CN101450852A - Nano-pore SiO2 aerogel thermal insulation composite material and preparation method thereof - Google Patents
Nano-pore SiO2 aerogel thermal insulation composite material and preparation method thereof Download PDFInfo
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- CN101450852A CN101450852A CNA2008101437439A CN200810143743A CN101450852A CN 101450852 A CN101450852 A CN 101450852A CN A2008101437439 A CNA2008101437439 A CN A2008101437439A CN 200810143743 A CN200810143743 A CN 200810143743A CN 101450852 A CN101450852 A CN 101450852A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 title abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 title abstract 3
- 239000011148 porous material Substances 0.000 title abstract 3
- 235000012239 silicon dioxide Nutrition 0.000 title abstract 3
- 229910052682 stishovite Inorganic materials 0.000 title abstract 3
- 229910052905 tridymite Inorganic materials 0.000 title abstract 3
- 238000009413 insulation Methods 0.000 title description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000835 fiber Substances 0.000 claims abstract description 56
- 239000002002 slurry Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 22
- 239000012530 fluid Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000011240 wet gel Substances 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 54
- 239000010703 silicon Substances 0.000 claims description 54
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 31
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 31
- 239000003054 catalyst Substances 0.000 claims description 28
- -1 silicon alkoxide Chemical class 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical group CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 16
- 239000011858 nanopowder Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- 230000002378 acidificating effect Effects 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 229920002748 Basalt fiber Polymers 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000003365 glass fiber Substances 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 4
- IVWFMGJMTYZKGO-UHFFFAOYSA-N CCO[Si](CC)(CC)OC(C)OC.CN(C)C Chemical compound CCO[Si](CC)(CC)OC(C)OC.CN(C)C IVWFMGJMTYZKGO-UHFFFAOYSA-N 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- MGQFVQQCNPBJKC-UHFFFAOYSA-N dibutoxy(diethyl)silane Chemical compound CCCCO[Si](CC)(CC)OCCCC MGQFVQQCNPBJKC-UHFFFAOYSA-N 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 239000002609 medium Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000002612 dispersion medium Substances 0.000 claims description 2
- 239000003733 fiber-reinforced composite Substances 0.000 claims description 2
- XQMTUIZTZJXUFM-UHFFFAOYSA-N tetraethoxy silicate Chemical group CCOO[Si](OOCC)(OOCC)OOCC XQMTUIZTZJXUFM-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 4
- 230000005855 radiation Effects 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 239000003605 opacifier Substances 0.000 abstract 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 20
- 239000000499 gel Substances 0.000 description 16
- 229960000935 dehydrated alcohol Drugs 0.000 description 11
- 238000000352 supercritical drying Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/56—Opacifiers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a nano-pore SiO2 aerogel heat-insulating composite material and a preparation method thereof. The nano-pore aerogel heat-insulating composite material comprises SiO2 aerogel, an infrared opacifier and reinforced fibers. The preparation method comprises: mixing silicasol and indium-tin oxide ITO nano alcohol slurry or nano composite alcohol slurry of ITO and TiO2 through supersonic wave action, mixing the mixture and the reinforced fibers, directly pouring the mixture into a die to form a wet gel complex, and performing supercutical fluid drying. The material has good heat transfer function and good obstructing function on solid heat conduction, air heat convection and infrared radiation heat conduction, simultaneously has good hydrophobicity, simple technique, low cost and wide application scope, has the mechanical strength reaching more than 1.2 MPa, and can be used in situations with higher heat protection requirement in the fields of avigation, spaceflight, military affairs and domestic use.
Description
Technical field
The invention belongs to the effectively insulating field of heat insulating materials, be specifically related to a kind of nanoporous SiO
2Aerogel heat-insulating composite material and preparation method thereof.
Background technology
SiO
2Aerogel has the feature of high-specific surface area, extremely-low density and nanoporous network structure, and porosity is up to 98.9%, and generally in mesoporous scope, specific surface area is up to 1000m for bore hole size
2/ g, density is at 3～600kg/m
3Adjustable in the scope.The structure specificity of aerogel makes that its specific refractory power, specific acoustic resistance and thermal conductivity are low, good adsorption performance, (Inertial Confinement Fusion ICF) etc. has extremely wide application prospect in the field at optics, acoustics, calorifics, absorption and catalysis and inertial confinement fusion.
SiO
2Aerogel is considered to the solid material of present heat-insulating property the best, but factor such as aerogel material inherent intensity is low, the big shaping difficulty of fragility and cost height have restricted its popularization in engineering is used.The existing technological method that addresses this problem mainly contains following a few class: 1. adopt organic or inorganic tackiness agent and aerogel powder material mixing, by press forming (referring to Chinese patent 95197068.2 " a kind of matrix material, its preparation method and application that contains aerogel ", " 96196879.6 the matrix material that contains aerogel and tamanori, its preparation method and application thereof ").After adding tackiness agent, though can improve the intensity of matrix material to a certain extent, the thermal insulation characteristic of also having lost aerogel material simultaneously; 2. by in the colloidal sol process, inorganic strengthening agent (staple fibre) and infrared light screening agent (titanium dioxide) being added the material (referring to Chinese patent 97106652.3 " modified nanometer heat insulating material and production technique thereof ") that the formation gel forms by supercritical fluid drying again, its infrared light screening agent is difficult to be uniformly dispersed, and physical strength improves limited, is difficult to satisfy the service requirements of severe rugged environment; 3. with fiber as wild phase, adopt so-gel technology, supercritical fluid drying technology to form aerogel composite (referring to U.S. Pat 6068882 and Chinese patent 200510031952.0 " a kind of aerogel heat-insulating composite material and preparation method thereof "), described material has good insulation effect and use properties, but U.S. Pat 6068882 is to reduce infrared breathability by the approach at fiber surface molecule deposition carbon or metal, technology more complicated, Chinese patent 200510031952.0 then are to prepare SiO by in-situ compositing
2/ TiO
2Introduce TiO behind the plural gel
2Reduce infrared breathability in aerogel, though technology is simple with respect to the former, because the TiO that forms
2Be non-crystalline state, it is limited that it reduces the infrared breathability effect more.In addition, the material hydrophobicity that U.S. Pat 6068882 is made is relatively poor, owing to absorb water, insulation effect can reduce in actual use.
Summary of the invention
The object of the present invention is to provide a kind of high thermal insulation, physical strength, good hydrophobic performance, the nanoporous SiO that can in wide temperature range, use preferably
2Aerogel heat-insulating composite material and preparation method thereof.
The objective of the invention is to be achieved through the following technical solutions:
A kind of SiO
2Nano-hole aerogel heat-insulating composite material is to mix the nano-hole aerogel heat-insulating composite material that cast forms by the silicon sol of silicon alkoxide preparation, infrared light screening agent and fortifying fibre, and described infrared light screening agent is to be indium tin oxide ITO nanometer alcohol slurry or the ITO and the TiO of dispersion agent with alcohol
2Nano combined pure slurry; Described fortifying fibre can bear the fiber of supercritical fluid drying condition simultaneously for not reacting with colloidal sol.
The weight ratio of described silicon alkoxide and ITO is: 1:0.005～0.2; The weight ratio of described silicon alkoxide and fortifying fibre is 1:0.3～3.
Described silicon alkoxide and ITO, TiO
2Weight ratio be: 1::0.005～0.2:0.01～0.3.
Described fortifying fibre is basalt fibre, silica fiber, high silica fiber, aluminum silicate fiber, carbon fiber or glass fibre.
Described nanoporous SiO
2The preparation method of aerogel heat-insulating composite material may further comprise the steps: the preparation of (1) silicon sol: with silicon alkoxide, surface-modifying agent, deionized water, alcoholic solvent, and acid and basic catalyst mixed preparing silicon sol; (2) with silicon sol and indium tin oxide ITO nanometer alcohol slurry or ITO and TiO
2Nano combined pure slurry mix and form complex sol, after again fortifying fibre and complex sol being mixed, pour in the mould; (3) contain the fiber-reinforced composite body of wet gel by supercritical fluid drying.
Under the ultrasonic wave effect with silicon sol and indium tin oxide ITO nanometer alcohol slurry or ITO and TiO
2Nano combined pure slurry, fortifying fibre mix.
The silicon sol compound method is as follows: adopt two-step approach, at first with after silicon alkoxide, surface-modifying agent and the alcoholic solvent mixing and stirring, again water and an acidic catalyst are dripped into stirring, after waiting its abundant hydrolysis, again basic catalyst is dripped into stirring and obtain silicon sol, wherein silicon alkoxide: surface-modifying agent: alcoholic solvent: deionized water: an acidic catalyst: the basic catalyst mol ratio is 1:0.1～1:3～10:2～9:0.0008～0.0054:0.0005～0.008.
Described silicon alkoxide is tetraethoxy or methyl silicate; Described surface-modifying agent is the organoalkoxysilane that contains 1-8 C atom; Described alcoholic solvent is methyl alcohol, ethanol, propyl alcohol or Virahol; Described an acidic catalyst is hydrochloric acid, hydrofluoric acid or acetic acid; Described basic catalyst is ammoniacal liquor or sodium hydroxide.
Described surface-modifying agent is a dimethyldiethoxysilane, dimethyldimethoxysil,ne, trimethylammonium methoxy diethyl diethoxy silane, diethyl dibutoxy silane, trimethylchlorosilane.
Described silicon alkoxide is a tetraethoxy, and surface-modifying agent is a dimethyldiethoxysilane, and alcoholic solvent is an ethanol, and an acidic catalyst is a hydrochloric acid, the best when basic catalyst is ammoniacal liquor.
Described ITO nanometer alcohol slurry or ITO and TiO
2Nano combined pure pulp preparation is as follows: with ethanol or Virahol is dispersion medium, by the mechanical ball milling mode with ITO nano-powder material or ITO and TiO
2The composite nano-powder dispersion of materials in ethanol or Virahol, form massfraction and be not higher than 30% aaerosol solution.
Described ITO nano-powder material or ITO and TiO
2The composite nano-powder dispersion of materials best in ethanol.
Described supercritical fluid drying process, its drying medium is ethanol or Virahol, the fiber composite formed body that will contain wet gel is put into supercritical fluid drying equipment, the nitrogen of preliminary filling 2～4MPa, be heated to 250～300 ℃ with 50～100 ℃/hour heat-up rate again, be incubated 1～2 hour, with 1～4MPa/ hour the slow relief pressure of speed, dash with nitrogen at last and swept 10～30 minutes again.
Nanoporous SiO of the present invention
2The aerogel heat-insulating composite material formation comprises SiO
2Aerogel, ITO nano-powder material or ITO and TiO with good infrared external reflection characteristic
2The composite nano-powder material as infrared light screening agent, fortifying fibre; Described fortifying fibre should not react with colloidal sol, simultaneously can bear the fiber of supercritical fluid drying condition, can be basalt fibre, silica fiber, high silica fiber, aluminum silicate fiber, carbon fiber or glass fibre etc., described fortifying fibre be continuous fibre body or staple fibre.
The present invention's nanoporous SiO
2Aerogel heat-insulating composite material prepares with following method: silicon alkoxide, surface-modifying agent, alcoholic solvent, an acidic catalyst, basic catalyst are mixed with silicon sol by a certain percentage, with silicon sol and ITO nano-powder material or ITO and TiO
2The composite nano-powder material mixing form complex sol, after again fortifying fibre and complex sol being mixed, pour in the mould; And then carry out supercritical fluid drying, promptly obtain nanoporous SiO
2Aerogel heat-insulating composite material.Above-mentioned colloidal sol mixed effect under the ultrasonic wave effect is better.
The first-selected tetraethoxy of described silicon alkoxide also can be methyl silicate etc.; The first-selected dimethyldiethoxysilane of described surface-modifying agent also can adopt organoalkoxysilanes such as dimethyldimethoxysil,ne, trimethylammonium methoxy diethyl diethoxy silane, diethyl dibutoxy silane, trimethylchlorosilane; The first-selected ethanol of described alcoholic solvent also can adopt methyl alcohol, propyl alcohol, Virahol etc.; The first-selected hydrochloric acid of described an acidic catalyst also can adopt hydrofluoric acid, acetic acid etc.; The first-selected ammoniacal liquor of described basic catalyst also can adopt sodium hydroxide etc.; Described infrared light screening agent is ITO nano-powder material or ITO and TiO
2The pure slurry of composite nano-powder material, the first-selected ethanol of pure slurry solvent also can adopt Virahol etc., compound concentration is lower than 30%.
Described two-step approach prepare silicon colloidal sol, at first with after silicon alkoxide, surface-modifying agent and the alcoholic solvent mixing and stirring, again water and an acidic catalyst are dripped into stirring, after waiting its abundant hydrolysis, again basic catalyst is dripped into stirring and obtain silicon sol, wherein silicon alkoxide: surface-modifying agent: alcoholic solvent: deionized water: an acidic catalyst: the basic catalyst proportioning is 1:0.1～1:3～10:2～9:0.0008～0.0054:0.0005～0.008 (mol ratio).
Silicon alkoxide: surface-modifying agent: alcoholic solvent: deionized water: an acidic catalyst: basic catalyst mole proportioning is that 1:0.3～0.5:10:3:0.002:0.004 is a preferred proportion.
The preferred mass ratio of ITO and tetraethoxy is: 0.05～0.09:1; ITO, TiO
2, tetraethoxy the preferred mass ratio be: 0.008～0.02:0.07～0.12:1.
Fortifying fibre is that 1:0.9 is a preferred proportion with the ratio of tetraethoxy weight.
With fortifying fibre and ITO nano-powder material or ITO and TiO
2The composite nano-powder material with directly pour in the mould after silicon sol mixes, treat that carrying out supercritical fluid drying again behind its gel promptly gets rigidity nanoporous SiO
2Aerogel heat-insulating composite material.
Described supercritical fluid drying condition optimization is, its drying medium is ethanol or Virahol, the fiber composite wet gel formed body that will contain the ITO nanoparticle is put into supercritical fluid drying equipment, the nitrogen of preliminary filling 2～4MPa, heat-up rate with 50～100 ℃/h is heated to 250～300 ℃ again, be incubated 1～2 hour, with 1～4MPa/ hour the slow relief pressure of speed, dash with nitrogen at last and swept 10～30 minutes again.
Advantage of the present invention:
(1) adopt colloidal sol-gel, supercritical fluid drying prepared nano-hole aerogel material, the porosity height, the aperture is little, and solid heat transfer and convection of air heat transfer are had good iris action;
(2) adopt nanometer infrared light screening agent-indium tin oxide alcohol slurry under the effect of ultrasonic cavitation effect by directly and silicon sol compound after, pass through supercritical fluid drying again, reached infrared light screening agent and SiO
2Aerogel is composite effect preferably, can give full play to nanoporous SiO
2Aerogel can intercept infrared radiation heat transfer again simultaneously effectively to solid heat transfer and the good iris action of convection of air heat transfer;
(3) make behind fiber and the colloidal sol uniform mixing directly cast and supercritical fluid drying technology by ultrasonic technique, between fiber and the fiber by nanoporous SiO
2Aerogel separates, and has reduced the solid conductive heat of fiber itself significantly;
(4) prepare surface-modifying agents such as adding dimethyldiethoxysilane in the colloidal sol process, make SiO in the aerogel
2Nano grain surface forms alkyl, and when use temperature was lower than 400 ℃, product had excellent hydrophobic property, and technology is simple, and cost is low;
(5) the nanoporous SiO of two-step approach preparation
2Aerogel heat-proof composite material, except possessing excellent heat-insulating property, mechanical property is also quite excellent, and physical strength can reach more than the 1.2MPa;
(6) prepared nanoporous SiO
2Aerogel heat-insulating composite material, can satisfy Aeronautics and Astronautics, military affairs and civilian in to the thermal protection requirement than using in the higher occasion.
Embodiment
The invention will be further described by the following examples, but protection domain is not subjected to the restriction of these embodiment.
Embodiment 1
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor 1:0.5:10:3:0.002:0.004 in molar ratio, be made into silicon sol with two-step approach, add 25%ITO ethanol slurry (ITO and tetraethyl silicate weight ratio are 0.09:1) and beta glass fibre (beta glass fibre is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, put into autoclave, preliminary filling N
2To 3.5MPa., be heated to 250 ℃ with the heat-up rate of 60 ℃/h, constant temperature kept temperature-resistant after 1 hour, with the slow relief pressure of speed of 3MPa/h, to the normal pressure with N
2Dash and swept autoclave 30 minutes, powered-down makes its naturally cooling, can make nanoporous SiO
2The rigidity heat insulation composite material, its density is about 0.16g/cm
3, physical strength is about 1.2MPa, and thermal conductivity is 0.016W/mK under the normal temperature and pressure.
Embodiment 2
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor in molar ratio 1:0.3:10:3:0.002:0.004 be made into silicon sol with two-step approach; Add 25%ITO ethanol slurry (ITO is 0.05:1 with the ratio of tetraethoxy weight) and ultra-fine basalt fiber (the ultra-fine basalt fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 3
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor in molar ratio 1:0.3:10:3:0.002:0.004 be made into silicon sol with two-step approach; Add 25%ITO ethanol slurry (ITO is 0.07:1 with the ratio of tetraethoxy weight) and superfine alumina silicate fiber (the superfine alumina silicate fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 4
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor is 1:0.5:10:3:0.002:0.004 in molar ratio, be made into silicon sol with two-step approach, add 25%ITO ethanol slurry (ITO and tetraethoxy weight ratio are 0.08:1) and ultra-fine high silica fiber (ultra-fine high silica fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 5
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor 1:0.5:10:3:0.002:0.004 in molar ratio, be made into silicon sol with two-step approach, add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.02:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.1:1) and beta glass fibre (beta glass fibre is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 6
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor in molar ratio 1:0.3:10:3:0.002:0.004 be made into silicon sol with two-step approach; Add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.01:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.07:1) and ultra-fine basalt fiber (the ultra-fine basalt fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 7
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor in molar ratio 1:0.3:10:3:0.002:0.004 be made into silicon sol with two-step approach; Add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.01:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.1:1) and superfine alumina silicate fiber (the superfine alumina silicate fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 8
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor 1:0.5:10:3:0.002:0.004 in molar ratio, be made into silicon sol with two-step approach, add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.01:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.12:1) and ultra-fine silica fiber (ultra-fine silica fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 9
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor in molar ratio 1:0.3:10:3:0.002:0.004 be made into silicon sol with two-step approach; Add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.008:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.1:1) and ultra-fine basalt fiber (the ultra-fine basalt fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 10
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor in molar ratio 1:0.3:10:3:0.002:0.004 be made into silicon sol with two-step approach; Add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.008:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.1:1) and superfine alumina silicate fiber (the superfine alumina silicate fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Embodiment 11
With tetraethoxy, dimethyldiethoxysilane, dehydrated alcohol, deionized water, hydrochloric acid, ammoniacal liquor 1:0.5:10:3:0.002:0.004 in molar ratio, be made into silicon sol with two-step approach, add 25%ITO/TiO
2(ITO and tetraethoxy weight ratio are 0.009:1 to compound ethanol slurry, TiO
2With the tetraethoxy weight ratio be 0.12:1) and ultra-fine high silica fiber (ultra-fine high silica fiber is 1:0.9 with the ratio of tetraethoxy weight), after ultrasonic mixing in 30 minutes, directly be poured in the mould, treat in ethanolic soln, to wear out 3 days behind its gel, carry out supercritical drying by embodiment 1 described method again, can make the fabulous nanoporous SiO of hydrophobicity
2Aerogel rigidity heat insulation composite material.
Claims (13)
1, a kind of SiO
2Nano-hole aerogel heat-insulating composite material, it is characterized in that, described matrix material is to mix the nano-hole aerogel heat-insulating composite material that cast forms by the silicon sol of silicon alkoxide preparation, infrared light screening agent and fortifying fibre, and described infrared light screening agent is to be indium tin oxide ITO nanometer alcohol slurry or the ITO and the TiO of dispersion agent with alcohol
2Nano combined pure slurry; Described fortifying fibre can bear the fiber of supercritical fluid drying condition simultaneously for not reacting with colloidal sol.
2, according to claim 1 nanoporous SiO
2Aerogel heat-insulating composite material is characterized in that, the weight ratio of described silicon alkoxide and ITO is: 1:0.005～0.2; The weight ratio of described silicon alkoxide and fortifying fibre is 1:0.3～3.
3, according to claim 1 nanoporous SiO
2Aerogel heat-insulating composite material is characterized in that, described silicon alkoxide and ITO, TiO
2Weight ratio be: 1:0.005～0.2:0.01～0.3.
4, a kind of nanoporous SiO according to claim 1
2Aerogel heat-insulating composite material is characterized in that described fortifying fibre is basalt fibre, silica fiber, high silica fiber, aluminum silicate fiber, carbon fiber or glass fibre.
5, the described nanoporous SiO of claim 1
2The preparation method of aerogel heat-insulating composite material is characterized in that, may further comprise the steps: (1) silicon sol preparation: with silicon alkoxide and surface-modifying agent, deionized water, alcoholic solvent, acidity and basic catalyst mixed preparing silicon sol; (2) with silicon sol and indium tin oxide ITO nanometer alcohol slurry or ITO and TiO
2Nano combined pure slurry mix and form complex sol, after again fortifying fibre and complex sol being mixed, pour in the mould; (3) contain the fiber-reinforced composite body of wet gel by supercritical fluid drying.
6, nanoporous SiO according to claim 5
2The preparation method of aerogel heat-insulating composite material is characterized in that, under the ultrasonic wave effect with silicon sol and indium tin oxide ITO nanometer alcohol slurry or ITO and TiO
2Nano combined pure slurry, fortifying fibre mix.
7, according to claim 5 or 6 described nanoporous SiO
2The preparation method of aerogel heat-insulating composite material, it is characterized in that, the silicon sol compound method is as follows: adopt two-step approach, at first with after silicon alkoxide, surface-modifying agent and the alcoholic solvent mixing and stirring, again water and an acidic catalyst are dripped into stirring, after waiting its abundant hydrolysis, again basic catalyst is dripped into stirring and obtain silicon sol, wherein silicon alkoxide: surface-modifying agent: alcoholic solvent: deionized water: an acidic catalyst: the basic catalyst mol ratio is 1:0.1～1:3～10:2～9:0.0008～0.0054:0.0005～0.008.
8, nanoporous SiO according to claim 7
2The preparation method of aerogel heat-insulating composite material is characterized in that, described silicon alkoxide is tetraethoxy or methyl silicate; Described surface-modifying agent is the organoalkoxysilane that contains 1-8 C atom; Described alcoholic solvent is methyl alcohol, ethanol, propyl alcohol or Virahol; Described an acidic catalyst is hydrochloric acid, hydrofluoric acid or acetic acid; Described basic catalyst is ammoniacal liquor or sodium hydroxide.
9, nanoporous SiO according to claim 7
2The preparation method of aerogel heat-insulating composite material is characterized in that, described surface-modifying agent is a dimethyldiethoxysilane, dimethyldimethoxysil,ne, trimethylammonium methoxy diethyl diethoxy silane, diethyl dibutoxy silane, trimethylchlorosilane.
10, according to claim 7 or 8 described nanoporous SiO
2The preparation method of aerogel heat-insulating composite material is characterized in that, described silicon alkoxide is a tetraethoxy, described surface-modifying agent is a dimethyldiethoxysilane, described alcoholic solvent is an ethanol, and described an acidic catalyst is a hydrochloric acid, and described basic catalyst is an ammoniacal liquor.
11, according to claim 5 or 6 described nanoporous SiO
2The preparation method of aerogel heat-insulating composite material is characterized in that, described ITO nanometer alcohol slurry or ITO and TiO
2Nano combined pure pulp preparation is as follows: with ethanol or Virahol is dispersion medium, by the mechanical ball milling mode with ITO nano-powder material or ITO and TiO
2The composite nano-powder dispersion of materials in ethanol or Virahol, form massfraction and be not higher than 30% aaerosol solution.
12, nanoporous SiO according to claim 11
2The preparation method of aerogel heat-insulating composite material is characterized in that, described ITO nano-powder material or ITO and TiO
2The composite nano-powder dispersion of materials in ethanol.
13, nanoporous SiO according to claim 5
2The preparation method of aerogel heat-insulating composite material, it is characterized in that, described supercritical fluid drying process, its drying medium is ethanol or Virahol, and the fiber composite formed body that will contain wet gel is put into supercritical fluid drying equipment, the nitrogen of preliminary filling 2～4MPa, be heated to 250～300 ℃ with 50～100 ℃/hour heat-up rate again, be incubated 1～2 hour, with 1～4MPa/ hour the slow relief pressure of speed, dash with nitrogen at last and swept 10～30 minutes again.
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