CN111844962B - Ceramic fiber reinforced aerogel felt and preparation method thereof - Google Patents
Ceramic fiber reinforced aerogel felt and preparation method thereof Download PDFInfo
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- CN111844962B CN111844962B CN202010665643.3A CN202010665643A CN111844962B CN 111844962 B CN111844962 B CN 111844962B CN 202010665643 A CN202010665643 A CN 202010665643A CN 111844962 B CN111844962 B CN 111844962B
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- 239000000835 fiber Substances 0.000 title claims abstract description 170
- 239000000919 ceramic Substances 0.000 title claims abstract description 77
- 239000004964 aerogel Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000003365 glass fiber Substances 0.000 claims abstract description 49
- 239000004744 fabric Substances 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000002002 slurry Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 28
- 239000004831 Hot glue Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 18
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 235000019441 ethanol Nutrition 0.000 claims abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 13
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000010030 laminating Methods 0.000 claims abstract description 9
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000007731 hot pressing Methods 0.000 claims abstract description 3
- 239000002131 composite material Substances 0.000 claims description 32
- 238000003892 spreading Methods 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 238000000465 moulding Methods 0.000 claims description 16
- 229910017855 NH 4 F Inorganic materials 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 10
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 10
- IWICDTXLJDCAMR-UHFFFAOYSA-N trihydroxy(propan-2-yloxy)silane Chemical compound CC(C)O[Si](O)(O)O IWICDTXLJDCAMR-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 8
- 230000001680 brushing effect Effects 0.000 claims description 8
- 229920002748 Basalt fiber Polymers 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 6
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 claims description 6
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 6
- 229910052863 mullite Inorganic materials 0.000 claims description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000006467 substitution reaction Methods 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 10
- 238000005470 impregnation Methods 0.000 abstract description 7
- 238000009413 insulation Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 229920006223 adhesive resin Polymers 0.000 abstract description 3
- 239000011229 interlayer Substances 0.000 abstract description 2
- 239000004965 Silica aerogel Substances 0.000 description 10
- 238000002791 soaking Methods 0.000 description 8
- 239000012783 reinforcing fiber Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of ceramic fiber reinforced aerogel felt, which comprises the steps of uniformly mixing orthosilicate, ethanol and water, and then sequentially adding NH 4 Stirring the solution F and ammonia water uniformly to obtain silica sol; dispersing the hot melt adhesive powder and ceramic fibers in water, and uniformly stirring and mixing to obtain viscous slurry; coating the thick slurry on glass fiber cloth, laminating, hot-pressing, performing gum dipping treatment in silica sol, then placing in absolute ethyl alcohol for solvent replacement, removing water, and drying to obtain the prepared ceramic fiber reinforced aerogel felt. According to the invention, ceramic fibers are pressed into the felt through the hot melt adhesive resin powder, so that the ceramic fiber felt layer has certain flexibility, and meanwhile, the glass fiber cloth with the interlayer can improve the tensile property of the fiber felt, so that the brittleness of the traditional ceramic fiber felt is solved. The invention can maintain the structural integrity of the felt body in the impregnation process, has convenient impregnation operation, and ensures the heat insulation performance of the ceramic fiber reinforced aerogel felt body.
Description
Technical Field
The invention belongs to the technical field of preparation of aerogel felts, and particularly relates to a ceramic fiber reinforced aerogel felt and a preparation method thereof.
Background
The silica aerogel is a continuous three-dimensional network structure formed by mutually polymerizing nano-scale particles, and has special nano-scale micropores and a skeleton structure, so that the thermal conductivity, the convection heat transfer efficiency and the radiation heat transfer efficiency are effectively limited, and therefore, the aerogel has very low heat conductivity and is a solid material with the lowest heat conductivity in the world at present. The material composition is inorganic matter, belongs to class A non-combustible materials, and can replace the application of the existing organic heat-insulating materials in industrial building heat-insulating systems. However, the mechanical strength and toughness of the pure aerogel are low, which results in poor dimensional stability of the aerogel material, and limits the operability and application of the aerogel material in construction. To solve such problems, fiber-reinforced aerogel mats, such as ceramic fiber mats, glass fiber mats, rock wool fiber mats, and the like, are currently used in production. Because of the good mechanical flexibility of the glass fiber mat, the glass fiber mat is widely focused and used in the fields of production, heat insulation and heat preservation. However, in view of the fact that the highest temperature resistance of the glass fiber reinforced aerogel can only reach 600 ℃, the requirement of the high-temperature technical field on heat insulation performance cannot be met.
The ceramic fiber reinforced silica aerogel felt is widely focused on the application of the ceramic fiber reinforced silica aerogel felt in the high-temperature field in view of the good high-temperature resistance of the ceramic fiber. However, the ceramic fiber is subject to the defects of poor tensile property and poor rebound resilience of ceramic fibers, and the fibers are easily broken in the impregnation process of the fiber mat, so that the heat insulation performance of the mat body is affected. In order to further overcome the problem that the ceramic fiber felt has poor tensile resistance and rebound resilience in practical application, the invention aims to design the ceramic fiber felt body so as to enhance the mechanical flexibility of the ceramic fiber felt body, thereby ensuring the performance stability of the fiber reinforced aerogel felt in the production and application processes.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: overcomes the defects existing in the prior art and provides a ceramic fiber reinforced aerogel felt and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating ceramic fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is a silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt is characterized by comprising the following specific steps of:
(1) Mixing orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, the orthosilicate: ethanol: water = 1: (4-12): (2-4); NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 F: orthosilicate= (0.002-0.01): 1, a step of; the addition amount of ammonia ensures that NH is calculated by mole ratio 3 Orthosilicate= (0.005-0.015): 1, a step of;
(2) Dispersing the hot melt adhesive powder and ceramic fibers in water, and uniformly stirring and mixing to obtain viscous slurry B; wherein, the hot melt adhesive powder comprises the following components in percentage by mass: ceramic fiber: water= (0.5 to 1.5): (0.1-0.5): 1, a step of;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth C, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber felt laminated body with the required thickness;
(4) Performing hot press molding on the fiber felt layer stack body obtained in the step (3) to obtain a reinforced fiber felt D;
(5) Dipping the reinforced fiber mat D obtained in the step (4) in the silica sol A obtained in the step (1), standing and aging for 8-24 h at 30-60 ℃ after dipping;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for multiple solvent replacement, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
Preferably, in step (1), the orthosilicate is one of ethyl orthosilicate, methyl orthosilicate, and isopropyl orthosilicate.
Preferably, in step (2), the hot melt adhesive powder is one or more of an ethylene-vinyl acetate copolymer powder, an ethylene-acrylic acid copolymer powder, or a polyvinyl alcohol powder.
Preferably, in the step (2), the ceramic fiber is one of aluminum silicate fiber, mullite fiber, quartz fiber, alumina fiber and basalt fiber.
Preferably, in the step (2), the ceramic fiber has a length of 20 to 100 μm.
Preferably, in the step (3), the thickness of the viscous slurry B is 0.2-1 mm.
Preferably, in the step (4), the hot pressing is performed at a temperature of 80 to 120 ℃ and a pressure of 0.2 to 1 Mpa.
Preferably, in the step (5), the time for the gum dipping is 12 to 24 and h.
Preferably, in the step (6), the number of solvent substitutions is 2 to 3, and the time for each substitution is 12 to 36 hours.
The invention has the following positive beneficial effects:
the invention provides a preparation method of a ceramic fiber reinforced aerogel felt, which comprises the steps of pressing ceramic fibers into a felt through hot melt adhesive resin powder, and performing sol-gel reaction to obtain an aerogel felt body, wherein the hot melt adhesive resin powder can play a role in adhering the ceramic fiber felt, so that the ceramic fiber felt layer has certain flexibility, and meanwhile, the glass fiber cloth of an interlayer can well improve the reinforced tensile property of the fiber felt, so that the brittleness of the traditional ceramic fiber felt is solved.
The reinforced fiber felt can maintain the structural integrity of the felt body in the impregnation process, improve the operation convenience degree in the impregnation process and ensure the heat insulation performance of the ceramic fiber reinforced aerogel felt body.
The method is simple in process operation, and overcomes the defects of poor tensile property and poor rebound resilience of the ceramic fiber. The prepared ceramic fiber reinforced aerogel felt has certain flexibility, expands the application range of the ceramic fiber reinforced aerogel felt in the field of heat insulation and heat preservation, and meets the use requirements of the ceramic fiber reinforced aerogel felt in the field of different high-temperature structures.
Detailed Description
The technical scheme of the present invention will be described in further detail and clearly in connection with the following specific embodiments, but the scope of the present invention is not limited thereto.
Example 1
The ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating aluminum silicate fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing ethyl orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, the tetraethoxysilane: ethanol: water = 1:9:2; NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 F: tetraethoxysilane=0.008: 1, a step of; the addition amount of ammonia ensures that NH is calculated by mole ratio 3 : tetraethoxysilane=0.012: 1, a step of;
(2) Dispersing hot melt adhesive powder ethylene-vinyl acetate copolymer and aluminum silicate fiber in water, and stirring and mixing uniformly to obtain viscous slurry B; wherein, the mass ratio of the hot melt adhesive powder ethylene-vinyl acetate copolymer is as follows: aluminum silicate fibers: water = 0.9:0.3:1, the length of the aluminum silicate fiber is 30 mu m;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber laminated body with required thickness;
(4) Performing hot press molding on the fiber laminated body obtained in the step (3) at 100 ℃ and 0.2Mpa to obtain a reinforced fiber felt D;
(5) Soaking the reinforcing fiber felt D obtained in the step (4) in the silica sol A obtained in the step (1) for 16 hours, and standing and aging at 50 ℃ for 18h after soaking;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for replacement for 2 times, wherein each replacement time is 24 hours, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
Example 2
The ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating mullite fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing methyl orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, methyl orthosilicate: ethanol: water = 1:10:4, a step of; NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 F: methyl orthosilicate = 0.004:1, a step of; ammonia water is added in a molar ratio of NH 3 : methyl orthosilicate = 0.006:1, a step of;
(2) Dispersing hot melt adhesive powder ethylene-acrylic acid copolymer and mullite fiber in water, and uniformly stirring and mixing to obtain viscous slurry B; wherein, the mass ratio of the hot melt adhesive powder ethylene-acrylic acid copolymer is as follows: mullite fiber: water = 1.2:0.4:1, the length of the mullite fiber is 50 mu m;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth C, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber laminated body with required thickness;
(4) Performing hot press molding on the fiber laminated body obtained in the step (3) at 110 ℃ and 0.5Mpa to obtain a reinforced fiber felt D;
(5) Soaking the reinforcing fiber felt D obtained in the step (4) in the silica sol A obtained in the step (1) for 24 hours, and standing and aging at 30 ℃ for 24h after soaking;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for replacement for 2 times, wherein each replacement time is 20 hours, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
Example 3
The ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating quartz fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing isopropyl orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, isopropyl orthosilicate: ethanol: water = 1:8:3, a step of; NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 Isopropyl orthosilicate=0.006:1; ammonia water is added in a molar ratio of NH 3 : isopropyl orthosilicate=0.01: 1, a step of;
(2) Dispersing hot melt adhesive powder polyvinyl alcohol and quartz fibers in water, and uniformly stirring and mixing to obtain viscous slurry B; wherein, the mass ratio is as follows, the hot melt adhesive powder polyvinyl alcohol: quartz fiber: water = 0.6:0.2:1, the length of the quartz fiber is 60 mu m;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber laminated body with required thickness;
(4) Performing hot press molding on the fiber laminated body obtained in the step (3) at 120 ℃ and 0.2Mpa to obtain a reinforced fiber felt D;
(5) Impregnating the reinforcing fiber felt D obtained in the step (4) in the silica sol A obtained in the step (1) for 20 hours, and standing and aging for 16 hours at 40 ℃ after impregnation;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for replacement for 3 times, wherein each replacement time is 16 hours, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
Example 4
The ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating alumina fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing ethyl orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, the tetraethoxysilane: ethanol: water = 1:4:2; NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 F: tetraethoxysilane=0.002: 1, a step of; the addition amount of ammonia ensures that NH is calculated by mole ratio 3 : tetraethoxysilane=0.005: 1, a step of;
(2) Dispersing hot melt adhesive powder ethylene-vinyl acetate copolymer and alumina fiber in water, and stirring and mixing uniformly to obtain viscous slurry B; wherein, the mass ratio of the hot melt adhesive powder ethylene-vinyl acetate copolymer is as follows: alumina fiber: water = 0.5:0.1:1, alumina fiber length 40 μm;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber laminated body with required thickness;
(4) Performing hot press molding on the fiber laminated body obtained in the step (3) at 80 ℃ and 0.3Mpa to obtain a reinforced fiber felt D;
(5) Soaking the reinforcing fiber felt D obtained in the step (4) in the silica sol A obtained in the step (1) for 15 hours, and standing and aging for 10h at 40 ℃ after soaking;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for replacement for 2 times, wherein the replacement time is 15 hours each time, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
Example 5
The ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is formed by coating basalt fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing methyl orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, methyl orthosilicate: ethanol: water = 1:12:4, a step of; NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 F: methyl orthosilicate = 0.01:1, a step of; ammonia water is added in a molar ratio of NH 3 : methyl orthosilicate = 0.015:1, a step of;
(2) Dispersing hot melt adhesive powder ethylene-acrylic acid copolymer and basalt fiber in water, and uniformly stirring and mixing to obtain a viscous slurry B; wherein, the mass ratio of the hot melt adhesive powder ethylene-acrylic acid copolymer is as follows: basalt fiber: water = 1.4:0.3:1, basalt fibers with the length of 60 mu m;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth C, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber laminated body with required thickness;
(4) Performing hot press molding on the fiber laminated body obtained in the step (3) at 100 ℃ and 0.8Mpa to obtain a reinforced fiber felt D;
(5) Soaking the reinforcing fiber felt D obtained in the step (4) in the silica sol A obtained in the step (1) for 22 hours, and standing and aging at 60 ℃ for 12 h after soaking;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for replacement for 3 times, wherein each replacement time is 15 hours, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
Example 6
The ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating quartz fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silica aerogel.
The preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing isopropyl orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, isopropyl orthosilicate: ethanol: water = 1:9:3, a step of; NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 Isopropyl orthosilicate=0.007:1; ammonia water is added in a molar ratio of NH 3 : isopropyl orthosilicate=0.011: 1, a step of;
(2) Dispersing hot melt adhesive powder polyvinyl alcohol and quartz fibers in water, and uniformly stirring and mixing to obtain viscous slurry B; wherein, the mass ratio is as follows, the hot melt adhesive powder polyvinyl alcohol: quartz fiber: water = 0.9:0.4:1, the length of the quartz fiber is 70 mu m;
(3) Spreading the glass fiber cloth C, brushing the viscous slurry B obtained in the step (2) on the surface of the glass fiber cloth, continuously spreading a layer of glass fiber cloth C, and sequentially spreading the glass fiber cloth C according to the sequence of C-B-C to obtain a fiber laminated body with required thickness;
(4) Performing hot press molding on the fiber laminated body obtained in the step (3) at 120 ℃ and 0.4Mpa to obtain a reinforced fiber felt D;
(5) Impregnating the reinforcing fiber felt D obtained in the step (4) in the silica sol A obtained in the step (1) for 18 hours, and standing and aging for 10 hours at 55 ℃ after impregnation;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for replacement for 2 times, wherein each replacement time is 22 hours, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A ceramic fiber reinforced aerogel blanket, characterized by: the ceramic fiber reinforced aerogel felt comprises a composite reinforced fiber felt body and aerogel, wherein the composite reinforced fiber felt body is obtained by coating ceramic fiber slurry on glass fiber cloth, laminating, and hot-press molding; the aerogel is silicon dioxide aerogel;
the preparation method of the ceramic fiber reinforced aerogel felt comprises the following specific steps:
(1) Mixing orthosilicate, ethanol and water uniformly, and sequentially adding NH 4 F, uniformly stirring the solution and ammonia water to obtain silica sol A; wherein, in terms of mole ratio, the orthosilicate: ethanol: water = 1: (4-12): (2-4); NH (NH) 4 The addition amount of F solution is calculated by mole ratio, NH 4 F: orthosilicate= (0.002-0.01): 1, a step of; the addition amount of ammonia ensures that N is calculated by mole ratioH 3 Orthosilicate= (0.005-0.015): 1, a step of;
(2) Dispersing the hot melt adhesive powder and ceramic fibers in water, and uniformly stirring and mixing to obtain ceramic fiber slurry; wherein, the hot melt adhesive powder comprises the following components in percentage by mass: ceramic fiber: water= (0.5 to 1.5): (0.1-0.5): 1, a step of;
(3) Spreading and placing the glass fiber cloth, brushing the ceramic fiber slurry obtained in the step (2) on the surface of the glass fiber cloth, continuously spreading a layer of glass fiber cloth, and sequentially spreading fiber mat laminated bodies with required thickness according to the sequence of the glass fiber cloth, the ceramic fiber slurry, the glass fiber cloth and the glass fiber cloth;
(4) Performing hot press molding on the fiber felt layer stack body obtained in the step (3) to obtain a reinforced fiber felt D;
(5) Dipping the reinforced fiber mat D obtained in the step (4) in the silica sol A obtained in the step (1), standing and aging for 8-24 h at 30-60 ℃ after dipping;
(6) Placing the fiber felt-gel composite obtained in the step (5) in absolute ethyl alcohol for multiple solvent replacement, and removing redundant water in the fiber felt-gel composite;
(7) And (3) drying the felt body obtained in the step (6) to obtain the prepared ceramic fiber reinforced aerogel felt.
2. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (1), the orthosilicate is one of ethyl orthosilicate, methyl orthosilicate, isopropyl orthosilicate.
3. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (2), the hot melt adhesive powder is one or more of an ethylene vinyl acetate copolymer powder, an ethylene acrylic acid copolymer powder, or a polyvinyl alcohol powder.
4. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (2), the ceramic fibers are one of aluminum silicate fibers, mullite fibers, quartz fibers, alumina fibers, basalt fibers.
5. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (2), the ceramic fibers have a length of 20 to 100 μm.
6. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (3), the ceramic fiber slurry is painted at a thickness of 0.2 to 1mm.
7. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (4), the hot pressing is at a temperature of 80 to 120 ℃ and a pressure of 0.2 to 1 Mpa.
8. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (5), the gum dipping time is 12 to 24 h.
9. The ceramic fiber reinforced aerogel blanket of claim 1, wherein in step (6), the number of solvent substitutions is 2 to 3, each for 12 to 36 hours.
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| CN104478394A (en) * | 2014-11-24 | 2015-04-01 | 天津大学 | Preparation method of fiber felt enhanced silica aerogel composite panel |
| CN210026533U (en) * | 2019-05-08 | 2020-02-07 | 航天海鹰(镇江)特种材料有限公司 | Composite aerogel heat insulation blanket |
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| CN104478394A (en) * | 2014-11-24 | 2015-04-01 | 天津大学 | Preparation method of fiber felt enhanced silica aerogel composite panel |
| CN210026533U (en) * | 2019-05-08 | 2020-02-07 | 航天海鹰(镇江)特种材料有限公司 | Composite aerogel heat insulation blanket |
| CN110922095A (en) * | 2019-11-07 | 2020-03-27 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of composite silica aerogel felt |
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