CN103130231B - A kind of silica aerogel material and preparation method thereof - Google Patents
A kind of silica aerogel material and preparation method thereof Download PDFInfo
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- CN103130231B CN103130231B CN201110382030.XA CN201110382030A CN103130231B CN 103130231 B CN103130231 B CN 103130231B CN 201110382030 A CN201110382030 A CN 201110382030A CN 103130231 B CN103130231 B CN 103130231B
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Abstract
The invention provides the novel silica aerogel material and preparation method thereof of a kind of printing opacity, heat-insulation and heat-preservation, sound insulation.Described silica aerogel material has the feature such as the ductile strength of raising, higher transparency, flawless, lightweight low density, especially large bulk.Except the energy-conservation building field such as glass curtain wall, door, window that can be used for heat insulating, sound insulation, 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.
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, the large block silica aerogel material of flawless and preparation method thereof.
Background technology
The gelatinous material of aerogel material to be a kind of dispersion medium be gas, mutually build up by colloidal particle or high-polymer molecular a kind of nanoporous solid material with network structure formed, 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, in calorifics, acoustics, optics, microelectronics, particle detection etc., all have very wide application potential.
There is the aerogel material of higher light transmittance in glass port interlayer, not only can meet daylighting illumination, simultaneously but also can thermal energy exchange inside and outside air lock, there is obvious building energy conservation effect, replace double glazing, vacuum glass in the market, can be used for covil construction door and window, main facilities ceiling etc., the objects such as daylighting in buildings, energy-conservation, sound insulation can be reached.
Based on Normal silica aerogel material achievement in research, also some research reports are had in prepared by printing opacity aerogel, as Nicholas Leventis (Acc Chem Res, 2007,40:874-884) add polyurethane flexible long-chain in the silica wet gel stage and carry out modification, substantially can keep the original lower thermal conductivity of aerogel, light transmission, can also material fragility be reduced.
Chinese patent CN200720077474.1 reports a kind of laminated glass and fills SiO
2aerogel material improves building energy conservation performance, and it reduces fragility, the existence of minimizing crackle of aerogel by being filled with a large amount of inorganic fibres in aerogel material, but greatly affects the transmittance of glass; Chinese patent CN200910193595.6 reports employing acid/alkali two-stage catalysis method Controlling Technology condition and has prepared transparency aerogel thin-film material, but does not report for work and can be used for the transparent agglomerate body aerogel material of laminated glass; Chinese patent CN200720077474.1 reports and adopts oxide nano thread to strengthen the method for aerogel material to have obtained a kind of aerogel material of transparent block, but performances 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 reports and adopts hydrofluoric acid treatment glass surface, and then compound thin layer SiO
2aerogel material, plays and reduces heat conducting energy-conserving action, but be not suitable for laminated glass.
To sum up, though there is the more research report about improving or improve aerosil various aspects of performance, but still have larger gap apart from the requirement of the aerogel material that provides over-all properties good, namely cannot disposable acquisition one not only transparent, flawless but also there is good snappiness, low-density large block aerogel material.Even if Aspen, Cabot company of aerogel most strength is also the polydimethyl silazane (PDMS) of employing with silicon source and the performance of derivative improvement or raising aerosil thereof for energy-saving glass printing opacity, Monolithic aerogel 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 in conjunction with supercritical co dry technology directly obtained aerosil, both enormously simplify preparation technology, again can disposable transparent, the large block silica aerogel material of flawless directly obtaining 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 feature such as the ductile strength of raising, higher transparency, flawless, lightweight low density, especially large bulk.
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 prepared by estersil or silane, alcoholic solvent, deionized water, gel particle structure linking agent, gel hole modifier, catalyzer, hydrophobic modifier.
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 hydrophobic modifier 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 be selected from the combination by one or more in 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 containing the functional groups such as hydroxyl, carboxyl, amino can with the organic polymer of silicone 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 is polyoxypropyleneglycol, polytetrahydrofuran diol, tetrahydrofuran (THF)-propylene oxide copolymer glycols etc. such as.
Wherein, described gel hole modifier is for being selected from by N, one or more combination 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 be selected from one or more the combination in the group that is made up of hydrofluoric acid, ammoniacal liquor, fluoride amine, tetramethyl-aqua ammonia and ammoniacal liquor/hydrochloric acid, and preferably, described catalyzer is ammoniacal liquor or fluoride amine, ammoniacal liquor/hydrochloric acid.
Wherein, described hydrophobic modifier is be selected from one or more the combination in the group that is made up of hexamethyldisilazane, trimethylchlorosilane, dimethyldimethoxysil,ne, dimethyldiethoxysilane, trimethylmethoxysilane, trimethylethoxysilane, preferably, described hydrophobic modifier is hexamethyldisilazane or trimethylchlorosilane.Hydrophobic modifier uses after being mixed with certain density alcoholic solution.
The preparation method of silica aerogel material of the present invention is described estersil or silane, gel particle structure linking agent, gel hole modifier, catalyzer, hydrophobic modifier obtain in conjunction with supercritical co drying process through a step catalysis method sol-gel technology in 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 be selected from one or more the combination in the group that is made up of methyl alcohol, ethanol, n-propyl alcohol and Virahol, is preferably the combination of methyl alcohol, ethanol, methyl alcohol and ethanol, is more preferably ethanol.
The preparation method of silica aerogel material of the present invention specifically comprises the steps:
(1) preparation of colloidal sol-gelling: by estersil or silane, alcoholic solvent, deionized water be in molar ratio 1: 1 ~ 20: 1 ~ 20 mix after, add gel particle structure linking agent and gel hole modifier gradually and stir, the amount being 1: 1 ~ 20 with the mol ratio of estersil or silane and catalyzer again adds catalyzer, obtains silicon sol after stirring; Then in container, after sealing under room temperature or be placed in the baking oven of 10 ~ 60 DEG C, gel is formed by filling for described silicon sol;
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) gel aging, hydrophobization, solvent exchange: by under the gel room temperature of preparation in step (1) or be placed in the aging 12 ~ 120h of baking oven (being preferably 48 ~ 72h) of 10 ~ 60 DEG C (being preferably 30 ~ 50 DEG C); The alcoholic solution of hydrophobic modifier is added, after sealing under room temperature or be placed in the baking oven hydrophobization 12 ~ 120h (being preferably 48 ~ 72h) of 10 ~ 60 DEG C (being preferably 30 ~ 50 DEG C) in this gelling vessel; Solvent system in container is poured out, and pours absolute alcohol solvent submergence gel into, carry out solvent exchange.After 12h, change alcoholic solvent, so repeatedly carry out solvent exchange 2 ~ 10 times, be preferably 5 ~ 7 times;
Wherein, the concentration of the alcoholic solution of described hydrophobic modifier 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 process: 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; At 40 DEG C ~ 80 DEG C, CO 2 medium is made to flow into separating still with 100 ~ 1000L/h flow and be separated with the alcoholic solvent brought into; Be separated with the speed relief pressure of 1 ~ 6MPa/h completely, until pressure in described separating still and ambient atmosphere pressure balanced.
Beneficial effect
(1) aerosil is the network structure of being piled up by silica dioxide granule.Aerosil of the prior art is owing to lacking the connection of effective chemical bond between particle, make its mutual reactive force little, 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, between particle, introduce long flexible chain, strengthen the binding strength of gel space network, reduce material fragility, therefore, the silica aerogel material of acquisition has complete flawless, toughness, large block feature.
(2) transmittance realizing aerogel material is high, must control the size of gel particle and gel hole, when making its particle and bore hole size be less than visible ray half-wavelength, reduces the reflection of visible ray, scattering and refraction.The present invention adopts gel modifier to carry out size control to gel particle and hole, makes its diameter under visible ray half-wavelength, and therefore, the aerogel material of acquisition has the feature of high-clarity.
(3) the present invention adopts a step catalysis method sol-gel technology can obtain the aerogel material with (1), (2) feature, compared with conventional acid-base catalysis two step method sol-gel technology, 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, obtain transparent, flawless, large block silica aerogel material in conjunction with follow-up supercritical co dry technology, meet the requirement that energy-saving glass window is transparent, heat insulation, insulate against sound.
Silica aerogel material prepared by the present invention has low density, lower thermal conductivity, toughness, transparent, flawless, large block feature, except the energy-conservation building field such as glass curtain wall, door, window that can be used for heat insulating, sound insulation, 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 group Beijing Company.Density measurement method is GB/T 5480-2008, and 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 1520g methyl silicate, and after with methyl silicate, methyl alcohol, deionized water, 1: 10: 10 ratio mixes in molar ratio, add gradually methyl silicate, methyl alcohol, deionized water the cetomacrogol 1000 of 1wt% of gross weight 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 add ammoniacal liquor stir after obtain silicon sol at 1: 0.05 by methyl silicate and catalyst molar ratio; Then by filling for silicon sol in the flat plate mold of 400x400mm, seal latter 20 DEG C at leave standstill, form gel after 2h.
(2) gel aging, hydrophobization, solvent exchange: by the gel aged at room temperature 72h of preparation in step (1); The mass percentage adding 3000g in this flat plate mold is that the methanol solution of the hexamethyldisilazane of 5wt% makes the complete submergence of gel, and after sealing, ambient temperatare is put 72h and carried out hydrophobization process; Methanol solvate in container is poured out, and pours anhydrous methanol solvent submergence gel into, carry out solvent exchange.Change methanol solvate after 2 days, so repeatedly carry out solvent exchange 5 times.
(3) supercritical drying process: the gel of preparation in step (2) is taken out and puts into the supercritical co drying that drying kettle carries out following steps: inject 10MPa carbonic acid gas to drying kettle and keep 5h; Be warming up to 50 DEG C gradually, make CO 2 medium flow into separating still with 500L/h flow and be separated with methanol solvate; Be separated with the speed relief pressure of 2MPa/h completely, until pressure in described separating still and ambient atmosphere pressure balanced, obtain silica aerogel material of the present invention thus.
After tested, the aerosil obtained by the present embodiment is of a size of 400x400x20mm, and density is 0.09g/cm
3, room temperature thermal conductivity is 0.011W/mK, visible light transmissivity is 91%, has good toughness without obvious crackle.
The mode identical with embodiment 1 is adopted to carry out embodiment 2 ~ 20.
The raw material that table 1 adopts for each embodiment and ratio condition thereof.
Table 2 each embodiment gel, aging, hydrophobization and CO 2 supercritical drying process condition
The performance perameter of the silica aerogel material that table 3 is obtained by each embodiment
Visible, silica aerogel material prepared by the present invention has low density, lower thermal conductivity, toughness, transparent, flawless, large block feature, except the energy-conservation building field such as glass curtain wall, door, window that can be used for heat insulating, sound insulation, 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 (1)
1. a preparation method for silica aerogel material, it comprises the steps:
(1) colloidal sol-gelling preparation: get 1520g methyl silicate, and after with methyl silicate, methyl alcohol, deionized water, 1: 10: 10 ratio mixes in molar ratio, add gradually methyl silicate, methyl alcohol, deionized water the cetomacrogol 1000 of 1wt% of gross weight 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 add ammoniacal liquor stir after obtain silicon sol at 1: 0.05 by methyl silicate and catalyst molar ratio; Then by filling for silicon sol in the flat plate mold of 400x400mm, seal latter 20 DEG C at leave standstill, form gel after 2h;
(2) gel aging, hydrophobization, solvent exchange: by the gel aged at room temperature 72h of preparation in step (1); The mass percentage adding 3000g in this flat plate mold is that the methanol solution of the hexamethyldisilazane of 5wt% makes the complete submergence of gel, and after sealing, ambient temperatare is put 72h and carried out hydrophobization process; Methanol solvate in container is poured out, and pours anhydrous methanol solvent submergence gel into, carry out solvent exchange; Change methanol solvate after 2 days, so repeatedly carry out solvent exchange 5 times;
(3) supercritical drying process: the gel of preparation in step (2) is taken out and puts into the supercritical co drying that drying kettle carries out following steps: inject 10MPa carbonic acid gas to drying kettle and keep 5h; Be warming up to 50 DEG C gradually, make CO 2 medium flow into separating still with 500L/h flow and be separated with methanol solvate; Be separated with the speed relief pressure of 2MPa/h completely, until pressure in described separating still and ambient atmosphere pressure balanced, obtain silica aerogel material thus.
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| CN102317400A (en) * | 2008-12-18 | 2012-01-11 | 3M创新有限公司 | The method for preparing the hydridization gas gel |
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