CN103130231A - Silica aerogel material and preparation method thereof - Google Patents
Silica aerogel material and preparation method thereof Download PDFInfo
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- CN103130231A CN103130231A CN201110382030XA CN201110382030A CN103130231A CN 103130231 A CN103130231 A CN 103130231A CN 201110382030X A CN201110382030X A CN 201110382030XA CN 201110382030 A CN201110382030 A CN 201110382030A CN 103130231 A CN103130231 A CN 103130231A
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- Prior art keywords
- silane
- gel
- estersil
- aerogel material
- silica aerogel
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- 239000000463 material Substances 0.000 title claims abstract description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002904 solvent Substances 0.000 claims description 41
- 230000001476 alcoholic effect Effects 0.000 claims description 34
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 26
- 229910000077 silane Inorganic materials 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 239000007863 gel particle Substances 0.000 claims description 16
- 239000003607 modifier Substances 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical group CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- -1 polyoxyethylene Polymers 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-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
- 238000003756 stirring Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 238000000352 supercritical drying Methods 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 235000011089 carbon dioxide Nutrition 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- MVHZHMKEBJJTCH-UHFFFAOYSA-N CN(C)C.CO[SiH3] Chemical compound CN(C)C.CO[SiH3] MVHZHMKEBJJTCH-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 claims description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 claims description 2
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical group CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 2
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 abstract description 10
- 239000003208 petroleum Substances 0.000 abstract description 3
- 238000005057 refrigeration Methods 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 33
- 239000000499 gel Substances 0.000 description 28
- 239000004964 aerogel Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 238000009413 insulation Methods 0.000 description 7
- 229910002012 Aerosil® Inorganic materials 0.000 description 6
- 238000004134 energy conservation Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 239000005340 laminated glass Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000012453 solvate Substances 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- IQXJCCZJOIKIAD-UHFFFAOYSA-N 1-(2-methoxyethoxy)hexadecane Chemical compound CCCCCCCCCCCCCCCCOCCOC IQXJCCZJOIKIAD-UHFFFAOYSA-N 0.000 description 1
- 241000183024 Populus tremula Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005815 base catalysis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229950009789 cetomacrogol 1000 Drugs 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Classifications
-
- 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
- Y02P20/10—Process efficiency
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention provides a novel silica aerogel material which is diaphanous, adiabatic, heat-retaining and noise-proof and a preparation method of the silica aerogel material. The silica aerogel material has the advantages of being high in tenacity strength, high in transparency, flawless, light in mass, low in density, especially big in block and the like. The silica aerogel material besides can be used in the field of energy saving buildings such as glass curtain walls, doors and windows which are heat-retaining, adiabatic and noise-proof, can be further used in the fields such as aerospace, petroleum and petrochemical, new energy resources, ships and refrigeration, and has good application prospect.
Description
Technical field
The present invention relates to a kind of silica aerogel material and preparation method thereof, particularly relate to a kind of low density, lower thermal conductivity, toughness, transparent, large block silica aerogel material of flawless and preparation method thereof.
Background technology
Aerogel material is that a kind of dispersion medium is the gelatinous material of gas, mutually to build up by colloidal particle or high-polymer molecular a kind of nanoporous solid material with network structure that consists of, this material has the distinguishing features such as porosity is high, transmittance is high, specific surface area is large, density is little, thermal conductivity is low, at aspects such as calorifics, acoustics, optics, microelectronics, particle detections, very wide application potential is arranged all.
Aerogel material with higher light transmittance is used for the glass port interlayer, but not only can satisfy daylighting illumination, simultaneously but also the inside and outside thermal energy exchange of air lock, has obvious building energy conservation effect, replace in the market double glazing, vacuum glass, can be used for covil construction door and window, main facilities ceiling etc., can reach the purposes such as daylighting in buildings, energy-conservation, sound insulation.
Based on Normal silica aerogel material achievement in research, some research reports are also arranged aspect preparing at the printing opacity aerogel, as Nicholas Leventis (Acc Chem Res, 2007,40:874-884) add the polyurethane flexible long-chain to carry out modification in the silica wet gel stage, the original lower thermal conductivity of aerogel, light transmission can be substantially kept, material fragility can also be reduced.
Chinese patent CN200720077474.1 has reported a kind of laminated glass filling SiO
2Aerogel material improves the building energy conservation performance, and its fragility, minimizing crackle that reduces aerogel by be filled with a large amount of inorganic fibres in aerogel material exists, but greatly affects the transmittance of glass; Chinese patent CN200910193595.6 has reported that employing acid/alkali two-stage catalysis method control processing condition have prepared the transparency aerogel thin-film material, not can be used for the transparent agglomerate body aerogel material of laminated glass but report for work; Chinese patent CN200720077474.1 has reported that the method that adopts oxide nano thread to strengthen aerogel material has made a kind of aerogel material of transparent block, but the performance such as the density of not mentioned material, thermal conductivity, hydrophobicity, snappiness, intensity and whether can be used for energy-saving glass; Japanese Patent JP09098073 has reported employing hydrofluoric acid treatment glass surface, and then compound thin layer SiO
2Aerogel material plays and reduces heat conducting energy-conserving action, but is not suitable for laminated glass.
To sum up, though have more about improving or improve the research report of aerosil various aspects of performance, but apart from providing the requirement of the good aerogel material of over-all properties to still have larger gap, namely can't disposable acquisition a kind of not only transparent, flawless but also have good snappiness, low-density large block aerogel material.Even the Aspen of the tool strength of aerogel, the Cabot company Monolithic aerogel of performance also just adopt polydimethyl silazane (PDMS) and derivative thereof with the silicon source to improve or improve aerosil with printing opacity, to(for) energy-saving glass in the world.The present invention adopts hydroxyl lower molecular weight polymer as aerogel molecular structure properties-correcting agent, adopt the step catalysis method sol-gel technology after optimizing directly to make aerosil in conjunction with the supercritical co dry technology, both greatly simplify preparation technology, can disposablely directly make again transparent, the large block silica aerogel material of flawless of low density, toughness.
Summary of the invention
Therefore, an object of the present invention is to provide the novel silica aerogel material of a kind of printing opacity, heat-insulation and heat-preservation, sound insulation, it has the toughness intensity of raising, higher transparency, flawless, lightweight low density, characteristics such as large bulk especially.
Another object of the present invention is to provide the preparation method of described silica aerogel material.
Silica aerogel material of the present invention is by estersil or silane, alcoholic solvent, deionized water, gel particle structure linking agent, gel hole modifier, catalyzer, hydrophobically modified agent preparation.
Wherein, the mol ratio of described estersil or silane, alcoholic solvent, deionized water, catalyzer is 1: 1～20: 1～20: 1～20; The add-on of gel particle structure linking agent is 0.1～10wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight; The add-on of gel hole modifier is 1～50wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight; The concentration of the alcoholic solution of hydrophobically modified agent is 5～10wt%, and the consumption of alcoholic solution is 50～100wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight.
Wherein, described estersil or silane are one or more the combination of selecting in free methyl silicate, tetraethoxy, methyltrimethoxy silane, Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane; Preferably, described estersil or silane are the combination of methyl silicate, tetraethoxy or two kinds.
Wherein, described gel particle structure linking agent be contain the functional groups such as hydroxyl, carboxyl, amino can with the organic polymer of silicon hydroxyl condensation, it is selected from one or more the combination in polyoxyethylene glycol, polyvinyl alcohol, polyacrylamide, polyacrylic acid, polymethyl acrylic acid, polyether glycol, polyvinylpyrrolidone, polymaleic anhydride, Mierocrystalline cellulose; Preferably, described gel particle structure linking agent is polyoxyethylene glycol, polyvinyl alcohol, polyether glycol, or its combination; Described polyether glycol such as polyoxypropyleneglycol, polytetrahydrofuran diol, tetrahydrofuran (THF)-propylene oxide copolymerization glycol etc.
Wherein, described gel hole modifier is for selecting free N, the combination of one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran (THF), glycerol, Virahol, ethyl acetate, hexanaphthene, hexalin, pimelinketone, quadrol, ketene; Preferably, described gel hole modifier is DMF, N,N-dimethylacetamide, tetrahydrofuran (THF), or its combination.Wherein, described catalyzer is one or more the combination of selecting in the group that free hydrofluoric acid, ammoniacal liquor, fluoride amine, tetramethyl-aqua ammonia and ammoniacal liquor/hydrochloric acid forms, and preferably, described catalyzer is ammoniacal liquor or fluoride amine, ammoniacal liquor/hydrochloric acid.
Wherein, described hydrophobically modified agent is one or more the combination of selecting in the group that free hexamethyldisilazane, trimethylchlorosilane, dimethyldimethoxysil,ne, dimethyldiethoxysilane, trimethylammonium methoxy silane, trimethylethoxysilane form, preferably, described hydrophobically modified agent is hexamethyldisilazane or trimethylchlorosilane.The hydrophobically modified agent is used after being mixed with certain density alcoholic solution.
The preparation method of silica aerogel material of the present invention is that described estersil or silane, gel particle structure linking agent, gel hole modifier, catalyzer, hydrophobically modified agent make in conjunction with the supercritical co drying process through a step catalysis method sol-gel technology in the liquid phase solvent system.
Wherein, described liquid phase solvent system is the mixture of deionized water and alcoholic solvent, and wherein a deionized water part is as solvent, and a part makes estersil or silane generation hydrolysis reaction as reaction raw materials.Described alcoholic solvent is one or more the combination of selecting in the group that free methyl alcohol, ethanol, n-propyl alcohol and Virahol form, and is preferably the combination of methyl alcohol, ethanol, methyl alcohol and ethanol, more preferably ethanol.
The preparation method of silica aerogel material of the present invention specifically comprises the steps:
(1) colloidal sol-gelling preparation: with estersil or silane, alcoholic solvent, deionized water be in molar ratio 1: 1～20: 1～20 mix after, add gradually gel particle structure linking agent and gel hole modifier and stir, amount take the mol ratio of estersil or silane and catalyzer as 1: 1～20 adds catalyzer again, obtains silicon sol after stirring; Then described silicon sol can sealed under rear room temperature in container or be placed in the baking oven of 10～60 ℃, forming gel;
Wherein, the add-on of described gel particle structure linking agent is 0.1～10wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight, is preferably 1～5wt%;
The add-on of described gel hole modifier is 1～50wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight, is preferably 10～20wt%.
(2) aging, the hydrophobization of gel, solvent exchange: with under the gel room temperature of preparation in step (1) or the aging 12～120h of baking oven that is placed in 10～60 ℃ (being preferably 30～50 ℃) (be preferably 48～72h); The alcoholic solution that adds the hydrophobically modified agent in this gelling vessel, after sealing under room temperature or the baking oven hydrophobization 12～120h that is placed in 10～60 ℃ (being preferably 30～50 ℃) (be preferably 48～72h); Solvent system in container is poured out, and poured into absolute alcohol solvent submergence gel, carry out solvent exchange.Change alcoholic solvent through after 12h, so repeatedly carry out solvent exchange 2～10 times, be preferably 5～7 times;
Wherein, the concentration of the alcoholic solution of described hydrophobically modified agent is 5～10wt%, and the consumption of alcoholic solution is 50～100%wt of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight.
(3) supercritical drying is processed: the gel of preparation in step (2) is put into the supercritical co drying that drying kettle carries out following steps: inject 8～16MPa carbonic acid gas to drying kettle; Under 40 ℃～80 ℃, make CO 2 medium flow into separating still and separate with the alcoholic solvent of bringing into 100～1000L/h flow; Separate fully rear speed relief pressure with 1～6MPa/h, until pressure and ambient atmosphere pressure balanced in described separating still.
Beneficial effect
(1) aerosil is to pile up by silica dioxide granule the network structure that forms.Aerosil of the prior art makes its mutual reactive force little due to the connection that lacks effective chemical bond between particle, and internal stress is very large on the contrary, easily broken, formation crackle.And the present invention adopts the organic polymer linking agent mode that increases, introduce long flexible chain between particle, strengthen the binding strength of gel space network, reduce material fragility, therefore, the silica aerogel material of acquisition has complete flawless, toughness, large block characteristics.
(2) realize that the transmittance of aerogel material is high, must control the size of gel particle and gel hole, when making its particle and bore hole size less than the visible light half-wavelength, reduce visible reflection of light, scattering and refraction.The present invention adopts the gel modifier to carry out size control to gel particle and hole, makes its diameter under the visible light half-wavelength, and therefore, the aerogel material of acquisition has the characteristics of high-clarity.
(3) the present invention adopt a step catalysis method sol-gel technology to make to have (1), the aerogel material of (2) characteristics, compare with acid-base catalysis two step method sol-gel technology commonly used, have the advantages that technique is simple, be easy to suitability for industrialized production.The more important thing is that the shortening due to sol-gel process makes gel particle and gel bore hole size be able to better control, make transparent, flawless, large block silica aerogel material in conjunction with follow-up supercritical co dry technology, satisfy that energy-saving glass window is transparent, heat insulation, the requirement of sound insulation.
The prepared silica aerogel material of the present invention has low density, lower thermal conductivity, toughness, transparent, flawless, large block characteristics, except energy-conservation building fields such as the glass curtain wall that can be used for heat insulating, sound insulation, door, windows, also can be used for the fields such as aerospace, petroleum and petrochemical industry, new forms of energy, boats and ships, refrigeration, have a good application prospect.
Embodiment
Estersil used or silane are Aldrich company, and other reagent is reagent company of traditional Chinese medicines groups Beijing Company.The density measurement method is GB/T 5480-2008, and the hydrophobicity testing method is GB/T 5480-2008, and room temperature thermal conductivity testing method is GB/T 13350-2000.
Embodiment 1:
(1) colloidal sol-gelling preparation: get the 1520g methyl silicate, and after mixing with 1: 10: 10 in molar ratio ratio of methyl silicate, methyl alcohol, deionized water, add gradually the cetomacrogol 1000 of 1wt% of gross weight of methyl silicate, methyl alcohol, deionized water as the N of the 10wt% of the gross weight of gel particle structure linking agent and methyl silicate, methyl alcohol, deionized water, dinethylformamide is as gel hole modifier, stir, then be to obtain silicon sol after adding ammoniacal liquor to stir at 1: 0.05 by methyl silicate and catalyst molar ratio; Then the silicon sol can is sealed under rear 20 ℃ standingly in the flat plate mold of 400x400mm, form gel after 2h.
(2) aging, the hydrophobization of gel, solvent exchange: with aging 72h under the gel room temperature of preparation in step (1); The quality percentage composition that adds 3000g in this flat plate mold is that the methanol solution of the hexamethyldisilazane of 5wt% makes the complete submergence of gel, places 72h after sealing under room temperature and carries out hydrophobization and process; Methanol solvate in container is poured out, and poured into anhydrous methanol solvent submergence gel, carry out solvent exchange.Change methanol solvate after 2 days, so repeatedly carry out solvent exchange 5 times.
(3) supercritical drying is processed: the supercritical co drying that drying kettle carries out following steps is put in the gel taking-up of preparation in step (2): inject the 10MPa carbonic acid gas to drying kettle and keep 5h; Be warming up to gradually 50 ℃, make CO 2 medium flow into separating still and separate with methanol solvate with the 500L/h flow; Separate fully rear speed relief pressure with 2MPa/h, until pressure and ambient atmosphere pressure balanced in described separating still obtain silica aerogel material of the present invention thus.
After tested, the prepared aerosil of the present embodiment is of a size of 400x400x20mm, and density is 0.09g/cm
3, the room temperature thermal conductivity is 0.011W/mK, visible light transmissivity is 91%, without obvious crackle and have good toughness.
Adopt the mode identical with embodiment 1 to carry out embodiment 2～20.
The raw material that table 1 adopts for each embodiment and ratio condition thereof.
Each embodiment gel of table 2, aging, hydrophobization and CO 2 supercritical drying process condition
The performance perameter of the silica aerogel material that table 3 is made by each embodiment
As seen, the prepared silica aerogel material of the present invention has low density, lower thermal conductivity, toughness, transparent, flawless, large block characteristics, except energy-conservation building fields such as the glass curtain wall that can be used for heat insulating, sound insulation, door, windows, also can be used for the fields such as aerospace, petroleum and petrochemical industry, new forms of energy, boats and ships, refrigeration, have a good application prospect.
Claims (8)
1. silica aerogel material, it is by estersil or silane, alcoholic solvent, deionized water, gel particle structure linking agent, gel hole modifier, catalyzer, hydrophobically modified agent preparation.
2. silica aerogel material as claimed in claim 1, wherein, the mol ratio of described estersil or silane, alcoholic solvent, deionized water, catalyzer is 1: 1～20: 1～20: 1～20; The add-on of gel particle structure linking agent is 0.1～10wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight; The add-on of gel hole modifier is 1～50wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight; The concentration of the alcoholic solution of hydrophobically modified agent is 5～10wt%, and its consumption is 50～100wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight.
3. silica aerogel material as claimed in claim 1, wherein, described estersil or silane are one or more the combination that is selected from methyl silicate, tetraethoxy, methyltrimethoxy silane, Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane.
4. silica aerogel material as claimed in claim 1, wherein, described gel particle structure linking agent is selected from one or more the combination in polyoxyethylene glycol, polyvinyl alcohol, polyacrylamide, polyacrylic acid, polymethyl acrylic acid, polyether glycol, polyvinylpyrrolidone, polymaleic anhydride, Mierocrystalline cellulose.
5. silica aerogel material as claimed in claim 1, wherein, described gel hole modifier is for being selected from N, the combination of one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran (THF), glycerol, Virahol, ethyl acetate, hexanaphthene, hexalin, pimelinketone, quadrol, ketene.
6. silica aerogel material as claimed in claim 1, wherein, described catalyzer is one or more the combination of selecting in the group that free hydrofluoric acid, ammoniacal liquor, fluoride amine, tetramethyl-aqua ammonia and ammoniacal liquor/hydrochloric acid forms.
7. silica aerogel material as claimed in claim 1, wherein, described hydrophobically modified agent is one or more the combination that is selected from the group that hexamethyldisilazane, trimethylchlorosilane, dimethyldimethoxysil,ne, dimethyldiethoxysilane, trimethylammonium methoxy silane, trimethylethoxysilane form.
8. the preparation method of a silica aerogel material, it comprises the steps:
(1) colloidal sol-gelling preparation: with estersil or silane, alcoholic solvent, deionized water be in molar ratio 1: 1～20: 1～20 mix after, add gradually gel particle structure linking agent and gel hole modifier and stir, amount take the mol ratio of estersil or silane and catalyzer as 1: 1～20 adds catalyzer again, obtains silicon sol after stirring; Then described silicon sol can sealed under rear room temperature in container or be placed in the baking oven of 10～60 ℃, forming gel;
Wherein, the add-on of described gel particle structure linking agent is 0.1～10wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight;
The add-on of described gel hole modifier is 1～50wt% of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight;
(2) aging, the hydrophobization of gel, solvent exchange: with under the gel room temperature of preparation in step (1) or be placed in the aging 12～120h of baking oven of 10～60 ℃; The alcoholic solution that adds the hydrophobically modified agent in this gelling vessel is after sealing under room temperature or be placed in the baking oven hydrophobization 12～120h of 10～60 ℃; Solvent system in container is poured out, and poured into absolute alcohol solvent submergence gel, carry out solvent exchange; Change alcoholic solvent through after 12h, so repeatedly carry out solvent exchange 2～10 times;
Wherein, the concentration of the alcoholic solution of described hydrophobically modified agent is 5～10wt%, and the consumption of alcoholic solution is 50～100%wt of estersil or silane, alcoholic solvent, deionized water and catalyst system gross weight;
(3) supercritical drying is processed: the gel of preparation in step (2) is put into the supercritical co drying that drying kettle carries out following steps: inject 8～16MPa carbonic acid gas to drying kettle; Under 40 ℃～80 ℃, make CO 2 medium flow into separating still and separate with the alcoholic solvent of bringing into 100～1000L/h flow; Separate fully rear speed relief pressure with 1～6MPa/h, until pressure and ambient atmosphere pressure balanced in described separating still.
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Effective date of registration: 20200417 Address after: 215000 3E Industrial Park, No.18, Chunyao Road, Caohu street, Xiangcheng economic and Technological Development Zone, Suzhou City, Jiangsu Province Patentee after: Haiying Aerospace Materials Research Institute (Suzhou) Co., Ltd Address before: 100074, No. 40, Yungang North Lane, Fengtai District, Beijing Patentee before: AEROSPACE RESEARCH INSTITUTE OF SPECIAL MATERIAL AND PROCESS TECHNOLOGY |