CN115744922A - Silicon aerogel flame retardant and preparation method and application thereof - Google Patents
Silicon aerogel flame retardant and preparation method and application thereof Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000004964 aerogel Substances 0.000 title claims abstract description 78
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 78
- 239000010703 silicon Substances 0.000 title claims abstract description 78
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000003063 flame retardant Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 123
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 110
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 54
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 28
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 230000032683 aging Effects 0.000 claims abstract description 21
- 239000000017 hydrogel Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001879 gelation Methods 0.000 claims abstract description 18
- 239000003085 diluting agent Substances 0.000 claims abstract description 17
- 238000002485 combustion reaction Methods 0.000 claims abstract description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 239000000499 gel Substances 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 238000000352 supercritical drying Methods 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000012774 insulation material Substances 0.000 claims description 6
- ZMAPKOCENOWQRE-UHFFFAOYSA-N diethoxy(diethyl)silane Chemical compound CCO[Si](CC)(CC)OCC ZMAPKOCENOWQRE-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 4
- MASNVFNHVJIXLL-UHFFFAOYSA-N ethenyl(ethoxy)silicon Chemical compound CCO[Si]C=C MASNVFNHVJIXLL-UHFFFAOYSA-N 0.000 claims description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 3
- DFJDZTPFNSXNAX-UHFFFAOYSA-N ethoxy(triethyl)silane Chemical compound CCO[Si](CC)(CC)CC DFJDZTPFNSXNAX-UHFFFAOYSA-N 0.000 claims description 3
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 3
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 92
- 238000006073 displacement reaction Methods 0.000 description 11
- 230000002209 hydrophobic effect Effects 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000002243 precursor Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 208000005156 Dehydration Diseases 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- 239000004254 Ammonium phosphate Substances 0.000 description 5
- 239000003377 acid catalyst Substances 0.000 description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 5
- 235000019289 ammonium phosphates Nutrition 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000002808 molecular sieve Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000004793 Polystyrene Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 3
- 125000000962 organic group Chemical group 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OGFYGJDCQZJOFN-UHFFFAOYSA-N [O].[Si].[Si] Chemical compound [O].[Si].[Si] OGFYGJDCQZJOFN-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- -1 silicon dioxide ions Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Images
Classifications
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- 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
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- Silicon Compounds (AREA)
Abstract
The invention relates to a silicon aerogel flame retardant, a preparation method and application thereof. The method comprises the following steps: respectively preparing a first solution and a second solution, and mixing to obtain silicon dioxide hydrosol; the first solution is obtained by adding phosphoric acid into an organic silicon source solution for hydrolysis; adding phosphoric acid into the silica sol diluent, and adding ethanol to dilute and dissolve the solution; the temperature of the first solution and the second solution is more than or equal to 21 ℃; adding an alkali catalyst into the silica hydrosol to carry out a gelation reaction to obtain the silica hydrogel; aging and replacing the silicon dioxide hydrogel to obtain silicon dioxide alcohol gel; and (4) supercritical drying to obtain the silicon aerogel flame retardant. The technical problem to be solved is how to improve the flame retardant property of the silicon dioxide aerogel, so that the limited oxygen index is more than or equal to 35 percent, the combustion heat value is less than or equal to 2.2MJ/kg, and the silicon dioxide aerogel has good heat insulation property (the heat conductivity coefficient is less than or equal to 0.021W/(m.k)) and hydrophobicity (the contact angle is more than or equal to 120 degrees) and can be used as a silicon aerogel flame retardant.
Description
Technical Field
The invention belongs to the technical field of flame-retardant materials, and particularly relates to a silicon aerogel flame retardant, and a preparation method and application thereof.
Background
At present, the traditional polystyrene heat-insulating material in China has poor fireproof performance, the combustion grade is mostly B grade, and a large amount of toxic and harmful gases can be generated during combustion, so that the potential safety hazard is large, the mechanical strength is low, and the wide application of the polystyrene heat-insulating material is limited. And SiO 2 Since the aerogel can effectively transmit sunlight and simultaneously prevent infrared heat radiation of ambient temperature and is an inorganic non-combustible material, researchers in recent years use SiO 2 A great deal of scientific research work is carried out on the aerogel serving as a flame retardant so as to improve the fireproof and flame retardant performance of the aerogel when the aerogel is used for a polystyrene thermal insulation material.
In the prior art, siO 2 Most of the aerogel preparation processes comprise a step of surface hydrophobic modification, and the hydrophobic modification step is necessarily carried out on SiO 2 Organic functional groups are introduced into the aerogel, so that the thermal stability of the aerogel material is poor; also, these introduced organic components may also be a potential fire risk factor. Therefore, how to promote SiO 2 The aerogel has the advantages of improving the heat insulation and flame retardant properties of the aerogel, improving the use reliability of the aerogel as a flame retardant and having very important significance for large-scale popularization and application of the aerogel.
Disclosure of Invention
The invention mainly aims to provide a silicon aerogel flame retardant and a preparation method and application thereof, and aims to solve the technical problem of improving the flame retardant property of silicon dioxide aerogel to ensure that the limited oxygen index is more than or equal to 35 percent, the combustion heat value is less than or equal to 2.2MJ/kg, and the silicon dioxide aerogel flame retardant also has good heat insulation property (the heat conductivity coefficient is less than or equal to 0.021W/(m.k)) and hydrophobicity (the contact angle is more than or equal to 120 degrees), can be used as the silicon aerogel flame retardant, and is more practical.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a preparation method of a silicon aerogel flame retardant, which comprises the following steps:
1) Respectively preparing a first solution and a second solution, and uniformly mixing the first solution and the second solution according to a volume ratio of 1-2.5; adding a phosphoric acid catalyst into the organic silicon source solution under stirring to carry out hydrolysis reaction for 1-3 h; adding a phosphoric acid catalyst into the silica sol diluent under stirring, and then adding ethanol to dilute and dissolve the solution for 0.5 to 1 hour; the temperature of the first solution and the second solution is more than or equal to 21 ℃;
2) Adding an alkali catalyst into the silica hydrosol to carry out a gelation reaction to obtain a silica hydrogel;
3) Carrying out aging replacement on the silicon dioxide hydrogel to obtain silicon dioxide alcohol gel;
4) And (4) supercritical drying to obtain the silicon aerogel flame retardant.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the preparation method, the organic silicon source solution comprises a molar ratio of 1: 8-10: 15-20 parts of organic silicon source, absolute ethyl alcohol and deionized water; the organic silicon source is at least one selected from methyltriethoxysilane, dimethyldiethoxysilane, trimethylethoxysilane, triethylethoxysilane, diethyldiethoxysilane, ethyltriethoxysilane and vinylethoxysilane.
Preferably, the preparation method is that the silica sol diluent is SiO 2 Diluting silica sol with the mass fraction of 15-40%, the PH value of 7.5-8.5 and the particle size of 4-6 nm, 8-15 nm or 10-20 nm to SiO by deionized water 2 The mass fraction is 10%.
Preferably, the preparation method, wherein the molar concentration of the phosphoric acid catalyst is 0.01-1 mol/L; the pH values of the first solution and the second solution are both 2.0-4.0.
Preferably, in the preparation method, the alkali catalyst is an ammonia solution with a molar concentration of 0.1-10 mol/L; the reaction temperature of the gelation reaction is 45-60 ℃.
Preferably, the preparation method comprises the following steps: adding absolute ethyl alcohol with the same volume into the silicon dioxide hydrogel, and aging for 12-24 h at the temperature of 45-55 ℃; then, replacing the liquid in the aging system with absolute ethyl alcohol to perform solvent replacement; the solvent replacement is carried out once every 12h for 2-4 times.
Preferably, in the supercritical drying, the silica alcohol gel is placed in a supercritical ethanol kettle, absolute ethanol is added, the drying kettle is sealed after being purged by nitrogen, the temperature is increased to 250-270 ℃, the drying kettle is kept for 4-6 hours under the pressure of 13-15 MPa, the drying kettle is restored to normal pressure, and the drying kettle is purged by nitrogen for 10min and cooled to room temperature.
Preferably, the preparation method further comprises a waste liquid disposal step: collecting aged and replaced ethanol, gasifying and dehydrating the ethanol until the water content is less than 5wt%, and cooling for later use.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the silicon aerogel flame retardant provided by the invention, the limiting oxygen index is more than or equal to 35 percent, the combustion heat value is less than or equal to 2.2MJ/kg, the heat conductivity coefficient is less than or equal to 0.021W/(m.k), and the contact angle is more than or equal to 120 degrees.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The invention provides application of the silicon aerogel flame retardant in the field of heat insulation materials.
By the technical scheme, the silicon aerogel flame retardant and the preparation method and application thereof provided by the invention at least have the following advantages:
the invention provides a silicon aerogel flame retardant and a preparation method and application thereof, wherein an organic silicon source solution and inorganic silica sol are used as precursors to prepare the silicon aerogel flame retardant; the inorganic silica sol is low in price and has a non-combustible property, and organic groups in the aerogel can be reduced; the organic silicon source in the organic silicon source solution may include methyl, ethyl or vinyl groups, so that the silicon aerogel of the invention The flame retardant has good hydrophobic property, and can obtain good hydrophobic property even if surface hydrophobic treatment is not carried out in the preparation process; through the use of the organic and inorganic composite precursors, the residue of organic groups in the aerogel flame retardant is reduced, and the overall thermal stability temperature of the hydrophobic aerogel is improved; meanwhile, phosphoric acid is used as an acid catalyst in the processes of hydrolyzing the organic silicon source solution and diluting and dissolving the inorganic silica sol, and an alkali catalyst is applied in the subsequent polycondensation process; the phosphoric acid can react with an alkali catalyst to generate phosphate which is uniformly reserved in the interior and pores of the aerogel to play a certain flame-retardant role; according to the technical scheme, the silicon aerogel flame retardant is prepared, and has good flame retardant performance, the limited oxygen index of the silicon aerogel flame retardant is more than or equal to 35%, and the combustion heat value of the silicon aerogel flame retardant is less than or equal to 2.2MJ/kg; the heat insulation material has good heat insulation performance, and the heat conductivity coefficient is less than or equal to 0.021W/(m.k); also has good hydrophobic performance, the contact angle is more than or equal to 120 degrees, and the product is hydrophobic SiO with flame retardant and heat insulation functions 2 The aerogel material can be used as a silicon aerogel flame retardant.
Furthermore, in the technical scheme of the invention, the organic silicon source only selects the organic silicon source containing ethoxysilane, so that the byproduct generated in the hydrolysis reaction is only water or ethanol, is nontoxic and does not need to be separated; byproduct ethanol and water can be advanced along with the reaction process, collect the form of ageing replacement liquid, after concentrating the waste liquid and handling, dehydration is the absolute ethyl alcohol that the water content is less than 5%, the raw materials that the circulation was used for silicon system aerogel flame retardant method, greatly reduced the manufacturing cost of silicon system aerogel flame retardant.
Furthermore, the preparation method adopts a supercritical ethanol drying method to extract components such as a solvent in the aerogel, and residual unreacted organic groups on the precursor are removed as far as possible by controlling the process conditions such as the reaction temperature of the supercritical drying, so that the hydrophobic SiO is greatly reduced 2 Aerogel as a flame retardant potential fire risk.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to make the technical solutions of the present invention practical in accordance with the contents of the specification, the following detailed description is given of preferred embodiments of the present invention with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of a preparation process of a silicon aerogel flame retardant.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, characteristics and effects of the silicon aerogel flame retardant, the preparation method and the application thereof according to the present invention are provided with the accompanying drawings and preferred embodiments.
The invention provides a preparation method of a silicon aerogel flame retardant, which comprises the following steps as shown in the attached figure 1:
firstly, respectively preparing a first solution and a second solution, and then uniformly mixing the first solution and the second solution to obtain the silica hydrosol.
The first solution is prepared by adding a phosphoric acid catalyst into an organic silicon source solution under the condition of stirring to perform hydrolysis reaction for 1-3 h; the organic silicon source solution comprises an organic silicon source, absolute ethyl alcohol and deionized water; wherein the organic silicon source can be methoxy silane or ethoxy silane containing methyl, ethyl and vinyl; the organic silicon source and deionized water are subjected to hydrolysis reaction in the presence of a phosphoric acid catalyst, namely, methoxysilane or ethoxysilane in the organic silicon source reacts with water to generate silanol and micromolecular byproducts such as methanol, ethanol and the like; in view of the toxicity of methanol and the difference between methanol and the ethanol environment in the hydrolysis reaction environment designed by the technical scheme of the invention, in order to avoid a byproduct separation process, the organic silicon source is preferably selected from at least one of methyltriethoxysilane, dimethyldiethoxysilane, trimethylethoxysilane, triethylethoxysilane, diethyldiethoxysilane, ethyltriethoxysilane and vinyl ethoxysilane, that is, the organic silicon source only contains ethoxysilane and does not contain methoxysilane, so that the byproduct of the hydrolysis reaction only comprises ethanol, and the separation and disposal of the byproduct are not needed. Due to the fact that the organic silicon source contains a plurality of methyl groups, ethyl groups or vinyl groups, a chain-type growing silicon-oxygen-silicon network structure can be formed through hydrolysis reaction.
In order to strictly control the progress of the hydrolysis reaction, the molar ratio of the organic silicon source, the absolute ethyl alcohol and the deionized water in the organic silicon source solution is preferably 1: 8-10: 15 to 20; the molar concentration of the phosphoric acid catalyst is 0.01-1 mol/L; adding a phosphoric acid catalyst into the organic silicon source solution while stirring, and adjusting the pH value of the reaction system to be 2.0-4.0.
The phosphoric acid belongs to medium and strong acid, the crystallization point (freezing point) of the phosphoric acid is 21 ℃, and semi-hydrate crystals (ice crystals) can be separated out when the temperature is lower than the crystallization point. In order to avoid crystallization of phosphoric acid during the hydrolysis reaction, it is preferable in the present invention to maintain the ambient temperature of the entire process at 21 ℃ or higher during the preparation and mixing of the first solution.
Adding a phosphoric acid catalyst into the silica sol diluent under the stirring condition, and then adding ethanol into the silica sol diluent to dilute and dissolve the silica sol diluent for 0.5 to 1 hour; the silica sol diluent is obtained by diluting silica sol with deionized water; the silica sol for dilution, siO thereof 2 15-40% by mass, a pH value of 7.5-8.5, and a particle size of 4-6 nm, 8-15 nm or 10-20 nm; silica is insoluble in water and cannot form a solution; the silica sol is a dispersion liquid of nano-scale silica particles in water or a solvent; siO in silica Sol 2 Contains a large amount of water and hydroxyl groups, and can be in a stable state. SiO in the silica sol diluent 2 The mass fraction is 10%. The silica sol diluent contains nano-scale silica particles and is in a stable state. Adding a phosphoric acid catalyst into a silica sol diluent while stirring to destroy the charge stability of the silica sol diluent, so that silicon dioxide particles are dissociated to form single particles or aggregates; in order to control the state of silicon dioxide ions in the system, the molar concentration of the phosphoric acid catalyst is 0.01-1 mol/L; adding a phosphoric acid catalyst into the silica sol diluent while stirring, and adjusting the pH value of the reaction system to 2.0-4.0. Then, ethanol was added to the system with further stirring, the purpose of this operation being toThe second solution creates an ethanol environment close to the first solution, so that the mixing process of the first solution and the second solution can be controlled conveniently; no chemical reaction occurs in the second solution after the addition of ethanol, and there is only a physical change in the dilution and dissolution of the silica particles.
The phosphoric acid belongs to medium and strong acid, the crystallization point (freezing point) of the phosphoric acid is 21 ℃, and semi-hydrate crystals (ice) can be separated out when the temperature is lower than the crystallization point. In order to avoid crystallization of phosphoric acid during the hydrolysis reaction, it is preferable in the present invention to maintain the ambient temperature of the entire process at 21 ℃ or higher during preparation and mixing of the second solution.
When the first solution and the second solution are mixed, the stirring time is preferably 0.5h. In the stirring process after mixing, the first solution and the second solution do not generate chemical reaction, but the nano-scale silicon dioxide particles or aggregates in the second solution permeate into the organic silicon network structure in the first solution to form an interpenetrating microscopically uniformly mixed structure; if the mixing and stirring time is too short, the interpenetrating penetration of the first solution and the second solution may be uneven; if the mixing and stirring time is too long, the hydrolysis reaction time may be too long; according to the invention, the stirring time of the first solution and the second solution is preferably 0.5h when the first solution and the second solution are mixed. When the first solution and the second solution are mixed, the volume ratio of the first solution to the second solution is 1 to 2.5.
Secondly, adding an alkali catalyst into the silica hydrosol to carry out gelation reaction to obtain the silica hydrogel. The concrete steps are that the alkali catalyst is added into the silica hydrosol prepared in the previous step while stirring to carry out polycondensation reaction.
In order to strictly control the progress of the gelation reaction, the alkali catalyst is an ammonia water solution with the molar concentration of 0.1-10 mol/L; the pH value of the reaction system is adjusted to 6.5-7.0 by adding ammonia water solution.
The gelation reaction time can be adjusted by adjusting the addition amount of aqueous ammonia and adjusting the temperature of the gelation reaction to a small extent. The ammonia water is added in an excessive amount generally; the phosphoric acid catalyst contained in the silica hydrosol in the reaction system can perform acid-base neutralization reaction with ammonia water to generate ammonium phosphate; since phosphoric acid is microscopically uniformly distributed in the silica hydrosol, ammonium phosphate is also microscopically uniformly distributed throughout the gel system. The reaction temperature of the gelation reaction is preferably 45 to 60 ℃. The end point of the gelation reaction can be judged from the appearance of the reaction system; generally, when the reaction liquid is inclined by 45 degrees and the liquid does not flow, the initial gel of the gelation reaction can be considered, the reaction system at the time is the silica hydrogel, and the subsequent operation can be carried out.
And aging and replacing the silica hydrogel to obtain the silica alcogel.
The step of aging and displacement is to add absolute ethyl alcohol with the same volume into the silicon dioxide hydrogel, and to stand the silicon dioxide hydrogel at the temperature of 45-55 ℃ so as to age the silicon dioxide hydrogel for 12-24 hours; then, replacing the liquid in the aging system with absolute ethyl alcohol to carry out solvent replacement; the solvent replacement is carried out once every 12h and is repeated for 2 to 4 times. The solvent displacement can displace only the liquid in the gel, while the phosphate uniformly distributed therein in microscopic form cannot be displaced.
The liquid obtained by the aging and the solvent replacement is an ethanol liquid containing water, and the ethanol liquid can be collected and dehydrated to be used as an anhydrous ethanol raw material. The specific dehydration step may include: pumping the liquid displaced in the aging step into an evaporator, heating and gasifying the liquid, then sending the liquid into a pervaporation molecular sieve membrane for dehydration treatment to finally obtain ethanol with the water content of less than 5wt%, and sending the absolute ethanol into a storage tank for later use after cooling. The absolute ethyl alcohol can be circularly applied to the preparation of an organic silicon source solution and the aging and replacement process of the silicon dioxide hydrogel.
And finally, carrying out supercritical drying on the silicon dioxide alcohol gel to obtain the silicon aerogel flame retardant. And the supercritical drying is to place the silicon dioxide aerogel in a supercritical ethanol kettle, add absolute ethanol, seal the drying kettle after purging with nitrogen, heat to 250-270 ℃, keep the pressure for 4-6 h under the pressure of 13-15 MPa, recover to normal pressure, purge for 10min with nitrogen, open the kettle after cooling to room temperature, and take out the silicon aerogel flame retardant prepared by the technical scheme of the invention.
The invention also provides a silicon aerogel flame retardant, wherein ammonium phosphate inorganic salt is uniformly distributed in pores of the aerogel, so that the flame retardance of the aerogel can be improved; meanwhile, the aerogel is not subjected to surface modification treatment, and no redundant organic component is introduced; the aerogel precursor is prepared from a composite precursor formed by an organic silicon source containing methyl, ethyl or vinyl groups and inorganic silica sol, wherein the methyl, ethyl or vinyl groups can endow the aerogel with excellent hydrophobicity, and although the surface modification treatment is not carried out, the hydrophobicity of the aerogel is not reduced; the silicon aerogel flame retardant provided by the invention has the limiting oxygen index of more than or equal to 35 percent, the combustion heat value of less than or equal to 2.2MJ/kg, the heat conductivity of less than or equal to 0.021W/(m.k), and the contact angle of more than or equal to 120 degrees.
The invention also provides application of the silicon aerogel flame retardant in the field of heat insulation materials.
The present invention will be further described with reference to the following specific examples, which should not be construed as limiting the scope of the invention, but rather as providing those skilled in the art with certain insubstantial modifications and adaptations of the invention based on the teachings of the invention set forth herein.
Unless otherwise specified, the following materials, reagents and the like are commercially available products well known to those skilled in the art; unless otherwise specified, all methods are well known in the art. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A silicon aerogel flame retardant and a preparation method thereof are disclosed, the method comprises the following steps:
mixing methyl triethoxysilane, anhydrous ethanol and deionized water according to a molar ratio of 1.
Mixing SiO 2 The silica sol with the mass fraction of 15 percent, the PH value range of 7.5-8.5 and the grain diameter of 4-6 nm is diluted by deionized water to obtain SiO 2 Adding 10% silica sol diluent by mass into 0.01mol/L phosphoric acid as an acid catalyst while stirring, maintaining the temperature of the reaction solution at more than 21 ℃, adjusting the pH value of the solution to 4.0, slowly adding an ethanol solution, and stirring for reacting for 0.5h to obtain a second solution.
And mixing the first solution and the second solution in a volume ratio of 13.
Adding 0.1mol/L ammonia water solution as an alkali catalyst, adjusting the pH value of the solution system to 7.0, and carrying out gelation reaction at the temperature of 45 ℃ to obtain the silicon dioxide hydrogel.
After primary gelation, adding anhydrous ethanol with the same volume, and aging at 45 deg.C for 12h; and replacing water in the pores of the silica hydrogel network with absolute ethyl alcohol, replacing the solution once every 12h, and repeating for 2 times to obtain the silica alcosol.
Placing the silicon dioxide alcohol gel in a supercritical ethanol kettle, adding absolute ethanol, sealing the drying kettle after purging with nitrogen, heating to 250 ℃, keeping the temperature for 4 hours under the pressure of 15MPa, recovering to normal pressure, purging with nitrogen for 10min, cooling to room temperature, and opening the kettle to take out the silicon aerogel flame retardant product.
Pumping the aging displacement liquid into an evaporator, heating and gasifying the aging displacement liquid, then conveying the aging displacement liquid into an infiltration and gasification molecular sieve membrane for dehydration treatment, cooling the final product, and then conveying the final product into a storage tank for later use, wherein the water content of the final product is less than 5 wt%.
The material prepared in the embodiment is tested according to the standard regulations of GB/T10294-2008 ' determination of steady-state thermal resistance and related characteristics of heat-insulating materials ' thermal shield board method ', GB 8624-2012 ' classification of combustion performance of building materials and products ', GB/T14403-2007 ' determination of combustion performance combustion calorific value of building materials and products ' and GB/T24368-2009 ' detection and measurement method of hydrophobic pollutants on glass surface ', and the test results are shown in the following table 1.
Example 2
A silicon aerogel flame retardant and a preparation method thereof are disclosed, wherein the method comprises the following steps:
mixing diethyldiethoxysilane, absolute ethyl alcohol and deionized water in a molar ratio of 1.
Mixing SiO 2 The silica sol with the mass fraction of 30 percent, the PH value range of 7.5-8.5 and the grain diameter of 10-20 nm is diluted by deionized water to obtain SiO 2 Adding 10% silica sol diluent with 0.1mol/L phosphoric acid as an acid catalyst while stirring, maintaining the temperature of the reaction solution at more than 21 ℃, adjusting the pH value of the solution to 3.0, then slowly adding an ethanol solution, and stirring for reaction for 0.5h to obtain a second solution.
And mixing the first solution and the second solution in a volume ratio of 3. And mixing the first solution and the second solution for reaction for 0.5h to obtain the silica hydrosol.
Adding 1.0mol/L ammonia water solution as an alkali catalyst, adjusting the pH value of the solution system to 6.8, and carrying out gelation reaction at 50 ℃ to obtain the silicon dioxide hydrogel.
After primary gelation, adding anhydrous ethanol with the same volume, and aging at 50 deg.C for 24h; and replacing water in the pores of the silica hydrogel network with absolute ethyl alcohol, replacing the solution once every 12 hours, and repeating for 3 times to obtain the silica alcosol.
Placing the silicon dioxide alcohol gel in a supercritical ethanol kettle, adding absolute ethanol, sealing the drying kettle after purging with nitrogen, heating to 255 ℃, keeping for 6 hours under the pressure of 14MPa, recovering to normal pressure, purging with nitrogen for 10min, and cooling to room temperature to obtain the silicon aerogel flame retardant product.
Pumping the aged displacement liquid into an evaporator, heating and gasifying the aged displacement liquid, then sending the aged displacement liquid into a permeable and gasified molecular sieve membrane for dehydration treatment, cooling the product, and then sending the product into a storage tank for later use, wherein the water content of the final product is less than 5 wt%.
The material prepared in this example was tested in the same manner as in example 1. The test results are shown in table 1 below.
Example 3
A silicon aerogel flame retardant and a preparation method thereof are disclosed, wherein the method comprises the following steps:
mixing vinyl ethoxysilane, absolute ethyl alcohol and deionized water according to a molar ratio of 1.
Mixing SiO 2 The silica sol with the mass fraction of 40 percent, the PH value range of 7.5-8.5 and the grain diameter of 8-15 nm is diluted by deionized water to obtain SiO 2 Adding 1.0mol/L phosphoric acid as an acid catalyst into 10% silica sol diluent while stirring, maintaining the temperature of the reaction solution at more than 21 ℃, adjusting the pH value of the solution to 2.0, slowly adding an ethanol solution, and stirring for reaction for 1h to obtain a second solution.
And mixing the first solution and the second solution in a volume ratio of 11. And mixing the first solution and the second solution for reaction for 0.5h to obtain the silica hydrosol.
Adding 10mol/L ammonia water solution as an alkali catalyst, adjusting the pH value of the solution system to 6.5, and carrying out gelation reaction at the temperature of 60 ℃ to obtain the silicon dioxide hydrogel.
After primary gelation, adding anhydrous ethanol with the same volume, and aging at 55 deg.C for 12h; and replacing water in the pores of the silica hydrogel network with absolute ethyl alcohol, replacing the solution once every 12 hours, and repeating for 4 times to obtain the silica alcosol.
Placing the silicon dioxide alcohol gel in a supercritical ethanol kettle, adding absolute ethanol, sealing the drying kettle after purging with nitrogen, heating to 270 ℃, keeping the temperature for 4 hours under the pressure of 13MPa, recovering to normal pressure, purging with nitrogen for 10min, cooling to room temperature, and opening the kettle to take out the silicon aerogel flame retardant product.
Pumping the aged displacement liquid into an evaporator, heating and gasifying the aged displacement liquid, then sending the aged displacement liquid into a permeable and gasified molecular sieve membrane for dehydration treatment, cooling the product, and then sending the product into a storage tank for later use, wherein the water content of the final product is less than 5 wt%.
The material prepared in this example was tested in the same manner as in example 1. The test results are shown in table 1 below.
Comparative example 1
The difference from example 1 is that the aerogel precursor includes only the inorganic silicon source, and the preparation step does not include the preparation of the first solution, and the step of mixing the first solution and the second solution.
The material prepared in this comparative example was tested in the same manner as in example 1. The test results are shown in table 1 below.
Comparative example 2
The difference from example 1 is that the aerogel precursor includes only the source of the organic silicon, and the preparation step does not include the preparation of the second solution, and does not include the step of mixing the first solution and the second solution.
The material prepared in this comparative example was tested in the same manner as in example 1. The test results are shown in table 1 below.
TABLE 1
| Technical index | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Thermal conductivity/W/(m.k) | 0.018 | 0.019 | 0.021 | 0.021 | 0.020 |
| Limiting oxygen index/% | 38 | 42 | 46 | 32 | 34 |
| Heat of combustion (MJ/kg) | 2.12 | 1.83 | 1.57 | 2.53 | 2.33 |
| Contact angle (°) | 142 | 135 | 129 | 0 | 148 |
Through a large number of experimental studies, it can be seen from the test data in table 1 above that, as the phosphoric acid concentration of the acid catalyst increases, for example, the phosphoric acid concentration in example 1 is 0.01mol/L, the phosphoric acid concentration in example 2 is 0.1mol/L, and the phosphoric acid concentration in example 3 is 1mol/L, the flame retardant performance of the prepared silicon aerogel flame retardant is significantly improved, specifically, the flame retardant performance is represented by the increase of the limiting oxygen index and the decrease of the combustion heat value, wherein the limiting oxygen index is increased from 38% to 46%, and the combustion heat value is decreased from 2.12MJ/kg to 1.57MJ/kg; the probable reason is that more phosphoric acid and ammonia water react with the increase of the concentration of the phosphoric acid to generate more ammonium phosphate which is uniformly distributed in the aerogel and the pores of the aerogel, so that the flame retardant property is improved; on the other hand, the thermal conductivity of the aerogel is slightly increased due to more ammonium phosphate filling in the pores of the aerogel, but the requirement of the heat insulation material can still be met on the whole.
Through a large number of experimental studies, it can be seen from the test data in table 1 that, as the content of the inorganic silicon source is increased, the hydrophobic property of the prepared silicon aerogel flame retardant is also decreased, which is specifically shown in that the content of the inorganic silicon source is increased from example 1 to example 3, the contact angle is gradually decreased, and the contact angle is decreased from 142 ° to 129 °; the reason may be that as the content of the inorganic silicon source increases, the content of methyl groups and/or vinyl groups contained in the organic silicon source decreases, thereby decreasing the hydrophobicity of the aerogel.
Features of the invention claimed and/or described in the specification may be combined and are not limited to the combinations specified in the claims. The technical solutions obtained by combining the technical features in the claims and/or the specification are also the protection scope of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the silicon aerogel flame retardant is characterized by comprising the following steps of:
1) Respectively preparing a first solution and a second solution, and uniformly mixing the first solution and the second solution according to a volume ratio of 1-2.5; adding a phosphoric acid catalyst into the organic silicon source solution under stirring to carry out hydrolysis reaction for 1-3 h; adding a phosphoric acid catalyst into the silica sol diluent under stirring, and then adding ethanol to dilute and dissolve the solution for 0.5 to 1 hour; the temperature of the first solution and the second solution is more than or equal to 21 ℃;
2) Adding an alkali catalyst into the silica hydrosol to carry out a gelation reaction to obtain a silica hydrogel;
3) Carrying out aging replacement on the silicon dioxide hydrogel to obtain silicon dioxide alcohol gel;
4) And (4) supercritical drying to obtain the silicon aerogel flame retardant.
2. The method of claim 1, wherein the organic silicon source solution comprises a molar ratio of 1: 8-10: 15-20 parts of organic silicon source, absolute ethyl alcohol and deionized water; the organic silicon source is at least one selected from methyltriethoxysilane, dimethyldiethoxysilane, trimethylethoxysilane, triethylethoxysilane, diethyldiethoxysilane, ethyltriethoxysilane and vinylethoxysilane.
3. The method according to claim 1, wherein the silica sol diluent is SiO 2 Diluting silica sol with the mass fraction of 15-40%, the PH value of 7.5-8.5 and the grain diameter of 4-6 nm, 8-15 nm or 10-20 nm to SiO by deionized water 2 The mass fraction is 10%.
4. The production method according to claim 1, wherein the molar concentration of the phosphoric acid catalyst is 0.01 to 1mol/L; the pH values of the first solution and the second solution are both 2.0-4.0.
5. The preparation method according to claim 1, wherein the base catalyst is an aqueous ammonia solution having a molar concentration of 0.1 to 10 mol/L; the reaction temperature of the gelation reaction is 45-60 ℃.
6. The method of claim 1, wherein the aging step comprises: adding absolute ethyl alcohol with the same volume into the silicon dioxide hydrogel, and aging for 12-24 h at the temperature of 45-55 ℃; then, replacing the liquid in the aging system with absolute ethyl alcohol to perform solvent replacement; the solvent replacement is carried out once every 12h for 2-4 times.
7. The preparation method of claim 1, wherein the supercritical drying is to place the silica alcogel in a supercritical ethanol kettle, add absolute ethanol, seal the drying kettle after purging with nitrogen, heat the drying kettle to 250-270 ℃, maintain the drying kettle at 13-15 MPa for 4-6 h, return to normal pressure, purge with nitrogen for 10min, and cool to room temperature.
8. The method of claim 1, further comprising a waste liquid disposal step of: collecting aged and replaced ethanol, gasifying and dehydrating the ethanol until the water content is less than 5wt%, and cooling for later use.
9. A silicon aerogel flame retardant is characterized in that the limiting oxygen index is more than or equal to 35 percent, the combustion heat value is less than or equal to 2.2MJ/kg, the heat conductivity coefficient is less than or equal to 0.021W/(m.k), and the contact angle is more than or equal to 120 degrees.
10. Use of the silicon aerogel flame retardant according to claim 9 in the field of thermal insulation materials.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587081A (en) * | 2016-12-01 | 2017-04-26 | 伊科纳诺（北京）科技发展有限公司 | Method for preparing hydrophobic hybrid aerosil |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| US20200398243A1 (en) * | 2018-01-24 | 2020-12-24 | Yuxin Wang | Light aerogel material and preparation method thereof |
| CN113980345A (en) * | 2021-11-22 | 2022-01-28 | 航天特种材料及工艺技术研究所 | Method for improving ablation resistance of organic silicon aerogel |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587081A (en) * | 2016-12-01 | 2017-04-26 | 伊科纳诺（北京）科技发展有限公司 | Method for preparing hydrophobic hybrid aerosil |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| US20200398243A1 (en) * | 2018-01-24 | 2020-12-24 | Yuxin Wang | Light aerogel material and preparation method thereof |
| CN113980345A (en) * | 2021-11-22 | 2022-01-28 | 航天特种材料及工艺技术研究所 | Method for improving ablation resistance of organic silicon aerogel |
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