfaces thereof.
In the figure: 1. the forming pool 2, the insulation board forming die 3, the vacuum tank 4, the water ring vacuum pump 5, the suction pipe 6, the lower die 7, the composite carbon fiber insulation board prefabricated product 8, the upper die 9, the composite carbon fiber insulation board 10, the adhesive layer 11, the protective layer 12 and the forming trolley
Detailed Description
The following further describes embodiments of the present invention in conjunction with the attached figures:
the invention relates to a manufacturing method of a high-performance composite carbon fiber insulation board, which comprises the following steps:
1) preparing short carbon fibers; chopping the carbon fibers to obtain chopped carbon fibers with the average length of 1-80 mm;
2) preparing ground carbon fibers; grinding carbon fibers to obtain ground carbon fibers with the average length of 100-800 mu m;
3) fully and uniformly mixing the chopped carbon fibers and the ground carbon fibers according to the weight part ratio of 10-90: 90-10 by adopting a cyclone separator to obtain mixed carbon fibers;
4) mixing the mixed carbon fibers with an organic binder and a solvent according to a weight part ratio of 100: 20-230: 3-920 to obtain a carbon fiber mixed solution; putting the carbon fiber mixed solution into a mesh bag, primarily filtering the carbon fiber mixed solution by using the mesh bag with the mesh aperture of 1-50 mu m, and then directly blowing hot air at 50-60 ℃ into the mesh bag for 10-30 min to completely volatilize a solvent in the carbon fiber mixed solution to obtain the composite carbon fiber with the surface coated with the organic binder;
5) fully mixing the composite carbon fiber coated with the organic binder on the surface with water and a dispersing agent according to a weight ratio of 0.3-6: 100: 0.1-2 to form uniform carbon fiber mixed slurry;
6) vacuum suction molding is adopted for the carbon fiber mixed slurry; as shown in fig. 1, a heat insulation board forming mold 2 for vacuum suction is immersed in a forming pool 1, the heat insulation board forming mold 2 is composed of an upper mold 8 and a lower mold 6 which are arranged in parallel in a forming mold body, and the upper mold 8 and the lower mold 6 are both of a flat plate structure; wherein the lower die 6 is made of a sieve plate, the upper surface of which is fixed with a screen, and the aperture of the screen is 30-200 μm; the upper die 8 is a grid plate (as shown in fig. 3), and the unilateral or radial size of the grid holes is 30-100 mm;
as shown in fig. 1 and 2, the upper mold and the lower mold 8 and 6 of the insulation board forming mold 2 are both placed in a forming pool 1 in a horizontal state, and the bottom of the forming pool 1 is provided with a conical structure adapted to a forming mold body; a vacuum forming chamber is formed among the upper die 8, the lower die 6 and the enclosing plate of the forming die body, and the vacuum forming chamber has the shape and the size matched with the composite carbon fiber heat-insulation plate; the bottom of the forming die body is provided with a suction pipe 5, and under the action of the suction pipe 5, the carbon fiber mixed slurry is arranged and formed in a vacuum forming chamber according to a rule to prepare a composite carbon fiber heat-insulation board prefabricated product 7;
7) taking the composite carbon fiber heat-insulation board prefabricated product 7 together with the heat-insulation board forming die 2 out of the forming pool 1, and heating the composite carbon fiber heat-insulation board prefabricated product 7 for 2-5 hours by adopting hot steam or hot air at the temperature of 100-240 ℃ to dehydrate the composite carbon fiber heat-insulation board prefabricated product and finish non-melting and non-dissolving treatment;
8) the prefabricated product 7 of the composite carbon fiber heat-insulation board after dehydration, infusibility and infusibility is demoulded and then is put into a vacuum furnace or carbonized under inert atmosphere, wherein the carbonization temperature is 800-1800 ℃; graphitization treatment can be carried out according to the use requirement, and the graphitization temperature is 1800-2500 ℃; carbonizing or graphitizing to obtain a high-performance composite carbon fiber insulation board 9;
9) the density of the prepared composite carbon fiber heat-insulation board 9 is 0.1-0.35 g/cm 3 The heat conductivity coefficient is less than 0.35W/m.K;
10) optionally carrying out surface treatment on the composite carbon fiber heat-insulation board 9 according to the requirement; so as to increase the airflow scouring resistance and the oxidation resistance of the composite material and prolong the service life of the composite material; the surface treatment comprises the following specific steps:
a. the composite carbon fiber heat-insulation board 9 is subjected to surface polishing through machining;
b. as shown in fig. 4 and 5, an adhesive layer 10 is coated on one or both surfaces of the composite carbon fiber insulation board 9, a protective layer 11 may be further adhered outside the adhesive layer 10 as required, and the protective layer 11 may be flexible graphite paper/carbon fiber cloth, carbon cloth or a graphite sheet, or may not be adhered with the protective layer 11;
c. and c, curing the composite carbon fiber insulation board treated in the step b, and then carbonizing/graphitizing to obtain the surface-treated composite carbon fiber insulation board.
By changing the mixing proportion of the organic binder, the chopped carbon fibers and the ground carbon fibers and the vacuum degree during vacuum suction forming, the density of the composite carbon fiber insulation board 9 can be accurately adjusted to meet the use requirements under different conditions.
The carbon fiber used in the preparation of the chopped carbon fiber or the ground carbon fiber is one or more of pitch-based carbon fiber, viscose-based carbon fiber and PAN-based carbon fiber, the chopped pitch-based carbon fiber is preferred, and more than one carbon fiber is mixed according to any proportion.
The mesh bag is made of non-woven fabrics, artificial cotton, polypropylene, Teflon or polyester materials, and the aperture of the mesh bag is 1-50 microns, preferably 5-30 microns.
The shape of the grid holes of the upper die 8 is one of triangle, circle, square, rectangle, rhombus, regular polygon or irregular polygon.
The organic binder is selected from one or more of phenolic resin, epoxy resin, furan resin, urea resin, vinyl ester resin, polyamide, acrylic resin, polyethylene, polypropylene, ethylene-propylene copolymer, polystyrene, monosaccharide, polysaccharide, asphalt and tar which are randomly mixed.
The solvent is one or more of methanol, ethanol, propanol, ethylene glycol, propylene glycol, glycerol, diethyl ether, furfuryl alcohol, furfural, acetone, benzene, toluene, furfuryl alcohol and furfural.
The dispersing agent is selected from one or more of methyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl methyl cellulose, hydroxymethyl cellulose, ethyl cellulose ether, methyl ethyl cellulose, hydroxypropyl ethyl cellulose, hydroxyethyl ethyl cellulose, hydroxymethyl ethyl cellulose, polyvinyl alcohol, polyvinyl acetal, starch and modified starch.
The following examples are carried out on the premise of the technical scheme of the invention, and detailed embodiments and specific operation procedures are given, but the scope of the invention is not limited to the following examples. The methods and materials used in the following examples are conventional methods and materials unless otherwise specified.
[ example 1 ] A method for producing a polycarbonate
In this embodiment, the manufacturing method of the high-performance composite carbon fiber insulation board is as follows:
1) preparing short carbon fibers; short cutting the pitch-based carbon fiber to obtain short carbon fiber with the average length of 40 mm;
2) preparing ground carbon fibers; grinding pitch-based carbon fibers to obtain ground carbon fibers having an average length of 100 μm;
3) mixing the chopped carbon fibers and the ground carbon fibers according to the weight ratio of 60: 40 parts by weight, and fully and uniformly mixing by adopting a cyclone separator to obtain mixed carbon fibers;
4) mixing the mixed carbon fiber with organic binder phenolic resin and solvent ethanol according to the ratio of 100: 30: 70 parts by weight of the raw materials are mixed to obtain carbon fiber mixed liquor; putting the carbon fiber mixed solution into a mesh bag, primarily filtering the carbon fiber mixed solution by using the mesh bag with the mesh aperture of 30 mu m, and then directly blowing hot air at 50 ℃ into the mesh bag for 30min to completely volatilize the solvent in the carbon fiber mixed solution to obtain the composite carbon fiber with the surface coated with the organic binder;
5) fully mixing the composite carbon fiber coated with the organic binder on the surface with water and methylcellulose according to the weight part ratio of 3: 100: 1 to form uniform carbon fiber mixed slurry;
6) vacuum suction molding is adopted for the carbon fiber mixed slurry; a heat insulation board forming die 2 for vacuum suction is immersed into a forming pool 1, and the forming pool 1 is arranged on a forming trolley 12, so that the transportation of materials after the forming is finished is facilitated; the insulation board forming die 2 consists of a lower die 6 and an upper die 8 which are arranged in a forming die body in parallel, wherein the lower die 6 is made of a sieve plate, a sieve mesh is fixed on the upper surface of the lower die, the aperture of the sieve mesh is 50 micrometers, the upper die 8 is a grid plate, and the unilateral or radial size of the grid hole is 60 mm;
the upper die 8 and the lower die 6 of the insulation board forming die 2 are both placed in the forming pool 1 in a horizontal state, the peripheries of the upper die 8 and the lower die 6 are respectively attached to the enclosing plate of the forming die body, and the formed space is a vacuum forming chamber; the vacuum forming chamber has the shape and size matched with the composite carbon fiber heat-insulation plate; the suction pipe 5 is arranged at the bottom of the forming die body, the suction pipe 5 is connected with the vacuum tank 3 through a hose, and the vacuum tank 3 is further connected with the water ring vacuum pump 4 to form a vacuum suction device; after a vacuum suction device is started, under the action of a suction pipe 5, carbon fiber mixed slurry is regularly arranged and formed in a vacuum forming chamber to form a composite carbon fiber heat insulation board prefabricated product 7;
7) taking the composite carbon fiber heat insulation board prefabricated product 7 together with the heat insulation board forming die 2 out of the forming pool 1, and heating the composite carbon fiber heat insulation board prefabricated product 7 for 3 hours by adopting hot steam or hot air at 150 ℃ to dehydrate the composite carbon fiber heat insulation board prefabricated product and finish non-melting and non-dissolving treatment;
8) the prefabricated product 7 of the composite carbon fiber heat-insulating board after dehydration, infusibility and infusibility is demoulded and then is put into a vacuum furnace or carbonized under inert atmosphere, and the carbonization temperature is 1200 ℃; then carrying out graphitization treatment at the graphitization temperature of 2100 ℃; carbonizing or graphitizing to obtain a high-performance composite carbon fiber insulation board 9;
9) the density of the prepared composite carbon fiber heat-insulation board 9 is 0.16g/cm 3 The thermal conductivity coefficient is 0.22W/m.K; carbon content 99.6%, ash content 0.01%; (test data of a specimen having a thickness of 45mm at 1500 ℃ under a nitrogen atmosphere).
[ example 2 ]
In order to increase the airflow scouring resistance and oxidation resistance of the composite carbon fiber heat-insulation board 9, the service life of the heat-insulation board is further prolonged; the composite carbon fiber heat-insulation board 9 prepared in embodiment 1 is subjected to surface treatment, and the specific steps of the surface treatment are as follows:
1) carrying out surface polishing treatment on the composite carbon fiber heat-insulation board 9 by mechanical processing to ensure that the surface is smooth;
2) respectively brushing 3-6 times of adhesive on the upper surface and the lower surface of the composite carbon fiber insulation board 9 with polished surfaces to form an adhesive layer 10, wherein the adhesive is a conventionally used adhesive;
3) putting the composite carbon fiber heat-insulation board 9 coated with the binder layer 10 into a heating furnace, heating to 240 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant at the temperature for 1h, and curing the binder layer 10; and then, putting the board at 1700 ℃ and carrying out carbonization treatment in inert atmosphere to prepare the composite carbon fiber insulation board with the coating.
The composite carbon fiber insulation board with the coating prepared by the embodiment is used on a monocrystalline silicon stretching furnace for 100 times, the phenomena of coating stripping, cracking, bubbling and the like do not occur, and the composite carbon fiber insulation board in the coating does not have the corrosion phenomenon.
[ example 3 ] A method for producing a polycarbonate
In this embodiment, the manufacturing method of the high-performance composite carbon fiber insulation board is as follows:
1) preparing short carbon fibers; short cutting the pitch-based carbon fiber to obtain short carbon fiber with the average length of 80 mm;
2) preparing ground carbon fibers; grinding pitch-based carbon fibers to obtain ground carbon fibers having an average length of 180 μm;
3) mixing the chopped carbon fibers and the ground carbon fibers according to a ratio of 50: 50 parts by weight of the carbon fiber are fully and uniformly mixed by adopting a cyclone separator to obtain mixed carbon fiber;
4) mixing the mixed carbon fiber with organic binder phenolic resin and solvent ethanol according to the ratio of 100: 55: 75 parts by weight of the raw materials are mixed to obtain carbon fiber mixed solution; putting the carbon fiber mixed solution into a mesh bag, primarily filtering the carbon fiber mixed solution by using the mesh bag with the mesh aperture of 30 mu m, and then directly blowing hot air at 60 ℃ into the mesh bag for 30min to completely volatilize a solvent in the carbon fiber mixed solution to obtain composite carbon fiber with the surface coated with an organic binder;
5) fully mixing the composite carbon fiber coated with the organic binder on the surface with water and methyl cellulose according to the weight ratio of 6: 100: 1 to form uniform carbon fiber mixed slurry;
6) vacuum suction molding is adopted for the carbon fiber mixed slurry; immersing a heat-insulation plate forming die 2 for vacuum suction into a forming pool 1; the insulation board forming die 2 consists of a lower die 6 and an upper die 8 which are arranged in a forming die body in parallel, wherein the lower die 6 is made of a sieve plate, a sieve mesh is fixed on the outer surface of the lower die, the aperture of the sieve mesh is 70 mu m, the upper die 8 is of a grid structure, and the unilateral or radial size of the grid hole is 100 mm;
under the action of the suction pipe 5, the carbon fiber mixed slurry is regularly arranged and formed in a vacuum forming chamber to prepare a composite carbon fiber heat-insulation board prefabricated product 7;
7) taking the composite carbon fiber heat insulation board prefabricated product 7 together with the heat insulation board forming die 2 out of the forming pool 1, and heating the composite carbon fiber heat insulation board prefabricated product 7 by adopting hot steam or hot air at 180 ℃ for 2.5 hours to dehydrate the composite carbon fiber heat insulation board prefabricated product and finish non-melting and non-dissolving treatment;
8) the prefabricated product 7 of the composite carbon fiber heat-insulating board after dehydration, infusibility and infusibility is demoulded and then is put into a vacuum furnace or carbonized under inert atmosphere, and the carbonization temperature is 1500 ℃; then carrying out graphitization treatment at the graphitization temperature of 2000 ℃; carbonizing or graphitizing to obtain a high-performance composite carbon fiber insulation board 9;
9) the density of the prepared composite carbon fiber heat-insulation board 9 is 0.19g/cm 3 The heat conductivity coefficient is 0.20W/m.K; carbon content 99.7%, ash content 0.01%; (test data of a specimen having a thickness of 45mm at 1500 ℃ under a nitrogen atmosphere).
In order to increase the airflow scouring resistance and oxidation resistance of the composite carbon fiber heat-insulation board 9, the service life of the heat-insulation board is further prolonged; the prepared composite carbon fiber insulation board 9 is further subjected to surface treatment, and the specific steps of the surface treatment are as follows:
1) the composite carbon fiber heat-insulation board 9 is subjected to surface polishing treatment through mechanical processing, so that the surface is smooth;
2) respectively brushing 3-6 times of adhesive on the upper surface and the lower surface of the composite carbon fiber insulation board 9 with polished surfaces to form an adhesive layer 10, wherein the adhesive is a conventionally used adhesive; a protective layer 11 is adhered outside the adhesive layer 10, and the protective layer 11 is flexible graphite paper;
3) putting the composite carbon fiber insulation board 9 which is coated with the adhesive layer 10 and is adhered with the protective layer 11 into a heating furnace, heating to 300 ℃ at a heating rate of 8 ℃/min, keeping the temperature at the temperature for 1h, and curing the adhesive layer 10; and then the composite carbon fiber insulation board is placed at 1800 ℃ and carbonized under inert atmosphere to prepare the composite carbon fiber insulation board with the protective layer.
The composite carbon fiber insulation board with the protective layer manufactured by the embodiment is used on a monocrystalline silicon stretching furnace for 100 times, the phenomena of stripping, cracking, bubbling and the like of the protective layer do not occur, and the composite carbon fiber insulation board in the protective layer is free of corrosion.
The embodiment can prove that the composite carbon fiber heat-insulation board with the coating or the protective layer can prevent impurity gas in the furnace from directly contacting the surface of the composite carbon fiber heat-insulation board, prevent the impurity gas from being corroded and resist air current scouring, have excellent oxidation resistance and corrosion resistance, and can obviously prolong the service life of the composite carbon fiber heat-insulation board.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (8)

1. A manufacturing method of a high-performance composite carbon fiber insulation board is characterized by comprising the following steps:
1) preparing short carbon fibers; chopping the carbon fibers to obtain chopped carbon fibers with the average length of 1-80 mm;
2) preparing ground carbon fibers; grinding carbon fibers to obtain ground carbon fibers with the average length of 100-800 mu m;
3) fully and uniformly mixing the chopped carbon fibers and the ground carbon fibers by a cyclone separator according to the weight ratio of 10-90: 90-10 to obtain mixed carbon fibers;
4) mixing the mixed carbon fibers with an organic binder and a solvent according to a weight part ratio of 100: 20-230: 3-920 to obtain a carbon fiber mixed solution; putting the carbon fiber mixed solution into a mesh bag, primarily filtering the carbon fiber mixed solution by using the mesh bag with the mesh aperture of 1-50 mu m, and then directly blowing hot air at 50-60 ℃ into the mesh bag for 10-30 min to completely volatilize a solvent in the carbon fiber mixed solution to obtain the composite carbon fiber with the surface coated with the organic binder;
5) fully mixing the composite carbon fiber coated with the organic binder on the surface with water and a dispersing agent according to a weight ratio of 0.3-6: 100: 0.1-2 to form uniform carbon fiber mixed slurry;
6) vacuum suction molding is adopted for the carbon fiber mixed slurry; immersing a heat-insulating plate forming die for vacuum suction into a forming pool, wherein the heat-insulating plate forming die consists of an upper die and a lower die which are arranged in a forming die body in parallel, and the upper die and the lower die are both of flat plate structures; wherein the lower die is made of a sieve plate, a screen is fixed on the upper surface of the lower die, and the aperture of the screen is 30-200 mu m; the upper die is a grid plate, and the unilateral or radial size of grid holes is 30-100 mm;
the upper die and the lower die of the insulation board forming die are horizontally placed in the forming pool, and the bottom of the forming pool is provided with a conical structure matched with the forming die body; a vacuum forming chamber is formed among the upper die, the lower die and the enclosing plate of the forming die body, and the vacuum forming chamber has the shape and the size matched with the composite carbon fiber heat-insulation plate; a suction pipe is arranged at the bottom of the forming die body, and carbon fiber mixed slurry is regularly arranged and formed in a vacuum forming chamber under the action of the suction pipe to form a composite carbon fiber heat-insulation board prefabricated product;
7) taking out the composite carbon fiber heat-insulation board prefabricated product together with the heat-insulation board forming die from the forming pool, and heating the composite carbon fiber heat-insulation board prefabricated product for 2-5 hours by adopting hot steam or hot air at the temperature of 100-240 ℃ to dehydrate the composite carbon fiber heat-insulation board prefabricated product and finish non-melting and non-dissolving treatment;
8) demolding the prefabricated product of the composite carbon fiber heat-insulating board subjected to dehydration, non-melting and non-dissolving treatment, and then putting the prefabricated product into a vacuum furnace or carbonizing the prefabricated product in an inert atmosphere, wherein the carbonization temperature is 800-1800 ℃; graphitization treatment can be carried out according to the use requirement, and the graphitization temperature is 1800-2500 ℃; carbonizing or graphitizing to obtain the high-performance composite carbon fiber insulation board;
9) the density of the prepared composite carbon fiber heat-insulation board is 0.1-0.35 g/cm 3 The heat conductivity coefficient is less than 0.35W/m.K;
10) optionally carrying out surface treatment on the composite carbon fiber heat-insulation board according to the requirement; so as to increase the airflow scouring resistance and oxidation resistance and prolong the service life of the device; the surface treatment comprises the following specific steps:
a. performing surface polishing on the composite carbon fiber heat-insulation board through mechanical processing;
b. coating a binder layer on the surface of one side or two sides of the composite carbon fiber heat-insulation board, and further pasting a protective layer outside the binder layer according to needs, wherein the protective layer is flexible graphite paper/carbon fiber cloth, carbon cloth or a graphite sheet or can be not pasted with the protective layer;
c. and c, curing the composite carbon fiber insulation board treated in the step b, and then performing carbonization/graphitization treatment to obtain the surface-treated composite carbon fiber insulation board.
2. The manufacturing method of the high-performance composite carbon fiber insulation board according to claim 1, characterized in that the density of the composite carbon fiber insulation board is accurately adjusted by changing the mixing ratio of the organic binder, the chopped carbon fibers and the ground carbon fibers and the vacuum degree during vacuum suction molding so as to meet the use requirements under different conditions.
3. The manufacturing method of the high-performance composite carbon fiber insulation board according to claim 1, wherein the carbon fibers used for preparing the chopped carbon fibers or the ground carbon fibers are one or more of pitch-based carbon fibers, viscose-based carbon fibers and PAN-based carbon fibers, and the carbon fibers are mixed according to any proportion when more than one carbon fiber is selected.
4. The manufacturing method of the high-performance composite carbon fiber insulation board according to claim 1, wherein the mesh bag is made of non-woven fabric, artificial cotton, polypropylene, Teflon or polyester material, and the aperture of the mesh bag is 1-50 μm.
5. The manufacturing method of the high-performance composite carbon fiber insulation board according to claim 1, wherein the shape of the grid holes of the upper die is one of a triangle, a circle, a rectangle, a diamond or an irregular polygon.
6. The method for manufacturing the high-performance composite carbon fiber insulation board according to claim 1, wherein the organic binder is one or more of phenolic resin, epoxy resin, furan resin, urea resin, vinyl ester resin, polyamide, acrylic resin, polyethylene, polypropylene, ethylene-propylene copolymer, polystyrene, monosaccharide, polysaccharide, asphalt and tar.
7. The manufacturing method of the high-performance composite carbon fiber insulation board according to claim 1, wherein the solvent is one or more of methanol, ethanol, propanol, ethylene glycol, propylene glycol, glycerol, diethyl ether, furfuryl alcohol, furfural, acetone, benzene, toluene, furfuryl alcohol, and furfural.
8. The method for manufacturing the high-performance composite carbon fiber heat-insulation board according to claim 1, wherein the dispersant is one or more selected from the group consisting of methyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl methyl cellulose, hydroxymethyl cellulose, ethyl cellulose ether, methyl ethyl cellulose, hydroxypropyl ethyl cellulose, hydroxyethyl ethyl cellulose, hydroxymethyl ethyl cellulose, polyvinyl alcohol, polyvinyl acetal, starch and modified starch.
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