CN119263794A - Composite heat insulation material of ceramic fiber and aerogel and preparation method thereof - Google Patents
Composite heat insulation material of ceramic fiber and aerogel and preparation method thereof Download PDFInfo
- Publication number
- CN119263794A CN119263794A CN202411795745.1A CN202411795745A CN119263794A CN 119263794 A CN119263794 A CN 119263794A CN 202411795745 A CN202411795745 A CN 202411795745A CN 119263794 A CN119263794 A CN 119263794A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- aerogel
- preparing
- treatment
- composite heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004964 aerogel Substances 0.000 title claims abstract description 115
- 239000000835 fiber Substances 0.000 title claims abstract description 103
- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 239000012774 insulation material Substances 0.000 title claims abstract description 50
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 103
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 80
- 238000011282 treatment Methods 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 239000000725 suspension Substances 0.000 claims abstract description 28
- 239000010439 graphite Substances 0.000 claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000352 supercritical drying Methods 0.000 claims abstract description 10
- 238000013329 compounding Methods 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 6
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 55
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 43
- 239000011810 insulating material Substances 0.000 claims description 38
- 239000000377 silicon dioxide Substances 0.000 claims description 33
- 235000012239 silicon dioxide Nutrition 0.000 claims description 31
- 238000010992 reflux Methods 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000011221 initial treatment Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 7
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 4
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 14
- 239000010703 silicon Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000009413 insulation Methods 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 230000035939 shock Effects 0.000 description 6
- 238000005470 impregnation Methods 0.000 description 5
- 125000003636 chemical group Chemical group 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000004965 Silica aerogel Substances 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- -1 aminopropyl Chemical group 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Landscapes
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a composite heat insulation material of ceramic fiber and aerogel and a preparation method thereof, belonging to the technical field of composite heat insulation materials, wherein the preparation method comprises the following steps of preparing a primary aerogel solution, preparing a secondary aerogel solution, preparing a modified silicon carbide whisker suspension by secondary treatment, and compounding; the preparation method of the primary aerogel solution comprises the following steps of preparing coated graphite, mixing, compounding, completely soaking a silicon carbide fiber felt subjected to secondary treatment in a modified silicon carbide whisker suspension in an argon atmosphere, standing at 55-60 ℃, adding into a high-pressure reaction kettle, performing supercritical drying by using carbon dioxide, and finally adding into a tubular furnace for high-temperature treatment to obtain the composite heat insulation material.
Description
Technical Field
The invention relates to the technical field of composite heat insulation materials, in particular to a composite heat insulation material of ceramic fibers and aerogel and a preparation method thereof.
Background
The heat insulating material is a material capable of retarding heat flow transmission, and is also called as a heat insulating material. The traditional heat insulation materials mainly comprise glass fiber, asbestos, rock wool, silicate and the like, and the novel heat insulation materials mainly comprise aerogel, vacuum heat insulation materials and the like. The most commonly used heat insulation material at present is aerogel, the aerogel is a nanoscale porous solid material formed by replacing liquid phase in gel with gas in a certain drying mode through a sol-gel method, and the heat insulation material has high porosity and low density, so that the heat insulation material has excellent heat insulation performance. Aerogels are mainly classified into silica-based aerogels, carbon-based aerogels, sulfur-based aerogels, metal oxide-based aerogels, metal-based aerogels, etc., wherein the most commonly used aerogels are silica-based aerogels.
However, in the use of the silicon aerogel, the problems are that firstly, the silicon aerogel is poor in hydrophobicity and easy to absorb moisture, the heat insulation performance is greatly reduced after moisture absorption, the application of the silicon aerogel in a humid environment is limited, secondly, the silicon aerogel is small in toughness and poor in mechanical property, the application effect of the silicon aerogel is affected, and thirdly, because the silicon aerogel is of a porous structure, the internal particles are fine, the particles of the silicon aerogel are easy to fall off in use, and the durability of the silicon aerogel is affected.
In order to solve the above problems, the inventors tried to compound ceramic fibers with silica aerogel, specifically, add ceramic fiber mat into silica aerogel solution for impregnation, curing and drying, to prepare composite thermal insulation material, and since ceramic fiber mat has good hydrophobicity and large toughness, the hydrophobicity and toughness of the prepared composite thermal insulation material are improved, and in addition, ceramic fiber mat can also play a role of fixing particles in silica aerogel, thereby improving durability of composite thermal insulation material. However, the prepared composite heat insulation material has the problems that firstly, when ceramic fiber felt is added into a silicon aerogel solution for impregnation, the impregnation is uneven, so that the prepared composite heat insulation material has uneven performance, particularly the hydrophobicity and heat insulation performance of the prepared composite heat insulation material are uneven, secondly, a large amount of hydroxyl groups still exist on the surface of the prepared composite heat insulation material after the ceramic fiber and the silicon aerogel are compounded, so that the hydrophobicity of the prepared composite heat insulation material is general, thirdly, the problem that the interaction force between the ceramic fiber felt and the silicon aerogel is small, and the interaction force is easy to be influenced by temperature, so that the thermal shock resistance of the prepared composite heat insulation material is poor.
In order to solve the problems, the existing method mainly comprises the steps of respectively carrying out chemical modification on the ceramic fiber felt and the silicon aerogel, respectively introducing different chemical groups into the ceramic fiber felt and the silicon aerogel, so that uniform impregnation is realized through non-covalent bonds between the different chemical groups, the interaction force between the ceramic fiber felt and the silicon aerogel is improved, and in addition, the hydrophobicity of the composite heat insulation material can be improved through introducing the chemical groups with strong hydrophobicity. However, the introduced chemical groups have poor high temperature resistance and are easy to decompose at high temperature, so that the high temperature resistance of the prepared composite heat insulation material is affected.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the composite heat-insulating material of the ceramic fiber and the aerogel and the preparation method thereof, and the prepared composite heat-insulating material has good heat insulation, hydrophobicity, toughness and durability, uniform performance and good thermal shock resistance and high temperature resistance.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
The preparation method of the composite heat insulation material of the ceramic fiber and the aerogel comprises the following steps of preparing a primary aerogel solution, preparing a secondary aerogel solution through primary treatment, preparing a modified silicon carbide whisker suspension through secondary treatment, and compounding;
the preparation of the primary aerogel solution comprises the steps of preparing coated graphite and mixing;
Mixing silica sol and gamma-aminopropyl triethoxysilane, stirring and refluxing at a stirring speed of 400-600rpm for 5-6 hours at 40-45 ℃, adding graphite powder, continuously stirring and refluxing for 1-1.5 hours, centrifuging, controlling the centrifuging speed at 6000-7000rpm for 5-6 minutes, cleaning the precipitate with deionized water for 3-4 times, and drying to obtain coated graphite;
in the preparation of the coated graphite, the volume mass ratio of the silica sol, the gamma-aminopropyl triethoxysilane and the graphite powder is 200-210mL:6-7mL:34-36g;
The particle size of the graphite powder is 50 mu m;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
Mixing, namely mixing silica sol and gamma-aminopropyl triethoxysilane, stirring and refluxing at a stirring speed of 400-600rpm for 5-6 hours at a temperature of 40-45 ℃, adding coated graphite and nickel sulfate, and continuously stirring and refluxing for 50-60 minutes to obtain a primary aerogel solution;
In the mixing, the volume mass ratio of the silica sol to the gamma-aminopropyl triethoxysilane to the coated graphite to the nickel sulfate is 2000-210ml:60-70 ml:50-55g:15-16g;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
adding the silicon carbide fiber felt into a mould, adding the mould into a vacuum device, adding the primary aerogel solution, ensuring that the silicon carbide fiber felt can be completely immersed in the primary aerogel solution and kept stand in vacuum;
in the primary treatment, the vacuum degree of the vacuum tank is 100-200Pa during vacuum standing, and the time of vacuum standing is 30-40min;
The temperature of the oven is 100-110 ℃ during the heat treatment, and the heat treatment time is 18-20h;
the high-temperature treatment is carried out, the temperature is raised to 1450-1550 ℃ at the temperature rising speed of 4-5 ℃ per minute in the argon atmosphere, and the mixture is kept stand for 2-2.5h;
The gram weight of the silicon carbide fiber felt is 300g/m 2, and the thickness is 2mm;
The preparation of a secondary aerogel solution, mixing silica sol and gamma-aminopropyl triethoxysilane, and stirring and refluxing at a stirring speed of 400-600rpm for 6-7h at a temperature of 40-45 ℃ to obtain the secondary aerogel solution;
In the preparation of the secondary aerogel solution, the volume ratio of silica sol to gamma-aminopropyl triethoxysilane is 2000-2100:100-120;
The average particle size of silicon dioxide in the silica sol is 7nm, the pH is 10, and the mass content of the silicon dioxide is 30%;
the secondary treatment, namely adding the silicon carbide fiber felt subjected to the primary treatment into a mould, adding the mould into a vacuum device, adding a secondary aerogel solution, ensuring that the silicon carbide fiber felt can be completely immersed in the secondary aerogel solution and subjected to vacuum standing;
In the secondary treatment, the vacuum degree of the vacuum tank is 100-200Pa during vacuum standing, and the time of vacuum standing is 50-60min;
the temperature of the oven is 50-55 ℃ during the heat treatment, and the heat treatment time is 50-60min;
The temperature during the aging treatment is 50-55 ℃, the time of the aging treatment is 70-75h, and every 10-12h;
The preparation of modified silicon carbide whisker suspension, mixing beta-silicon carbide whisker, gamma- (2, 3-glycidoxy) propyl trimethoxy silane and absolute ethyl alcohol, stirring and refluxing for 3-4 hours at a stirring speed of 100-200rpm at 60-65 ℃, filtering, washing a precipitate with absolute ethyl alcohol for 3-4 times, drying, mixing with methanol, and stirring for 20-30 minutes at a stirring speed of 100-200rpm at room temperature to obtain modified silicon carbide whisker suspension;
In the preparation of the modified silicon carbide whisker suspension, the mass volume ratio of the beta-silicon carbide whisker to the gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane to the absolute ethyl alcohol to the methanol is 100-110g to 50-60mL to 900-1100mL to 8700-9000mL;
the length of the beta-type silicon carbide whisker is 20 mu m, and the diameter is 1 mu m;
The composite is prepared by completely immersing a silicon carbide fiber felt subjected to secondary treatment in a modified silicon carbide whisker suspension in an argon atmosphere, standing for 5-5.5h at 55-60 ℃, adding the mixture into a high-pressure reaction kettle, performing supercritical drying by using carbon dioxide, and finally adding the mixture into a tubular furnace for high-temperature treatment to obtain a composite heat insulation material;
in the compounding, the mass volume ratio of the silicon carbide fiber felt after the secondary treatment to the modified silicon carbide whisker suspension is 300g:3000-3200mL;
The temperature of the high-pressure reaction kettle in the supercritical drying is 45-50 ℃, the pressure is 10-12MPa, and the supercritical drying time is 2.5-3h;
And (3) the high-temperature treatment is carried out, the temperature is raised to 800-850 ℃ at the temperature rising speed of 4-5 ℃ per minute in the argon atmosphere, and the mixture is kept stand for 2-2.5h.
A composite heat insulation material prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the composite heat insulation material of the ceramic fiber and the aerogel comprises the steps of preparing a primary aerogel solution, carrying out primary treatment, preparing a secondary aerogel solution, carrying out secondary treatment, preparing a modified silicon carbide whisker suspension and compounding. The preparation of the primary aerogel solution comprises a step of preparing coated graphite and a mixing step, wherein the step of preparing coated graphite is to coat graphite powder by using silica sol with large particle size to obtain coated graphite, namely the graphite powder coated by the silica sol, and the mixing step is to mix the graphite powder coated by the silica sol with large particle size to obtain the primary aerogel solution; the preparation method comprises the steps of carrying out dipping treatment on a silicon carbide fiber felt by using a primary aerogel solution, then carrying out high-temperature treatment in an argon atmosphere after drying, carrying out reaction between graphite and silicon dioxide in the high-temperature treatment, coating a layer of silicon carbide nanowire on the surface of the silicon carbide fiber felt to obtain the silicon carbide fiber felt subjected to the primary treatment, preparing a secondary aerogel solution, carrying out treatment on silica sol by using gamma-aminopropyl triethoxysilane to obtain a secondary aerogel solution with aminopropyl on the surface, carrying out heat treatment and aging after dipping the silicon carbide fiber felt subjected to the primary treatment by using the secondary aerogel solution with aminopropyl to obtain the silicon carbide fiber felt subjected to the secondary treatment, preparing a modified silicon carbide whisker suspension, carrying out treatment on beta-type silicon carbide whisker by using gamma- (2, 3-glycidoxy) propyl trimethoxysilane to obtain beta-type silicon carbide whisker with epoxy groups on the surface, then mixing with methanol to obtain a beta-type silicon carbide whisker suspension with epoxy groups on the surface, namely, carrying out cross-linking treatment on the silicon carbide whisker after the silicon carbide fiber felt subjected to the secondary treatment in an argon atmosphere, carrying out supercritical cross-linking treatment on the silicon carbide fiber felt after the silicon carbide whisker suspension is subjected to the secondary treatment in the argon atmosphere, the cross-linked matter of the silicon carbide nanowire and the silicon carbide whisker on the surface can improve the hydrophobicity, toughness, durability, thermal shock resistance and high temperature resistance of the composite heat insulation material, and the purpose of coating the silicon carbide nanowire on the surface of the silicon carbide fiber felt before silica sol impregnation is to fix the silica sol and improve the dispersibility of the silica sol, so that the heat insulation property of the composite heat insulation material can be improved and the uniformity of the performance of the composite heat insulation material is ensured;
(2) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has good heat insulation performance, 5 samples are taken from the composite heat-insulating material of the ceramic fiber and the aerogel, and the average heat conductivity coefficient is 0.027-0.029W/(m.K);
(3) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has good hydrophobicity, 5 samples are taken from the composite heat-insulating material of the ceramic fiber and the aerogel, and the average water contact angle is 130.2-132.3 degrees;
(4) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has uniform performance, 5 samples are taken from the composite heat-insulating material of the ceramic fiber and the aerogel, the difference between the maximum heat conductivity coefficient and the minimum heat conductivity coefficient is 0.02-0.03W/(m.K), and the difference between the maximum water contact angle and the minimum water contact angle is 1.2-1.6 degrees;
(5) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has good toughness, and no crack exists at a bending position after bending for 30 degrees;
(6) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has good durability, and the composite heat-insulating material of the ceramic fiber and the aerogel prepared by the preparation method has no problem of particle falling after being stood for 10 days at 800 ℃;
(7) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has good thermal shock resistance, the temperature of the composite heat-insulating material of the ceramic fiber and the aerogel is raised to 1200 ℃, the temperature raising time is 4h, the heat is preserved for 10min at 1200 ℃, and then the composite heat-insulating material is cooled to 20 ℃ through cold air, so that the composite heat-insulating material is taken as a primary circulation and is circulated for 20 times altogether, and no crack exists on the surface;
(8) According to the preparation method of the composite heat-insulating material of the ceramic fiber and the aerogel, the prepared composite heat-insulating material has good high temperature resistance, 5 samples are taken from the composite heat-insulating material of the ceramic fiber and the aerogel, and the average heat conductivity coefficient at 1000 ℃ is 0.036-0.038W/(m.K).
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
The preparation method of the composite heat insulation material of the ceramic fiber and the aerogel specifically comprises the following steps:
1. preparing a primary aerogel solution:
(1) Preparing coated graphite, namely mixing 200mL of silica sol and 6mL of gamma-aminopropyl triethoxysilane, stirring and refluxing at the stirring speed of 400rpm for 5 hours at 40 ℃, adding 34g of graphite powder, continuously stirring and refluxing for 1 hour, centrifuging, controlling the centrifuging speed to be 6000rpm during centrifuging for 5 minutes, cleaning the precipitate by using deionized water for 3 times, and drying to obtain the coated graphite;
The particle size of the graphite powder is 50 mu m;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
(2) Mixing, namely mixing 2000mL of silica sol and 60mL of gamma-aminopropyl triethoxysilane, stirring and refluxing for 5 hours at a stirring speed of 400rpm at 40 ℃, adding 50g of coated graphite and 15g of nickel sulfate, and continuously stirring and refluxing for 50 minutes to obtain a primary aerogel solution;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
2. Adding the silicon carbide fiber felt into a mould, adding the mould into a vacuum device, vacuumizing the vacuum device until the vacuum degree is 100Pa, adding the aerogel solution once to ensure that the silicon carbide fiber felt can be completely immersed in the aerogel solution once and standing for 30min, then adding the silicon carbide fiber felt into an oven, controlling the temperature of the oven to be 100 ℃, standing for 18h, adding the silicon carbide fiber felt into a tube furnace, heating to 1450 ℃ at a heating rate of 4 ℃ per min in an argon atmosphere, and standing for 2h to obtain the silicon carbide fiber felt after the primary treatment;
The gram weight of the silicon carbide fiber felt is 300g/m 2, and the thickness is 2mm;
3. preparing a secondary aerogel solution, namely mixing 2000mL of silica sol and 100mL of gamma-aminopropyl triethoxysilane, and stirring and refluxing for 6 hours at 40 ℃ at a stirring speed of 400rpm to obtain the secondary aerogel solution;
The average particle size of silicon dioxide in the silica sol is 7nm, the pH is 10, and the mass content of the silicon dioxide is 30%;
4. Adding the silicon carbide fiber felt subjected to primary treatment into a mould, adding the mould into a vacuum device, vacuumizing the vacuum device until the vacuum degree is 100Pa, adding a secondary aerogel solution to ensure that the silicon carbide fiber felt can be completely immersed in the secondary aerogel solution and kept stand for 50min, then adding the silicon carbide fiber felt into an oven, controlling the temperature of the oven to 50 ℃, and keeping stand for 50min, completely immersing in absolute ethyl alcohol and keeping stand for 70h at 50 ℃, and changing the absolute ethyl alcohol every 10h during the period to obtain the silicon carbide fiber felt subjected to secondary treatment;
5. Preparing a modified silicon carbide whisker suspension, namely mixing 100g of beta-silicon carbide whisker, 50mL of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and 900mL of absolute ethyl alcohol, stirring and refluxing for 3 hours at a stirring speed of 100rpm at 60 ℃, filtering, washing a precipitate with absolute ethyl alcohol for 3 times, drying, mixing with 8700mL of methanol, and stirring for 20 minutes at a stirring speed of 100rpm at room temperature to obtain the modified silicon carbide whisker suspension;
the length of the beta-type silicon carbide whisker is 20 mu m, and the diameter is 1 mu m;
6. the method comprises the steps of fully immersing a silicon carbide fiber felt subjected to secondary treatment in a modified silicon carbide whisker suspension in an argon atmosphere, controlling the mass-volume ratio of the silicon carbide fiber felt subjected to secondary treatment to be 300 g/3000 mL, standing for 5h at 55 ℃, adding the mixture into a high-pressure reaction kettle, performing supercritical drying by using carbon dioxide, controlling the temperature of the high-pressure reaction kettle to 50 ℃, controlling the pressure to 12MPa, standing for 2.5h, finally adding the mixture into a tubular furnace, heating to 800 ℃ at a heating rate of 4 ℃ per min in the argon atmosphere, and standing for 2h to obtain the composite heat insulation material.
The embodiment also provides a composite heat insulation material prepared by the preparation method.
Example 2
The preparation method of the composite heat insulation material of the ceramic fiber and the aerogel specifically comprises the following steps:
1. preparing a primary aerogel solution:
(1) Preparing coated graphite, namely mixing 205mL of silica sol and 6.5mL of gamma-aminopropyl triethoxysilane, stirring and refluxing at a stirring speed of 500rpm for 5.5 hours at 42 ℃, adding 35g of graphite powder, continuously stirring and refluxing for 1.5 hours, centrifuging, controlling the centrifuging speed to 6500rpm for 5 minutes, cleaning the precipitate with deionized water for 3 times, and drying to obtain the coated graphite;
The particle size of the graphite powder is 50 mu m;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
(2) Mixing, namely mixing 2050mL of silica sol and 65mL of gamma-aminopropyl triethoxysilane, stirring and refluxing at a stirring speed of 500rpm for 5.5h at 42 ℃, adding 52g of coated graphite and 15.5g of nickel sulfate, and continuously stirring and refluxing for 55min to obtain a primary aerogel solution;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
2. adding the silicon carbide fiber felt into a mould, adding the mould into a vacuum device, vacuumizing the vacuum device to 150Pa, adding the primary aerogel solution to ensure that the silicon carbide fiber felt can be completely immersed in the primary aerogel solution and standing for 35min, then adding the silicon carbide fiber felt into an oven, controlling the temperature of the oven to be 100 ℃, standing for 19h, adding the silicon carbide fiber felt into a tube furnace, heating to 1500 ℃ at a heating rate of 4 ℃ per min in an argon atmosphere, and standing for 2h to obtain the silicon carbide fiber felt after the primary treatment;
The gram weight of the silicon carbide fiber felt is 300g/m 2, and the thickness is 2mm;
3. Preparing a secondary aerogel solution, namely mixing 2050mL of silica sol and 110mL of gamma-aminopropyl triethoxysilane, and stirring and refluxing at 42 ℃ for 6.5 hours at a stirring speed of 500rpm to obtain the secondary aerogel solution;
The average particle size of silicon dioxide in the silica sol is 7nm, the pH is 10, and the mass content of the silicon dioxide is 30%;
4. adding the silicon carbide fiber felt subjected to primary treatment into a mould, adding the mould into a vacuum device, vacuumizing the vacuum device until the vacuum degree is 150Pa, adding a secondary aerogel solution to ensure that the silicon carbide fiber felt can be completely immersed in the secondary aerogel solution and kept stand for 55min, then adding the silicon carbide fiber felt into an oven, controlling the temperature of the oven to 52 ℃, and keeping stand for 55min, completely immersing in absolute ethyl alcohol and keeping stand for 72h at 52 ℃, and changing the absolute ethyl alcohol every 11h during the period to obtain the silicon carbide fiber felt subjected to secondary treatment;
5. preparing a modified silicon carbide whisker suspension, namely mixing 105g of beta-silicon carbide whisker, 55mL of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and 1000mL of absolute ethyl alcohol, stirring and refluxing at a stirring speed of 150rpm for 3.5h at 62 ℃, filtering, washing a precipitate with absolute ethyl alcohol for 3 times, drying, mixing with 8800mL of methanol, and stirring at a stirring speed of 150rpm for 25min at room temperature to obtain the modified silicon carbide whisker suspension;
the length of the beta-type silicon carbide whisker is 20 mu m, and the diameter is 1 mu m;
6. The method comprises the steps of fully immersing a silicon carbide fiber felt subjected to secondary treatment in a modified silicon carbide whisker suspension in an argon atmosphere, controlling the mass-volume ratio of the silicon carbide fiber felt subjected to secondary treatment to be 300 g/310ml, standing for 5.5 hours at 58 ℃, adding the mixture into a high-pressure reaction kettle, performing supercritical drying by using carbon dioxide, controlling the temperature of the high-pressure reaction kettle to 50 ℃, controlling the pressure to 12MPa, standing for 2.5 hours, and finally adding the mixture into a tube furnace, heating to 820 ℃ at a heating rate of 5 ℃ per minute in the argon atmosphere, and standing for 2.5 hours to obtain the composite heat insulation material.
The embodiment also provides a composite heat insulation material prepared by the preparation method.
Example 3
The preparation method of the composite heat insulation material of the ceramic fiber and the aerogel specifically comprises the following steps:
1. preparing a primary aerogel solution:
(1) Preparing coated graphite, namely mixing 210mL of silica sol and 7mL of gamma-aminopropyl triethoxysilane, stirring and refluxing at a stirring speed of 600rpm for 6 hours at 45 ℃, adding 36g of graphite powder, continuously stirring and refluxing for 1.5 hours, centrifuging, controlling the centrifuging speed at 7000rpm for 6 minutes, cleaning the precipitate by using deionized water for 4 times, and drying to obtain the coated graphite;
The particle size of the graphite powder is 50 mu m;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
(2) Mixing 2100mL of silica sol and 70mL of gamma-aminopropyl triethoxysilane, stirring and refluxing for 6h at a stirring speed of 600rpm at 45 ℃, adding 55g of coated graphite and 16g of nickel sulfate, and continuously stirring and refluxing for 60min to obtain a primary aerogel solution;
the average particle diameter of silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%;
2. Adding the silicon carbide fiber felt into a mould, adding the mould into a vacuum device, vacuumizing the vacuum device until the vacuum degree is 200Pa, adding the primary aerogel solution to ensure that the silicon carbide fiber felt can be completely immersed in the primary aerogel solution and standing for 40min, then adding the silicon carbide fiber felt into an oven, controlling the temperature of the oven to be 100 ℃, standing for 20h, adding the silicon carbide fiber felt into a tube furnace, heating to 1550 ℃ at a heating rate of 5 ℃ per min in an argon atmosphere, and standing for 2.5h to obtain the silicon carbide fiber felt after primary treatment;
The gram weight of the silicon carbide fiber felt is 300g/m 2, and the thickness is 2mm;
3. Preparing a secondary aerogel solution, namely mixing 2100mL of silica sol and 120mL of gamma-aminopropyl triethoxysilane, and stirring and refluxing for 7 hours at 45 ℃ at a stirring speed of 600rpm to obtain the secondary aerogel solution;
The average particle size of silicon dioxide in the silica sol is 7nm, the pH is 10, and the mass content of the silicon dioxide is 30%;
4. adding the silicon carbide fiber felt subjected to primary treatment into a mould, adding the mould into a vacuum device, vacuumizing the vacuum device until the vacuum degree is 200Pa, adding a secondary aerogel solution to ensure that the silicon carbide fiber felt can be completely immersed in the secondary aerogel solution and kept stand for 60min, then adding the silicon carbide fiber felt into an oven, controlling the temperature of the oven to 55 ℃ and keeping stand for 60min, completely immersing in absolute ethyl alcohol and keeping stand for 75h at 55 ℃, and changing the absolute ethyl alcohol every 12h during the period to obtain the silicon carbide fiber felt subjected to secondary treatment;
5. Preparing a modified silicon carbide whisker suspension, namely mixing 110g of beta-silicon carbide whisker, 60mL of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and 1100mL of absolute ethyl alcohol, stirring and refluxing for 4 hours at a stirring speed of 200rpm at 65 ℃, filtering, washing a precipitate for 4 times by using the absolute ethyl alcohol, drying, mixing with 9000mL of methanol, and stirring for 30 minutes at a stirring speed of 200rpm at room temperature to obtain the modified silicon carbide whisker suspension;
the length of the beta-type silicon carbide whisker is 20 mu m, and the diameter is 1 mu m;
6. The method comprises the steps of fully immersing a silicon carbide fiber felt subjected to secondary treatment in a modified silicon carbide whisker suspension in an argon atmosphere, controlling the mass volume ratio of the silicon carbide fiber felt subjected to secondary treatment to be 300 g/3200 mL, standing for 5.5h at 60 ℃, adding the mixture into a high-pressure reaction kettle, performing supercritical drying by using carbon dioxide, controlling the temperature of the high-pressure reaction kettle to 50 ℃, controlling the pressure to 12MPa, standing for 3h, finally adding the mixture into a tubular furnace, heating to 850 ℃ at a heating rate of 5 ℃ per min in the argon atmosphere, and standing for 2.5h to obtain the composite heat insulation material.
The embodiment also provides a composite heat insulation material prepared by the preparation method.
Comparative example 1
The steps of preparing the aerogel solution in the step 1 and treating the aerogel in the step 2 are omitted on the basis of the embodiment 1, and in the step 4, a silicon carbide fiber felt with the untreated gram weight of 300g/m 2 and the thickness of 2mm is used for replacing the silicon carbide fiber felt after the primary treatment.
The rest of the procedure is the same as in example 1.
Comparative example 2
The step of preparing the modified silicon carbide whisker suspension in the step 5 and the step of compounding in the step 6 are omitted on the basis of the embodiment 1, and the secondarily treated silicon carbide fiber felt obtained in the step 4 is used as a composite heat insulation material.
The rest of the procedure is the same as in example 1.
Performance test 1
5 Samples were taken on the composite heat insulating materials prepared in examples 1 to 3 and comparative examples 1 to 2, the interval between each sample was 20cm, then the heat conductivity and the water contact angle of the 5 samples were tested, respectively, the average heat conductivity and the average water contact angle were calculated, respectively, and the difference between the maximum heat conductivity and the minimum heat conductivity, the difference between the maximum water contact angle and the minimum water contact angle were calculated, and the calculation results are shown in table 1:
TABLE 1
Performance test 2
The composite heat-insulating materials prepared in examples 1 to 3 and comparative examples 1 to 2 were bent by 30 °, and whether or not cracks were present at the bent portions was observed, and the observation results are shown in table 2:
TABLE 2
Performance test 3
After the composite heat-insulating materials prepared in examples 1 to 3 and comparative examples 1 to 2 were allowed to stand at 800℃for 10 days, it was observed whether the composite heat-insulating materials had a problem of particle shedding, and the observation results are shown in Table 3:
TABLE 3 Table 3
Performance test 4
The composite heat-insulating materials prepared in examples 1 to 3 and comparative examples 1 to 2 were heated to 1200 ℃ for 4 hours, kept at 1200 ℃ for 10 minutes, and then cooled to 20 ℃ by cold air, and the composite heat-insulating materials were circulated for 20 times as a single cycle, and whether cracks exist on the surface of the composite heat-insulating materials or not was observed, and the observation results are shown in table 4:
TABLE 4 Table 4
Performance test 5
5 Samples were taken on the composite thermal insulation materials prepared in examples 1-3 and comparative examples 1-2, each with a 20cm interval therebetween, and then the thermal conductivity of the 5 samples at 1000 ℃ was tested, the average thermal conductivity at 1000 ℃ was calculated, and the calculation results are shown in table 5:
TABLE 5
As can be seen from the results of the performance tests 1 to 5, the composite heat insulating material prepared in comparative example 1 has lower heat insulating properties, lower hydrophobicity, toughness, durability, thermal shock resistance and high temperature resistance than those of the composite heat insulating material prepared in example 1, and the composite heat insulating material prepared in comparative example 3 has lower hydrophobicity, toughness, durability, thermal shock resistance and high temperature resistance than those of the composite heat insulating material prepared in example 1 and comparative example 2, and has the problem of uneven performance.
The percentages used in the present invention are mass percentages unless otherwise indicated.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto, but may be modified or substituted for some of the technical features thereof 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. The preparation method of the composite heat insulation material of the ceramic fiber and the aerogel is characterized by comprising the following steps of preparing a primary aerogel solution, carrying out primary treatment, preparing a secondary aerogel solution, carrying out secondary treatment, preparing a modified silicon carbide whisker suspension, and compounding;
the preparation of the primary aerogel solution comprises the steps of preparing coated graphite and mixing;
Mixing silica sol and gamma-aminopropyl triethoxysilane, stirring and refluxing at 40-45 ℃, adding graphite powder, continuously stirring and refluxing, centrifuging, cleaning precipitate, and drying to obtain coated graphite;
Mixing, namely mixing silica sol and gamma-aminopropyl triethoxysilane, stirring and refluxing at 40-45 ℃, adding coated graphite and nickel sulfate, and continuously stirring and refluxing to obtain a primary aerogel solution;
adding the silicon carbide fiber felt into a mould, adding the mould into a vacuum device, adding the primary aerogel solution, ensuring that the silicon carbide fiber felt can be completely immersed in the primary aerogel solution and kept stand in vacuum;
the preparation method comprises the steps of preparing a secondary aerogel solution, mixing silica sol and gamma-aminopropyl triethoxysilane, and stirring and refluxing at 40-45 ℃ to obtain the secondary aerogel solution;
the secondary treatment, namely adding the silicon carbide fiber felt subjected to the primary treatment into a mould, adding the mould into a vacuum device, adding a secondary aerogel solution, ensuring that the silicon carbide fiber felt can be completely immersed in the secondary aerogel solution and subjected to vacuum standing;
the preparation method comprises the steps of preparing a modified silicon carbide whisker suspension, mixing beta-silicon carbide whisker, gamma- (2, 3-glycidoxy) propyl trimethoxy silane and absolute ethyl alcohol, stirring and refluxing at 60-65 ℃, filtering, cleaning precipitate, drying, mixing with methanol, and stirring at room temperature to obtain the modified silicon carbide whisker suspension;
The composite is prepared by immersing the silicon carbide fiber felt subjected to secondary treatment in modified silicon carbide whisker suspension completely in argon atmosphere, standing at 55-60 ℃, adding into a high-pressure reaction kettle, performing supercritical drying by using carbon dioxide, and finally adding into a tubular furnace for high-temperature treatment.
2. The method for preparing the composite heat insulation material of the ceramic fiber and the aerogel according to claim 1, wherein in the preparation of the coated graphite, the volume mass ratio of silica sol, gamma-aminopropyl triethoxysilane and graphite powder is 200-210mL:6-7mL:34-36g;
The particle size of the graphite powder is 50 mu m;
the average particle diameter of the silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%.
3. The method for preparing the composite heat insulation material of ceramic fiber and aerogel according to claim 1, wherein in the mixing, the volume mass ratio of silica sol, gamma-aminopropyl triethoxysilane, coated graphite and nickel sulfate is 2000-2100ml:60-70ml:50-55g:15-16g;
the average particle diameter of the silicon dioxide in the silica sol is 22nm, the pH is 9, and the mass content of the silicon dioxide is 30%.
4. The method for preparing a composite thermal insulation material of ceramic fiber and aerogel according to claim 1, wherein in the one-time treatment, the vacuum degree of the vacuum tank is 100-200Pa during vacuum standing, and the time of vacuum standing is 30-40min;
The temperature of the oven is 100-110 ℃ during the heat treatment, and the heat treatment time is 18-20h;
the high-temperature treatment is carried out, the temperature is raised to 1450-1550 ℃ at the temperature rising speed of 4-5 ℃ per minute in the argon atmosphere, and the mixture is kept stand for 2-2.5h;
The gram weight of the silicon carbide fiber felt is 300g/m 2, and the thickness is 2mm.
5. The method for preparing the composite heat insulation material of ceramic fiber and aerogel according to claim 1, wherein the volume ratio of silica sol and gamma-aminopropyl triethoxysilane in the secondary aerogel solution is 2000-2100:100-120;
The average particle size of the silicon dioxide in the silica sol is 7nm, the pH is 10, and the mass content of the silicon dioxide is 30%.
6. The method for preparing a composite thermal insulation material of ceramic fiber and aerogel according to claim 1, wherein in the secondary treatment, the vacuum degree of the vacuum tank is 100-200Pa during vacuum standing, and the time of vacuum standing is 50-60min;
the temperature of the oven is 50-55 ℃ during the heat treatment, and the heat treatment time is 50-60min;
The temperature of the aging treatment is 50-55 ℃, the aging treatment time is 70-75h, and every 10-12h.
7. The method for preparing the composite heat insulation material of the ceramic fiber and the aerogel according to claim 1, wherein in the preparation of the modified silicon carbide whisker suspension, the mass-volume ratio of beta silicon carbide whisker, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, absolute ethyl alcohol and methanol is 100-110g:50-60mL:900-1100mL:8700-9000mL;
the length of the beta-type silicon carbide whisker is 20 mu m, and the diameter is 1 mu m.
8. The method for preparing the composite heat-insulating material of ceramic fibers and aerogel according to claim 1, wherein in the compounding, the mass-volume ratio of the secondarily treated silicon carbide fiber felt to the modified silicon carbide whisker suspension is 300g:3000-3200mL;
The temperature of the high-pressure reaction kettle in the supercritical drying is 45-50 ℃, the pressure is 10-12MPa, and the supercritical drying time is 2.5-3h;
And (3) the high-temperature treatment is carried out, the temperature is raised to 800-850 ℃ at the temperature rising speed of 4-5 ℃ per minute in the argon atmosphere, and the mixture is kept stand for 2-2.5h.
9. A composite thermal insulation material prepared by the preparation method of any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202411795745.1A CN119263794A (en) | 2024-12-09 | 2024-12-09 | Composite heat insulation material of ceramic fiber and aerogel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202411795745.1A CN119263794A (en) | 2024-12-09 | 2024-12-09 | Composite heat insulation material of ceramic fiber and aerogel and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN119263794A true CN119263794A (en) | 2025-01-07 |
Family
ID=94121554
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202411795745.1A Pending CN119263794A (en) | 2024-12-09 | 2024-12-09 | Composite heat insulation material of ceramic fiber and aerogel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN119263794A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020094426A1 (en) * | 2000-12-22 | 2002-07-18 | Aspen Aerogels, Inc. | Aerogel composite with fibrous batting |
| CN102276236A (en) * | 2011-04-29 | 2011-12-14 | 中国人民解放军国防科学技术大学 | High temperature resistant Si-C-O aerogel thermal insulation composite material and preparation method thereof |
| CN113246556A (en) * | 2021-06-16 | 2021-08-13 | 中南大学 | Ultra-light heat-insulation scouring-resistant function-integrated composite material and preparation method thereof |
| CN118545709A (en) * | 2024-04-30 | 2024-08-27 | 宁波石墨烯创新中心有限公司 | A controllable size graphene oxide modified aerogel composite material and preparation method thereof |
| CN118791292A (en) * | 2024-09-13 | 2024-10-18 | 山东工业陶瓷研究设计院有限公司 | Preparation method of a reusable flexible aerogel composite material with hydrophobic performance resistant to 800°C |
| CN119059795A (en) * | 2024-11-04 | 2024-12-03 | 山东工业陶瓷研究设计院有限公司 | A method for preparing phenolic aerogel composite thermal insulation tile |
-
2024
- 2024-12-09 CN CN202411795745.1A patent/CN119263794A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020094426A1 (en) * | 2000-12-22 | 2002-07-18 | Aspen Aerogels, Inc. | Aerogel composite with fibrous batting |
| CN102276236A (en) * | 2011-04-29 | 2011-12-14 | 中国人民解放军国防科学技术大学 | High temperature resistant Si-C-O aerogel thermal insulation composite material and preparation method thereof |
| CN113246556A (en) * | 2021-06-16 | 2021-08-13 | 中南大学 | Ultra-light heat-insulation scouring-resistant function-integrated composite material and preparation method thereof |
| CN118545709A (en) * | 2024-04-30 | 2024-08-27 | 宁波石墨烯创新中心有限公司 | A controllable size graphene oxide modified aerogel composite material and preparation method thereof |
| CN118791292A (en) * | 2024-09-13 | 2024-10-18 | 山东工业陶瓷研究设计院有限公司 | Preparation method of a reusable flexible aerogel composite material with hydrophobic performance resistant to 800°C |
| CN119059795A (en) * | 2024-11-04 | 2024-12-03 | 山东工业陶瓷研究设计院有限公司 | A method for preparing phenolic aerogel composite thermal insulation tile |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112301508B (en) | Silicon dioxide aerogel composite thermal insulation fabric and preparation method thereof | |
| CN108385375A (en) | A kind of preparation method of super-hydrophobic antibiotic fabric | |
| CN116354355A (en) | Preparation method of spherical silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler | |
| CN112897980A (en) | Preparation method of fiber-reinforced silica aerogel thermal insulation material | |
| CN112709075A (en) | High-strength aerogel modified heat insulation felt and preparation method thereof | |
| CN119263794A (en) | Composite heat insulation material of ceramic fiber and aerogel and preparation method thereof | |
| CN109721330B (en) | A kind of preparation method of GO-SiO2 composite ultra-high molecular weight polyethylene fiber cloth aerogel | |
| CN109626954B (en) | A temperature-resistant and moisture-proof silica aerogel composite material and its preparation method and application | |
| CN1586711A (en) | Aluminium modified silica-gel adsorbent material and its preparing process | |
| CN101328014A (en) | A kind of manufacturing method of doped quartz glass fiber | |
| CN118791292B (en) | Preparation method of a reusable flexible aerogel composite material with hydrophobic performance resistant to 800°C | |
| CN108144575B (en) | Graphite sulfide silica gel lithium chloride curing composite dehumidifier and preparation method thereof | |
| CN113061287B (en) | A kind of preparation method of flame retardant wood-based composite aerogel | |
| CN114455934A (en) | Preparation method of basalt fiber felt reinforced aerogel material | |
| CN116410516B (en) | High-temperature low-thermal-conductivity aerogel composite material and preparation method thereof | |
| CN111362665A (en) | Preparation method of mesoporous MSQ aerogel/glass fiber composite material | |
| CN114403501B (en) | Cooling fiber for cigarette filter tip and preparation method and application thereof | |
| CN110499078B (en) | Preparation method and application of radar antenna housing or antenna window compressive stress coating | |
| CN112551506B (en) | Antioxidant carbon aerogel composite material and preparation method and application thereof | |
| JPS6212321B2 (en) | ||
| KR102190889B1 (en) | Method for preparing silica aerogel blanket with high thermal insulation and high strength | |
| CN108503240A (en) | A kind of resurrection glass fibre cotton and preparation method thereof | |
| CN118343821B (en) | Barium sulfate-containing multi-element composite aerogel porous heat insulation material and preparation method thereof | |
| CN115159926B (en) | A crack-resistant microcement with low shrinkage | |
| CN108947357B (en) | Construction material containing potassium feldspar and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |