CN114014633A - Preparation method of aerogel heat insulation felt - Google Patents
Preparation method of aerogel heat insulation felt Download PDFInfo
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- CN114014633A CN114014633A CN202111388254.1A CN202111388254A CN114014633A CN 114014633 A CN114014633 A CN 114014633A CN 202111388254 A CN202111388254 A CN 202111388254A CN 114014633 A CN114014633 A CN 114014633A
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- coupling agent
- silane coupling
- aerogel
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- acetylacetone
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- 239000004964 aerogel Substances 0.000 title claims abstract description 41
- 238000009413 insulation Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 43
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 31
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- SGNLDVYVSFANHW-UHFFFAOYSA-N pentane-2,4-dione;zirconium Chemical compound [Zr].CC(=O)CC(C)=O SGNLDVYVSFANHW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000003605 opacifier Substances 0.000 claims abstract description 8
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 8
- 238000006462 rearrangement reaction Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 13
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000003365 glass fiber Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 5
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002748 Basalt fiber Polymers 0.000 claims description 3
- 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 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- YOBOXHGSEJBUPB-MTOQALJVSA-N (z)-4-hydroxypent-3-en-2-one;zirconium Chemical compound [Zr].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O YOBOXHGSEJBUPB-MTOQALJVSA-N 0.000 description 1
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
- C04B14/064—Silica aerogel
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
- C04B14/42—Glass
-
- 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
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/06—Oxides, Hydroxides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a preparation method of an aerogel heat insulation felt, which comprises the following steps: s1, adding the reinforced fibers into a silane coupling agent solution, stirring for 0.5-2 h, taking out and rinsing, carrying out heat treatment at 100-120 ℃ for 1-5 h, and cooling to room temperature to obtain pretreated reinforced fibers for later use; s2, drying insoluble and infusible polydimethylsiloxane, and heating to 400-450 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use; s3, uniformly mixing an opacifier and the pretreated reinforcing fibers obtained in the step S1, putting the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen to evacuate, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, then preserving the temperature for 1-2 hours, removing carbon at high temperature, taking out the product, and cooling to room temperature to obtain the aerogel heat insulation felt. The method is simple to operate and low in cost, and the prepared aerogel heat insulation felt has good heat insulation performance.
Description
Technical Field
The invention relates to a preparation method of an aerogel heat insulation felt.
Background
The aerogel felt is a flexible heat-insulating felt which is formed by compounding nano silicon dioxide aerogel serving as a main material with fiber felts such as glass fiber cotton or pre-oxidized fiber felt and the like through a special process, is characterized by low heat conductivity coefficient, certain tensile strength and compressive strength, and convenient application of heat-insulating construction, and belongs to heat-insulating materials.
Currently, the aerogel is generally prepared by taking tetraethoxysilane or methyl orthosilicate as a raw material, obtaining gel through a sol-gel method, and then performing a supercritical drying process. The method has the advantages of high price of raw materials, complex preparation process, harsh conditions and high energy consumption, so that the preparation cost of the silicon dioxide aerogel is high, and the preparation method comprises hydrolysis and polycondensation, so that the selection of the preparation conditions and the structural control of the aerogel are quite complex.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an aerogel heat insulation felt, which is simple to operate and low in cost, and the prepared aerogel heat insulation felt has good heat insulation performance.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method of making an aerogel insulation blanket comprising the steps of:
s1, adding the reinforced fibers into a silane coupling agent solution, stirring for 0.5-2 h, taking out and rinsing, carrying out heat treatment at 100-120 ℃ for 1-5 h, and cooling to room temperature to obtain pretreated reinforced fibers for later use;
s2, drying insoluble and infusible polydimethylsiloxane, and heating to 400-450 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing an opacifier and the pretreated reinforcing fibers obtained in the step S1, putting the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen to evacuate, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, then preserving the temperature for 1-2 hours, removing carbon at high temperature, taking out the product, and cooling to room temperature to obtain the aerogel heat insulation felt.
Further, in step S1 of the present invention, the reinforcing fiber is one of basalt fiber, glass fiber, or polycrystalline mullite fiber.
Further, in step S1 of the present invention, the silane coupling agent in the silane coupling agent solution is one of γ -aminopropyltriethoxysilane, γ -glycidoxypropyltrimethoxysilane, and γ -methacryloxypropyltrimethoxysilane,
in step S1, the solvent in the silane coupling agent solution is absolute ethyl alcohol, and the volume ratio of the silane coupling agent to the absolute ethyl alcohol in the silane coupling agent solution is 1 (500-2000).
Further, in step S3, the opacifier is zirconium dioxide with a particle size of 2-5 μm.
In step S3, the mass ratio of the light-screening agent to the pretreated reinforcing fibers to the liquid polycarbosilane to the acetylacetone to the zirconium acetylacetonate is 1:15:37.5 (37.5-56.25): 3.75.
Further, in the step S3, the specific operation of high-temperature carbon removal is to keep the temperature at 500-600 ℃ for 12-18 h.
Compared with the prior art, the invention has the following beneficial effects:
1) the silicon-containing polymer-polydimethylsiloxane is used for preparing the silicon dioxide aerogel by the supercritical method, so that the preparation process is simplified, the preparation speed of the silicon dioxide aerogel is increased, the preparation period is shortened, and the preparation cost can be effectively reduced.
2) According to the invention, zirconium dioxide is used as an opacifier, and the opacifier is doped in the aerogel to play a good infrared shielding role, so that the thermal conductivity of the aerogel thermal insulation felt is reduced, and the thermal insulation performance of the aerogel thermal insulation felt is improved.
3) The invention uses the reinforcing fiber as a reinforcing phase, and the strength of the aerogel can be obviously improved by combining the reinforcing fiber with the silica aerogel.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
An aerogel insulation blanket was prepared according to the following steps:
s1, adding glass fiber into a silane coupling agent solution, stirring for 1 hour, taking out and rinsing, carrying out heat treatment at 120 ℃ for 5 hours, cooling to room temperature to obtain pretreated glass fiber for later use, wherein a silane coupling agent in the silane coupling agent solution is gamma-aminopropyltriethoxysilane, a solvent in the silane coupling agent solution is absolute ethanol, and the volume ratio of the silane coupling agent to the absolute ethanol in the silane coupling agent solution is 1: 1000;
s2, drying insoluble and infusible polydimethylsiloxane, and then heating to 400 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing zirconium dioxide with the particle size of 2-5 microns with the pretreated reinforcing fibers obtained in the step S1, placing the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen into the mold, evacuating, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, keeping the temperature for 1h, keeping the temperature at 550 ℃ for 15h, removing carbon at high temperature, taking out, cooling to room temperature to obtain the aerogel heat insulation felt, wherein the mass ratio of the zirconium dioxide, the pretreated reinforcing fibers, the liquid polycarbosilane, the acetylacetone and the acetylacetone zirconium acetylacetonate is 1:15:37.5:37.5: 3.75.
Example 2
An aerogel insulation blanket was prepared according to the following steps:
s1, adding glass fiber into a silane coupling agent solution, stirring for 0.5h, taking out and rinsing, carrying out heat treatment at 100 ℃ for 4h, cooling to room temperature to obtain pretreated glass fiber for later use, wherein a silane coupling agent in the silane coupling agent solution is gamma-aminopropyl triethoxysilane, a solvent in the silane coupling agent solution is absolute ethanol, and the volume ratio of the silane coupling agent in the silane coupling agent solution to the absolute ethanol is 1: 1500;
s2, drying insoluble and infusible polydimethylsiloxane, and then heating to 425 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing zirconium dioxide with the particle size of 2-5 microns with the pretreated reinforcing fibers obtained in the step S1, placing the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen into the mold, evacuating, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, then preserving heat for 1.5h, preserving heat at 500 ℃ for 18h, removing carbon at high temperature, taking out, cooling to room temperature to obtain the aerogel heat insulation felt, wherein the mass ratio of the zirconium dioxide, the pretreated reinforcing fibers, the liquid polycarbosilane, the acetylacetone and the acetylacetone zirconium acetylacetonate is 1:15:37.5:37.5: 3.75.
Example 3
An aerogel insulation blanket was prepared according to the following steps:
s1, adding glass fiber into a silane coupling agent solution, stirring for 2 hours, taking out and rinsing, carrying out heat treatment at 110 ℃ for 1 hour, cooling to room temperature to obtain pretreated glass fiber for later use, wherein a silane coupling agent in the silane coupling agent solution is gamma-aminopropyltriethoxysilane, a solvent in the silane coupling agent solution is absolute ethanol, and the volume ratio of the silane coupling agent to the absolute ethanol in the silane coupling agent solution is 1: 2000;
s2, drying insoluble and infusible polydimethylsiloxane, and then heating to 450 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing zirconium dioxide with the particle size of 2-5 microns with the pretreated reinforcing fibers obtained in the step S1, placing the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen into the mold, evacuating, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, keeping the temperature for 2h, keeping the temperature at 600 ℃ for 12h, removing carbon, taking out the mixture, cooling to room temperature to obtain the aerogel heat insulation felt, wherein the mass ratio of the zirconium dioxide, the pretreated reinforcing fibers, the liquid polycarbosilane, the acetylacetone and the acetylacetone zirconium acetylacetonate is 1:15:37.5:56.25: 3.75.
Experimental example: test of Heat insulating Property
The thermal conductivity of the aerogel thermal insulation blankets prepared in examples 1-3 were measured using a steady state method. In the steady state method, a heat source is firstly utilized to heat a sample, the temperature difference in the sample leads the heat to be conducted from high temperature to low temperature, and the temperature of each point in the sample changes along with the influence of the heating speed and the heat transfer speed; when the experiment conditions and the experiment parameters are properly controlled to enable the heating and heat transfer processes to reach an equilibrium state, stable temperature distribution can be formed inside the sample to be detected, and the heat conductivity coefficient is calculated according to the temperature distribution.
The lower the thermal conductivity, the better the insulation performance, and the test results are shown in the following table:
| thermal conductivity/W/(m.k), 25 deg.C | |
| Example 1 | 0.02417 |
| Example 2 | 0.02408 |
| Example 3 | 0.02438 |
As can be seen from the above table, the thermal conductivity coefficients of examples 1-3 are all low, indicating that the aerogel thermal insulation blanket prepared by the invention has better thermal insulation performance.
Example 4
An aerogel insulation blanket was prepared according to the following steps:
s1, adding basalt fibers into a silane coupling agent solution, stirring for 1.5h, taking out and rinsing, carrying out heat treatment at 105 ℃ for 3h, cooling to room temperature to obtain pretreated glass fibers for later use, wherein a silane coupling agent in the silane coupling agent solution is gamma-glycidyl ether oxypropyl trimethoxysilane, a solvent in the silane coupling agent solution is absolute ethyl alcohol, and the volume ratio of the silane coupling agent in the silane coupling agent solution to the absolute ethyl alcohol is 1: 500;
s2, drying insoluble and infusible polydimethylsiloxane, and heating to 420 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing zirconium dioxide with the particle size of 2-5 microns with the pretreated reinforcing fibers obtained in the step S1, placing the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen into the mold, evacuating, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, then preserving heat for 1.2h, preserving heat at 520 ℃ for 16h, removing carbon at high temperature, taking out, cooling to room temperature to obtain the aerogel heat insulation felt, wherein the mass ratio of the zirconium dioxide, the pretreated reinforcing fibers, the liquid polycarbosilane, the acetylacetone and the acetylacetone zirconium acetylacetonate is 1:15:37.5:50: 3.75.
Example 5
An aerogel insulation blanket was prepared according to the following steps:
s1, adding polycrystalline mullite fiber into a silane coupling agent solution, stirring for 1.5h, taking out and rinsing, carrying out heat treatment at 115 ℃ for 2h, cooling to room temperature to obtain pretreated glass fiber for later use, wherein a silane coupling agent in the silane coupling agent solution is gamma-methacryloxypropyl trimethoxy silane, a solvent in the silane coupling agent solution is absolute ethyl alcohol, and the volume ratio of the silane coupling agent in the silane coupling agent solution to the absolute ethyl alcohol is 1: 1000;
s2, drying insoluble and infusible polydimethylsiloxane, and then heating to 425 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing zirconium dioxide with the particle size of 2-5 microns with the pretreated reinforcing fibers obtained in the step S1, placing the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen into the mold, evacuating, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, then preserving the temperature for 1.8h, preserving the temperature at 560 ℃ for 14h, removing carbon at high temperature, taking out the mixture, cooling to room temperature to obtain the aerogel heat insulation felt, wherein the mass ratio of the zirconium dioxide, the pretreated reinforcing fibers, the liquid polycarbosilane, the acetylacetone and the acetylacetone zirconium acetylacetonate is 1:15:37.5:40: 3.75.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. A preparation method of aerogel heat insulation felt is characterized by comprising the following steps: the method comprises the following steps:
s1, adding the reinforced fibers into a silane coupling agent solution, stirring for 0.5-2 h, taking out and rinsing, carrying out heat treatment at 100-120 ℃ for 1-5 h, and cooling to room temperature to obtain pretreated reinforced fibers for later use;
s2, drying insoluble and infusible polydimethylsiloxane, and heating to 400-450 ℃ under the protection of nitrogen to perform thermal decomposition rearrangement reaction to obtain liquid polycarbosilane for later use;
s3, uniformly mixing an opacifier and the pretreated reinforcing fibers obtained in the step S1, putting the mixture into a mold, pouring the liquid polycarbosilane obtained in the step S2 into the mold, adding acetylacetone and acetylacetone zirconium into the liquid polycarbosilane, sealing the mold, introducing nitrogen to evacuate, simultaneously adding 50KPa pressure, heating to the supercritical point of the polycarbosilane, then preserving the temperature for 1-2 hours, removing carbon at high temperature, taking out the product, and cooling to room temperature to obtain the aerogel heat insulation felt.
2. The method of making an aerogel thermal insulation blanket of claim 1, wherein: in the step S1, the reinforcing fiber is one of basalt fiber, glass fiber, or polycrystalline mullite fiber.
3. The method of making an aerogel thermal insulation blanket of claim 1, wherein: in the step S1, the silane coupling agent in the silane coupling agent solution is one of γ -aminopropyltriethoxysilane, γ -glycidoxypropyltrimethoxysilane, and γ -methacryloxypropyltrimethoxysilane.
4. The method of making an aerogel thermal insulation blanket of claim 1, wherein: in the step S1, the solvent in the silane coupling agent solution is absolute ethyl alcohol, and the volume ratio of the silane coupling agent in the silane coupling agent solution to the absolute ethyl alcohol is 1 (500-2000).
5. The method of making an aerogel thermal insulation blanket of claim 1, wherein: in the step S3, the opacifier is zirconium dioxide with a particle size of 2-5 μm.
6. The method of making an aerogel thermal insulation blanket of claim 1, wherein: in the step S3, the mass ratio of the opacifier, the pretreated reinforcing fibers, the liquid polycarbosilane, the acetylacetone and the acetylacetone zirconium is 1:15:37.5 (37.5-56.25) to 3.75.
7. The method of making an aerogel thermal insulation blanket of claim 1, wherein: in the step S3, the specific operation of high-temperature carbon removal is to keep the temperature at 500-600 ℃ for 12-18 h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111388254.1A CN114014633A (en) | 2021-11-22 | 2021-11-22 | Preparation method of aerogel heat insulation felt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111388254.1A CN114014633A (en) | 2021-11-22 | 2021-11-22 | Preparation method of aerogel heat insulation felt |
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| CN114014633A true CN114014633A (en) | 2022-02-08 |
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