CN114804927A - Waterproof heat-insulating tile and production process thereof - Google Patents
Waterproof heat-insulating tile and production process thereof Download PDFInfo
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- CN114804927A CN114804927A CN202210562366.2A CN202210562366A CN114804927A CN 114804927 A CN114804927 A CN 114804927A CN 202210562366 A CN202210562366 A CN 202210562366A CN 114804927 A CN114804927 A CN 114804927A
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- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000004964 aerogel Substances 0.000 claims abstract description 57
- 238000009413 insulation Methods 0.000 claims abstract description 39
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 10
- 238000000352 supercritical drying Methods 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 5
- 239000000835 fiber Substances 0.000 claims description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 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 24
- 229910052863 mullite Inorganic materials 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 229920000742 Cotton Polymers 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000499 gel Substances 0.000 claims description 10
- 239000011268 mixed slurry Substances 0.000 claims description 10
- 229920002472 Starch Polymers 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 235000019698 starch Nutrition 0.000 claims description 9
- 239000008107 starch Substances 0.000 claims description 9
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910052580 B4C Inorganic materials 0.000 claims description 5
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 5
- 239000000411 inducer Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000013112 stability test Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000004753 textile Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000011240 wet gel Substances 0.000 claims description 5
- 238000012512 characterization method Methods 0.000 claims description 4
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 3
- 159000000013 aluminium salts Chemical class 0.000 claims description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 2
- 238000004581 coalescence Methods 0.000 claims 1
- 230000001419 dependent effect Effects 0.000 claims 1
- 230000006835 compression Effects 0.000 abstract description 5
- 238000007906 compression Methods 0.000 abstract description 5
- 238000003980 solgel method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 15
- 238000001816 cooling Methods 0.000 description 7
- 238000011056 performance test Methods 0.000 description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 239000011810 insulating material Substances 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 229940063656 aluminum chloride Drugs 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- 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
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention relates to the technical field of heat insulation tiles, in particular to a waterproof heat insulation tile which comprises a tile body layer, wherein an aerogel layer is arranged on the outer surface of the tile body layer, and a ceramic layer is arranged on the outer surface of the aerogel layer. The invention takes a high-temperature heat-insulating tile as a framework, alumina sol prepared by a sol-gel process is dipped in the heat-insulating tile in vacuum, and the air-gel composite high-temperature heat-insulating tile is prepared by the steps of gelling, aging, supercritical drying and the like, thereby representing the microstructure of the air-gel composite high-temperature heat-insulating tile after being processed at different temperatures, analyzing the heat-insulating property through high-temperature heat conductivity and a back temperature curve, and testing the mechanical property after being processed at different temperatures and the compression strength at high temperature.
Description
Technical Field
The invention relates to the technical field of heat insulation tiles, in particular to a waterproof heat insulation tile and a production process thereof.
Background
The heat insulating tile is also called as heat eliminating tile, the first main material of the heat insulating tile is aluminum, and with the development of science and technology, a novel magnesium cementing material heat insulating tile is attracted by people. The heat conductivity coefficient of the heat insulation tile is as low as 0.169W/mk, the fire-retardant rating reaches B1 level of a non-combustible material, the transverse rupture strength reaches 3754N/m, the longitudinal rupture strength reaches 399N, and the heat insulation tile is a relatively ideal novel building material;
the heat insulation tile in the existing market can not realize heat insulation, and meanwhile, the waterproof function is improved, and the structural stability of the heat insulation tile is not enough.
Disclosure of Invention
The invention aims to solve the defects that the waterproof function cannot be improved while heat insulation is realized and the structural stability of a heat insulation tile is insufficient in the prior art, and provides a waterproof heat insulation tile and a production process thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the design is a waterproof and heat-insulating tile, which comprises a tile body layer, wherein an aerogel layer is arranged on the outer surface of the tile body layer, and a ceramic layer is arranged on the outer surface of the aerogel layer.
Preferably, the outer surface of the ceramic layer is arranged in a loose and porous manner.
Preferably, the aerogel layer is specifically an aerogel layer and specifically an alumina aerogel layer.
The invention also provides a preparation process of the waterproof heat-insulation tile, which comprises the following steps:
s, selecting the raw materials of the aerogel layer according to the parts by weight: 160 parts of mullite fiber loose cotton 115-55 parts, 40-55 parts of aluminum chloride hexahydrate, 41-66 parts of propylene oxide, 33-43 parts of absolute ethyl alcohol and 25-50 parts of deionized water;
s2, adding mullite fiber loose cotton and a certain amount of sintering aid into water, stirring uniformly to prepare a slurry solution, and pouring the slurry solution into a mould for suction filtration molding; drying the wet blank at the temperature of 100-1600 ℃, carrying out heat treatment at the temperature of 1500-1600 ℃ for 1-2h to obtain a high-temperature heat insulation tile, wherein the porosity is about 85% -87%, the use temperature is 1400-1600 ℃, aluminium trichloride hexahydrate is used as a precursor, is prepared into a solution with deionized water and absolute ethyl alcohol, the solution is fully stirred to dissolve aluminium salt, after a colorless transparent solution is formed, propylene oxide in a certain proportion is added as a gel network inducer, and the solution is fully stirred for 15-30min to obtain alumina sol;
s3, introducing alumina sol into the high-temperature heat-insulating tile by a vacuum impregnation method, and sealing and standing to form gel; adding absolute ethyl alcohol to fully soak the tile body layer, aging for 2-5 days at room temperature, performing absolute ethyl alcohol solvent replacement on the wet gel for multiple times, and finally placing the sample into a high-pressure kettle, and performing supercritical drying by taking the ethyl alcohol as a drying medium to prepare the alumina aerogel composite high-temperature heat-insulation tile;
s4, the ceramic fibers can be mutually overlapped by utilizing the textile characteristics or the fineness of the ceramic fibers, and a three-dimensional hole structure is formed by the method, the dispersibility of the fibers in the slurry directly depends on the length of the chopped fibers, the shorter the length of the fibers is, the better the dispersibility in the slurry is, and the better the uniformity in the manufactured blank is, but the chopped fibers are overlapped to form a porous reticular framework in the material, and the too short fibers cannot form a framework structure, so that the material density is too high, and the heat insulation performance is reduced;
repeatedly rinsing the cut mullite chopped fibers in a hydrochloric acid solution with the pH value equal to 3 and deionized water until the pH value of the mullite chopped fibers is 7, washing fiber balls in the chopped fibers, and then respectively adding a dispersant polyacrylamide, soluble starch, boron carbide and silicon carbide;
placing the mixed slurry into a stirrer to be stirred for 100min by strong force, fully and uniformly mixing, then pouring the mixed slurry into a special mould, wherein the bottom of the mould is distributed with fine holes with the diameter of 4mm, a fine mesh screen with 100 meshes is covered on the fine holes, a pressure head is placed at the upper part of the mould, a certain pressure is applied on the pressure head, so that the moisture in the slurry is rapidly discharged through the mesh screen and the fine holes, and the pressure is kept for 110 min;
and S5, detecting.
Preferably, the wet blank demoulded in the step S4 still has certain moisture, and needs to be dried overnight in a drying oven at 70 ℃ to ensure that the moisture in the wet blank is fully volatilized, then sintering can be carried out, the temperature is kept for two hours under the air to ensure that the starch used as the temporary bonding agent is completely oxidized and disappears, then the temperature is raised to 1200 ℃ at a temperature rise speed of 5 ℃/min, the temperature is kept for two hours, and then the material is cooled along with the oven, so that the mullite-based porous rigid heat-insulating material can be obtained.
Preferably, the S5 detecting step specifically includes a performance characterization test and a thermal stability test, wherein the performance characterization test includes thermal stability and mechanical properties after heat treatment, and the sample is treated at 1000-1400 ℃, and the treatment method includes: heating the sample along with the furnace, wherein the heating rate is 3 ℃/min, keeping the temperature for 30min after the temperature is raised to the specified temperature, and opening the furnace door to take out the sample; wherein, the sample after heat preservation for 30min at 1400 ℃ adopts a furnace cooling mode due to higher temperature.
Preferably, after the heat insulation tile is subjected to heat preservation at 1200 ℃ for 30min, the shrinkage of the heat insulation tile in the thickness direction is observed, and in an original state, the size of holes formed by uniformly filling the aerogel in gaps among the fibers of the heat insulation tile is obviously reduced; the aerogel is observed to have typical nanoparticle and nano-pore structures, and secondly, the phenomenon that crystal grains are fused and grown up is observed along with the increase of the heat treatment temperature.
The waterproof heat insulation tile and the production process thereof have the beneficial effects that: the waterproof heat-insulating tile and the production process thereof are characterized in that the high-temperature heat-insulating tile is used as a framework, alumina sol prepared by a sol-gel process is soaked in vacuum into the heat-insulating tile, and the aerogel composite high-temperature heat-insulating tile is prepared by the steps of gelling, aging, supercritical drying and the like, the microstructure of the aerogel composite high-temperature heat-insulating tile is characterized after the heat-insulating tile is processed at different temperatures, the heat-insulating property is analyzed through high-temperature heat conductivity and a back temperature curve, and the mechanical property and the compression strength at high temperature after the heat-insulating tile is processed at different temperatures are tested.
Drawings
Fig. 1 is a schematic structural view of a waterproof and heat-insulating tile and a production process thereof.
In the figure: ceramic layer 1, aerogel layer 2, tile body layer 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
Referring to fig. 1, a waterproof and heat-insulating tile comprises a tile body layer 3, an aerogel layer 2 is arranged on the outer surface of the tile body layer 3, a ceramic layer 1 is arranged on the outer surface of the aerogel layer 2, the outer surface of the ceramic layer 1 is porous, the aerogel layer 2 is specifically an aerogel layer 2 and is specifically an alumina aerogel layer,
the invention also provides a preparation process of the waterproof heat-insulation tile, which comprises the following steps:
s1, selecting the raw materials of the aerogel layer 2 according to the parts by weight: 115 parts of mullite fiber loose cotton, 40 parts of hexahydrated aluminum chloride, 41 parts of propylene oxide, 33 parts of absolute ethyl alcohol and 25 parts of deionized water;
s2, adding mullite fiber loose cotton and a certain amount of sintering aid into water, stirring uniformly to prepare a slurry solution, and pouring the slurry solution into a mould for suction filtration molding; drying the wet blank at 100 ℃, carrying out heat treatment at 1500 ℃ for 1h to obtain a high-temperature heat insulation tile, wherein the porosity is about 85%, the use temperature is 1400 ℃, adopting aluminum trichloride hexahydrate as a precursor, preparing a solution with deionized water and absolute ethyl alcohol, fully stirring to dissolve aluminum salt, adding a certain proportion of propylene oxide as a gel network inducer after forming a colorless transparent solution, and fully stirring for 15min to obtain alumina sol;
s3, introducing alumina sol into the high-temperature heat-insulating tile by a vacuum impregnation method, and sealing and standing to form gel; adding absolute ethyl alcohol to fully soak the tile body layer 3, aging for 2d at room temperature, performing absolute ethyl alcohol solvent replacement on the wet gel for multiple times, and finally placing the sample into a high-pressure kettle, and performing supercritical drying by taking the ethyl alcohol as a drying medium to prepare the alumina aerogel composite high-temperature heat-insulating tile;
s4, utilizing the textile characteristics or the fine shape of the ceramic fibers to enable the ceramic fibers to be mutually overlapped and form a three-dimensional pore structure, wherein the dispersibility of the fibers in the slurry directly depends on the length of the chopped fibers, the shorter the length of the fibers is, the better the dispersibility in the slurry is, and the better the uniformity in the prepared blank is, but the chopped fibers are overlapped to form a porous reticular framework in the material, and the too short fibers cannot form a framework structure, so that the material density is too high, and the heat insulation performance is reduced;
repeatedly rinsing the cut mullite chopped fibers in a hydrochloric acid solution with the pH value equal to 3 and deionized water until the pH value of the mullite chopped fibers is 7, washing fiber balls in the chopped fibers, and then respectively adding a dispersant polyacrylamide, soluble starch, boron carbide and silicon carbide;
the mixed slurry is put into a stirrer to be strongly stirred for 100min so as to be fully and uniformly mixed, then pouring the mixed slurry into a special mould, wherein the bottom of the mould is distributed with fine holes with the diameter of 4mm, and a fine mesh screen with 100 meshes is covered on the fine holes, a pressure head is arranged on the upper part of the mould, and certain pressure is applied on the pressure head, so that the water in the slurry is rapidly discharged through the mesh screen and the fine holes, keeping the pressure for 110min, drying the demoulded wet blank at 70 ℃ overnight in a drying oven to ensure that the moisture in the demoulded wet blank is fully volatilized, then sintering the blank, the process is carried out in the air, the temperature is kept for two hours, the starch used as the temporary adhesive is ensured to be completely oxidized and disappear, then raising the temperature to 1200 ℃ at the temperature rise speed of 5 ℃/min, preserving the heat for two hours, and then cooling the material along with the furnace to obtain the mullite-based porous rigid heat-insulating material;
s5, detection, wherein the detection step specifically comprises a characteristic performance test and a thermal stability test, the characteristic performance test comprises thermal stability and mechanical property after heat treatment, the sample is treated at 1000 ℃, and the treatment mode is as follows: heating the sample along with the furnace, wherein the heating rate is 3 ℃/min, keeping the temperature for 30min after the temperature is raised to the specified temperature, and opening the furnace door to take out the sample; wherein, the sample after heat preservation for 30min at 1400 ℃ adopts a furnace cooling mode due to higher temperature.
Observing the shrinkage of the heat insulation tile in the thickness direction after the heat insulation tile is insulated at 1200 ℃ for 30min, wherein in the original state, the size of the holes of the aerogel uniformly filled in the gaps among the fibers of the heat insulation tile is obviously reduced; observing that the aerogel has typical nano-particle and nano-pore structures, and observing that the aerogel generates the phenomena of grain fusion and growth along with the rise of the heat treatment temperature;
the alumina sol prepared by the sol-gel process is vacuum-dipped into the heat-insulating tile by taking the high-temperature heat-insulating tile as a framework, and then the alumina sol is subjected to gelling, aging, supercritical drying and other steps to prepare the aerogel composite high-temperature heat-insulating tile, so that the microstructure of the aerogel composite high-temperature heat-insulating tile after different temperature treatment is represented, the heat-insulating property is analyzed through high-temperature heat conductivity and a back temperature curve, and the mechanical property after different temperature treatment and the compression strength at high temperature are tested.
Example 2
Referring to fig. 1, the difference between this embodiment and embodiment 1 is that the waterproof and heat insulating tile comprises a tile body layer 3, an aerogel layer 2 is disposed on the outer surface of the tile body layer 3, a ceramic layer 1 is disposed on the outer surface of the aerogel layer 2, the outer surface of the ceramic layer 1 is porous, the aerogel layer 2 is specifically an alumina aerogel layer,
the invention also provides a preparation process of the waterproof heat-insulation tile, which comprises the following steps:
s1, selecting the raw materials of the aerogel layer 2 according to the parts by weight: 130 parts of mullite fiber loose cotton, 48 parts of hexahydrated aluminum chloride, 55 parts of propylene oxide, 37 parts of absolute ethyl alcohol and 34 parts of deionized water;
s2, adding mullite fiber loose cotton and a certain amount of sintering aid into water, stirring uniformly to prepare a slurry solution, and pouring the slurry solution into a mould for suction filtration molding; drying the wet blank at 110 ℃, carrying out heat treatment at 1550 ℃ for 1-2h to obtain a high-temperature heat-insulating tile, wherein the porosity of the tile is about 86%, the use temperature is 1500 ℃, adopting aluminum trichloride hexahydrate as a precursor, preparing a solution with deionized water and absolute ethyl alcohol, fully stirring to dissolve aluminum salt, adding a certain proportion of propylene oxide as a gel network inducer after a colorless transparent solution is formed, and fully stirring for 22min to obtain alumina sol;
s3, introducing alumina sol into the high-temperature heat-insulating tile by a vacuum impregnation method, and sealing and standing to form gel; adding absolute ethyl alcohol to fully soak the tile body layer 3, aging for 3d at room temperature, performing absolute ethyl alcohol solvent replacement on the wet gel for multiple times, and finally placing the sample into a high-pressure kettle, and performing supercritical drying by taking the ethyl alcohol as a drying medium to prepare the alumina aerogel composite high-temperature heat-insulating tile;
s4, utilizing the textile characteristics or the fine shape of the ceramic fibers to enable the ceramic fibers to be mutually overlapped and form a three-dimensional pore structure, wherein the dispersibility of the fibers in the slurry directly depends on the length of the chopped fibers, the shorter the length of the fibers is, the better the dispersibility in the slurry is, and the better the uniformity in the prepared blank is, but the chopped fibers are overlapped to form a porous reticular framework in the material, and the too short fibers cannot form a framework structure, so that the material density is too high, and the heat insulation performance is reduced;
repeatedly rinsing the cut mullite chopped fibers in a hydrochloric acid solution with the pH value equal to 3 and deionized water until the pH value of the mullite chopped fibers is 7, washing fiber balls in the chopped fibers, and then respectively adding a dispersant polyacrylamide, soluble starch, boron carbide and silicon carbide;
the mixed slurry is put into a stirrer to be strongly stirred for 100min so as to be fully and uniformly mixed, then pouring the mixed slurry into a special mould, wherein the bottom of the mould is distributed with fine holes with the diameter of 4mm, and a fine mesh screen with 100 meshes is covered on the fine holes, a pressure head is arranged on the upper part of the mould, and certain pressure is applied on the pressure head, so that the water in the slurry is rapidly discharged through the mesh screen and the fine holes, keeping the pressure for 110min, drying the demoulded wet blank at 70 ℃ overnight in a drying oven to ensure that the moisture in the demoulded wet blank is fully volatilized, then sintering the blank, the process is carried out in the air, the temperature is kept for two hours, the starch used as the temporary adhesive is ensured to be completely oxidized and disappear, then raising the temperature to 1200 ℃ at the temperature rise speed of 5 ℃/min, preserving the heat for two hours, and then cooling the material along with the furnace to obtain the mullite-based porous rigid heat-insulating material;
s5, detecting, wherein the detecting step specifically comprises a characteristic performance test and a thermal stability test, the characteristic performance test comprises thermal stability and mechanical property after heat treatment, the sample is treated at 1200 ℃, and the treatment mode is as follows: heating the sample along with the furnace, wherein the heating rate is 3 ℃/min, keeping the temperature for 30min after the temperature is raised to the specified temperature, and opening the furnace door to take out the sample; wherein, the sample after heat preservation for 30min at 1400 ℃ adopts a furnace cooling mode due to higher temperature.
Observing the shrinkage of the heat insulation tile in the thickness direction after the heat insulation tile is insulated at 1200 ℃ for 30min, wherein in the original state, the size of the holes of the aerogel uniformly filled in the gaps among the fibers of the heat insulation tile is obviously reduced; observing that the aerogel has typical nano-particle and nano-pore structures, and observing that the aerogel generates the phenomena of grain fusion and growth along with the rise of the heat treatment temperature;
the alumina sol prepared by the sol-gel process is vacuum-dipped into the heat-insulating tile by taking the high-temperature heat-insulating tile as a framework, and then the alumina sol is subjected to gelling, aging, supercritical drying and other steps to prepare the aerogel composite high-temperature heat-insulating tile, so that the microstructure of the aerogel composite high-temperature heat-insulating tile after different temperature treatment is represented, the heat-insulating property is analyzed through high-temperature heat conductivity and a back temperature curve, and the mechanical property after different temperature treatment and the compression strength at high temperature are tested.
Example 3
Referring to fig. 1, the difference between this embodiment and embodiments 1 and 2 is that the waterproof and heat insulating tile includes a tile body layer 3, an aerogel layer 2 is disposed on the outer surface of the tile body layer 3, a ceramic layer 1 is disposed on the outer surface of the aerogel layer 2, the outer surface of the ceramic layer 1 is porous, the aerogel layer 2 is specifically an alumina aerogel layer,
the invention also provides a preparation process of the waterproof heat-insulation tile, which comprises the following steps:
s1, selecting the raw materials of the aerogel layer 2 according to the parts by weight: 160 parts of mullite fiber loose cotton, 55 parts of aluminum chloride hexahydrate, 66 parts of propylene oxide, 43 parts of absolute ethyl alcohol and 50 parts of deionized water;
s2, adding mullite fiber loose cotton and a certain amount of sintering aid into water, stirring uniformly to prepare a slurry solution, and pouring the slurry solution into a mould for suction filtration molding; drying the wet blank at 120 ℃, carrying out heat treatment at 1600 ℃ for 2h to obtain a high-temperature heat insulation tile, wherein the porosity is about 87%, the use temperature is 1600 ℃, adopting aluminum trichloride hexahydrate as a precursor, preparing a solution with deionized water and absolute ethyl alcohol, fully stirring to dissolve aluminum salt, adding a certain proportion of propylene oxide as a gel network inducer after forming a colorless transparent solution, and fully stirring for 30min to obtain alumina sol;
s3, introducing alumina sol into the high-temperature heat-insulating tile by a vacuum impregnation method, and sealing and standing to form gel; adding absolute ethyl alcohol to fully soak the tile body layer 3, aging for 5d at room temperature, performing absolute ethyl alcohol solvent replacement on the wet gel for multiple times, and finally placing the sample into a high-pressure kettle, and performing supercritical drying by taking the ethyl alcohol as a drying medium to prepare the alumina aerogel composite high-temperature heat-insulating tile;
s4, utilizing the textile characteristics or the fine shape of the ceramic fibers to enable the ceramic fibers to be mutually overlapped and form a three-dimensional pore structure, wherein the dispersibility of the fibers in the slurry directly depends on the length of the chopped fibers, the shorter the length of the fibers is, the better the dispersibility in the slurry is, and the better the uniformity in the prepared blank is, but the chopped fibers are overlapped to form a porous reticular framework in the material, and the too short fibers cannot form a framework structure, so that the material density is too high, and the heat insulation performance is reduced;
repeatedly rinsing the cut mullite chopped fibers in a hydrochloric acid solution with the pH value equal to 3 and deionized water until the pH value of the mullite chopped fibers is 7, washing fiber balls in the chopped fibers, and then respectively adding a dispersant polyacrylamide, soluble starch, boron carbide and silicon carbide;
the mixed slurry is put into a stirrer to be strongly stirred for 100min so as to be fully and uniformly mixed, then pouring the mixed slurry into a special mould, wherein the bottom of the mould is distributed with fine holes with the diameter of 4mm, and a fine mesh screen with 100 meshes is covered on the fine holes, a pressure head is arranged on the upper part of the mould, and certain pressure is applied on the pressure head, so that the water in the slurry is rapidly discharged through the mesh screen and the fine holes, keeping the pressure for 110min, drying the demoulded wet blank at 70 ℃ overnight in a drying oven to ensure that the moisture in the demoulded wet blank is fully volatilized, then sintering the blank, the process is carried out in the air, the temperature is kept for two hours, the starch used as the temporary adhesive is ensured to be completely oxidized and disappear, then raising the temperature to 1200 ℃ at the temperature rise speed of 5 ℃/min, preserving the heat for two hours, and then cooling the material along with the furnace to obtain the mullite-based porous rigid heat-insulating material;
s5, detection, wherein the detection step specifically comprises a characteristic performance test and a thermal stability test, the characteristic performance test comprises thermal stability and mechanical property after heat treatment, the sample is treated at 1400 ℃, and the treatment mode is as follows: heating the sample along with the furnace, wherein the heating rate is 3 ℃/min, keeping the temperature for 30min after the temperature is raised to the specified temperature, and opening the furnace door to take out the sample; wherein, the sample after heat preservation for 30min at 1400 ℃ adopts a furnace cooling mode due to higher temperature.
Observing the shrinkage of the heat insulation tile in the thickness direction after the heat insulation tile is insulated for 30min at 1200 ℃, wherein in the original state, the size of the holes formed by uniformly filling the aerogel in the gaps among the fibers of the heat insulation tile is obviously reduced; observing that the aerogel has typical nano-particle and nano-pore structures, and observing that the aerogel generates the phenomena of grain fusion and growth along with the rise of the heat treatment temperature;
the alumina sol prepared by the sol-gel process is vacuum-dipped into the heat-insulating tile by taking the high-temperature heat-insulating tile as a framework, and then the alumina sol is subjected to gelling, aging, supercritical drying and other steps to prepare the aerogel composite high-temperature heat-insulating tile, so that the microstructure of the aerogel composite high-temperature heat-insulating tile after different temperature treatment is represented, the heat-insulating property is analyzed through high-temperature heat conductivity and a back temperature curve, and the mechanical property after different temperature treatment and the compression strength at high temperature are tested.
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 (7)
1. The utility model provides a waterproof thermal-insulated tile, includes tile body layer (3), its characterized in that, the surface of tile body layer (3) is provided with aerogel layer (2), the surface of aerogel layer (2) is provided with ceramic layer (1).
2. The tile according to claim 1, characterized in that the outer surface of said ceramic layer (1) is porous.
3. The tile according to claim 2, characterized in that said aerogel layer (2), in particular aerogel layer (2), is an alumina aerogel layer.
4. A process for the preparation of a waterproof and insulating tile according to any one of claims 1 to 3, characterized in that it comprises the following steps:
s1, selecting the raw materials of the aerogel layer (2) according to the parts by weight: 160 parts of mullite fiber loose cotton 115-55 parts, 40-55 parts of aluminum chloride hexahydrate, 41-66 parts of propylene oxide, 33-43 parts of absolute ethyl alcohol and 25-50 parts of deionized water;
s2, adding mullite fiber loose cotton and a certain amount of sintering aid into water, stirring uniformly to prepare a slurry solution, and pouring the slurry solution into a mould for suction filtration molding; drying the wet blank at the temperature of 100-1600 ℃, carrying out heat treatment at the temperature of 1500-1600 ℃ for 1-2h to obtain a high-temperature heat insulation tile, wherein the porosity is about 85% -87%, the use temperature is 1400-1600 ℃, aluminium trichloride hexahydrate is used as a precursor, is prepared into a solution with deionized water and absolute ethyl alcohol, the solution is fully stirred to dissolve aluminium salt, after a colorless transparent solution is formed, propylene oxide in a certain proportion is added as a gel network inducer, and the solution is fully stirred for 15-30min to obtain alumina sol;
s3, introducing alumina sol into the high-temperature heat-insulating tile by a vacuum impregnation method, and sealing and standing to form gel; then adding absolute ethyl alcohol to fully soak the tile body layer (3), aging for 2-5d at room temperature, then carrying out absolute ethyl alcohol solvent replacement on the wet gel for multiple times, finally placing the sample into a high-pressure kettle, and carrying out supercritical drying by taking ethyl alcohol as a drying medium to prepare the alumina aerogel composite high-temperature heat-insulating tile;
s4, utilizing the textile characteristics or the fine morphology of the ceramic fibers, the dispersibility of the fibers in the slurry is directly dependent on the length of the chopped fibers, and the shorter the length of the fibers is, the better the dispersibility in the slurry is;
repeatedly rinsing the cut mullite chopped fibers in a hydrochloric acid solution with the pH value equal to 3 and deionized water until the pH value of the mullite chopped fibers is 7, washing fiber balls in the chopped fibers, and then respectively adding a dispersant polyacrylamide, soluble starch, boron carbide and silicon carbide;
placing the mixed slurry into a stirrer, stirring for 100min, pouring the mixed slurry into a special mould, wherein the bottom of the mould is distributed with fine holes with the diameter of 4mm, the fine holes are covered with a fine mesh screen with the size of 100 meshes, and a pressure head is placed at the upper part of the mould;
and S5, detecting.
5. The process for preparing a waterproof and heat-insulating tile according to claim 4, wherein the wet green tile demoulded in step S4 still has a certain moisture, and is dried overnight in a drying oven at 70 ℃ to ensure that the moisture is sufficiently volatilized, and then the green tile is sintered and is subjected to heat preservation in air for two hours.
6. The preparation process of the waterproof and heat-insulating tile as claimed in claim 4, wherein the step of S5 detection specifically comprises a performance characterization test and a thermal stability test, wherein the performance characterization test comprises the thermal stability and a mechanical property after heat treatment, and the sample is treated at 1000 ℃ and 1400 ℃ in the following way: the temperature of the sample is increased along with the furnace, the temperature increasing rate is 3 ℃/min, and the temperature is maintained for 30min after the temperature is increased to the specified temperature.
7. The process for preparing a waterproof and heat-insulating tile according to claim 4, wherein the shrinkage in the thickness direction of the tile is observed after the tile is kept at 1200 ℃ for 30min,
in the original state, the size of the pores uniformly filled in the gaps among the fibers of the heat insulation tile is obviously reduced; the aerogel was observed to have typical nanoparticle and nanoporous structures, and secondly, the phenomenon of grain coalescence and growth of the aerogel was observed as the heat treatment temperature increased.
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