CN104030301A - Silicon dioxide aerogel material and preparation method thereof - Google Patents
Silicon dioxide aerogel material and preparation method thereof Download PDFInfo
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- CN104030301A CN104030301A CN201410270352.9A CN201410270352A CN104030301A CN 104030301 A CN104030301 A CN 104030301A CN 201410270352 A CN201410270352 A CN 201410270352A CN 104030301 A CN104030301 A CN 104030301A
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Abstract
The invention relates to a silicon dioxide aerogel material and a preparation method thereof. The method comprises the following steps: by using water glass as silicon source, adding an acid-containing organic solvent free of chlorine ions and fluorine ions to generate a precipitate of sodium ions, potassium ions and other metal salt ions, filtering to remove the precipitate to obtain high-purity silica sol, carrying out a sol-gel process, aging, acidifying, modifying, and drying to obtain the silicon dioxide aerogel material. The acidification before modification enhances the surface reaction activity of the silicon gel, thereby obviously enhancing the modification effect and efficiency. The method has the advantages of low cost and simple and efficient technique, is beneficial to mass high-efficiency production, is free of chlorine ions and fluorine ions in the whole technical process, and enhances the equipment operation safety and reliability; and the product can be used for heat preservation and thermal insulation of nuclear power and liquefied natural gas equipment and pipelines with higher requirement for corrosion resistance, and can also be used for thermal insulation in the field of aerospace, petrochemical engineering, track transportation, ships, automobiles, construction and the like.
Description
Technical field
The present invention relates to a kind of silica aerogel material and preparation method thereof, be particularly related to and take water glass as silicon source, by adding not chloride ion-containing and fluorion containing sour organic solvent, thereby desalination obtains high-purity silicasol fast, again through sol-gel, aging, acidifying, modification, drying process, thereby obtain aerogel material.This aerogel material is chloride ion-containing and fluorion not, the heat-insulation and heat-preservation of the nuclear power that can be used for protection against corrosion to have relatively high expectations and liquefied natural gas facility and pipeline, can also be for the insulation in the fields such as aerospace, petrochemical industry chemical industry, track traffic, boats and ships automobile, refrigerator freezer, building.
Background technology
Aerogel is a kind of novel nano thermal insulation material, 1931 Nian You U.S. Kistler.S. inventions, " blue smoke ", " cigarette freezing " are otherwise known as, be known as the magical material that changes the world, having classified one of 10 big hot topic science and technology since the nineties in 20th century as, is to have the dual-use technology that huge applications is worth.
Aerogel has with nanometer scale ultrafine particle mutually to be assembled and forms nanoporous network structure, and porosity is up to 80～99.8%, and density can lowly reach 0.003g/cm
3, room temperature thermal conductivity can lowly reach 0.013w/ (mk), and use temperature can reach 1300 ℃, is the lightest up to now solid material and heat-insulating property best material, is called as super insulating material, can be widely used in the adiabatic heat-insulation in each field.
The aerogel material of selling in the market, many employing tetraethoxys are silicon source, trimethylchlorosilane is done hydrophobically modified agent, although technical maturity, quality is better, but organosilicon fancy price has still had a strong impact on application and the popularization of aerogel material, and the high-efficiency insulated needs in the fields such as nuclear power and the natural gas liquids aerogel material of chloride ion-containing and fluorion not, on current market, product is also difficult to meet the demands.
Water glass silicon source, due to the raw material cheapness that is easy to get, is subject to researchist's extensive concern, especially for water glass silicon source, prepares in aerogel material process, how to remove sodium ion and all kinds of impurity has carried out a large amount of developments.
Patent CN1087271C(ZL96198951.3) preparation method of the organically-modified aerogel of the salt precipitation that can make formation is disclosed, its method of removing salinity in water glass is, now by water glass and acid-respons, the acidic silicasol that generation is contained salt, then this silicon sol is cooled to 0 ~ 30 ℃, particularly preferably 0 ~ 5 ℃, then because the solubleness of salinity under low temperature in the aqueous solution reduces and separates out from silicon sol.Then use filtration unit to divide isolated precipitation.
Patent CN1126591C(ZL97181105.9) method of organically-modified aerogel is disclosed, its method of removing salinity in water glass is, first under acidic ion exchange resin, mineral acid or hydrochloric acid solution's effect, water glass solution is adjusted to pH<3, by adding alkali to carry out the silicic acid of polycondensation gained, form aerosil.Wash afterwards gel with water, to dissociate wherein all ionogen.
Patent CN200710175741.3 discloses a kind of low-cost preparation SiO
2the method of aerogel microball, its method of removing salinity in water glass is, volume ratio 35 ~ 3:1 by water and water glass dilutes, and then join in sodium type strong acid type styrene type cation exchange resin and stir 10 minutes, more extremely neutral through deionized water or distilled water wash.
Patent CN200880010090.5 discloses method and the hydrophobic aerogel prepared therefrom of preparing hydrophobic aerogel, its method of removing salinity in water glass is, at room temperature water glass (water glass) is joined in hydrochloric acid l, until the pH of solution is adjusted to 3～4; Again by adding nonionogenic tenside and water glass to make, under the acidic conditions of solution in pH 4～6, to form silicon gel, the silicon gel then forming with distilled water wash.
Patent CN 200810011646.4 discloses a kind of TiO
2-SiO
2composite aerogel and preparation method thereof, its method of removing salinity in water glass is, by the service water glass of modulus 3.38 and deionized water 1:4 dilution by volume, then with strongly acidic styrene's Zeo-karb, to carry out ion-exchange.
Patent CN201110107204.1 discloses a kind of method of preparing aerosil, and in its removal water glass, method of salinity is: water glass is joined in hydrochloric acid and reacted, until the pH of solution is adjusted to 3～4, form silica hydrogel; Described silica hydrogel is placed in to one and is placed with in the container of water, described container two ends connect respectively positive and negative electrode the desalination of switching on.
Open and the enforcement of above-mentioned patent will be conducive to the propelling of water glass silicon source aerogel material exploitation, but still have many problems.Aerogel material is prepared in above-mentioned disclosed water glass silicon source, and removing salinity in water glass and the method for impurity must have following four kinds: 1) low temperature crystallization method.This method need to be carried out refrigeration cool-down to colloidal sol, and energy consumption is larger, under low temperature, can not guarantee that salinity separates out completely simultaneously, even if at 0 ℃, the solubleness of sodium sulfate in water also has 4.9g/100g water; 2) ion exchange method.Adopt storng-acid cation exchange resin to remove the metal ions such as sodium ion in water glass.Due to Zeo-karb finite capacity (being generally 5mmol/g), this method test rank still can, if suitability for industrialized production, the sodium at high concentration ion in water glass (content is 7.5 ~ 12.8% wt) can cause ion exchange resin exchange capacity saturated rapidly, cannot produce continuously at all; 3) deionized water or distillation washing.This method is by washing, constantly to be diluted and removed salinity in gel after gel formation.Can realize suitability for industrialized production, shortcoming is large, the consuming time length of water loss, and the brackish water treatment capacity washing out is large.4) electrode desalination.This method is also after gel formation, utilizes the electrolytical characteristic of salinity to carry out positive and negative electrode desalination.The difficulty that this method faces and the sea water desaltination of electrode method are similar, are difficult to find jumbo cheap electrode.
The disclosed preparation method of above-mentioned patent goes back the situation that ubiquity is used hydrochloric acid or hydrofluoric acid, and properties-correcting agent also generally adopts the chloro-containing reagents such as trimethylchlorosilane.According to national relevant industries standard, the lagging material of chloride ion-containing and fluorion is strictly limited the use of in the heat insulating work of austenitic steel equipment and pipeline, in the projects such as nuclear power and natural gas liquids, forbid especially to use, this will affect the promotion and application of aerogel material.
The deficiency of preparing the desalination mode of aerogel material for above-mentioned water glass, the present invention proposes new desalination mode, and method is simple, efficiency is high, cost is low.The whole technological process of the present invention simultaneously does not contain chlorion and fluorion, the product making can be applicable to the insulation of the e-quipment and pipe in nuclear power and natural gas liquids field, can also be for the insulation in the fields such as aerospace, petrochemical industry chemical industry, track traffic, boats and ships automobile, building.
Summary of the invention
For solving traditional water glass silicon source, prepare in aerogel material technique, impurity is more, except salinity process loaded down with trivial details consuming time, contain the problems such as chlorion fluorion, a kind of silica aerogel material and preparation method thereof has been proposed, it comprises following step:
(1) after water glass is diluted with pure water, mix with the organic solvent containing sour, then remove the precipitation of generation, obtain high-purity acidic silicasol;
(2) with alkali, finely tune the pH value of above-mentioned acidic silicasol, direct standing formation gel or be compounded to form plural gel with fiber, opalizer is standing aging;
(3) above-mentioned gel is soaked with acidic substance, carry out acidifying;
(4) with hydrophobically modified agent, the gel after to acidifying carries out hydrophobically modified;
(5) gel is dried and obtains aerogel material, comprise supercritical drying or constant pressure and dry or microwave vacuum drying.
The described water glass of step (1) dilutes with pure water, and the volume ratio of water glass and pure water is 1:0.1 ~ 20, preferably 1:0.5 ~ 10; Water glass comprises potash water glass and sodium silicate.
The described acid of step (1) be the mineral acid of not chloride ion-containing and fluorion or organic acid one or more.Mineral acid comprises oxygen acid, oxygen-free acid, complex acid, preferably sulfuric acid and phosphoric acid; Organic acid comprises carboxylic acid (COOH), sulfonic acid (SO
3h),-sulfinic acid (RSOOH), thionothiolic acid (RCOSH), preferably oxalic acid, acetic acid, formic acid, propionic acid, butanic acid, positive valeric acid.
The described organic solvent of step (1) is one or more in alcohol, ether, ester, ketone, aliphatic series or aromatic hydrocarbon, in preferred molecular structure, carbonatoms is less than 8, particularly preferably methyl alcohol, ethanol, ethylene glycol, propyl alcohol, glycerol, vinylcarbinol, acetone, formaldehyde, acetaldehyde, propionic aldehyde.
After the dilution of the described water glass of step (1) with containing sour organic solvent, mixes, can be first to mix with acid after water glass dilution, then mix with organic solvent, can be also sourly first to mix with organic solvent, then with dilute rear water glass and mix.
The precipitation of the described generation of step (1) adopts the mode of filtering to remove, and comprises centrifuging, vacuum filtration, pressure filtration.
After the dilution of the described water glass of step (1), be 0.1 ~ 4 with mix the pH value of the acidic silicasol of gained afterwards containing sour organic solvent, preferably 1.5 ~ 3.5.
Step (2) described with alkali finely tune above-mentioned acidic silicasol pH value, pH value is 3.0 ~ 7.0, alkali is one or more in sodium hydroxide, potassium hydroxide, calcium hydroxide and ammoniacal liquor.
Step (2) described with alkali finely tune above-mentioned acidic silicasol pH value after, form plural gel with fiber composite, described fiber comprise inorganic fibre and organic fibre one or more, and above-mentioned fiber is made felt, plate, cloth etc.; Organic fibre comprises terylene, polyamide fibre, spandex, acrylic fibers, aramid fiber, tynex, pre-oxidized polyacrylonitrile fiber, Kafra fiber, cellulosic fibre, carbon fiber, and inorganic fibre comprises silica fiber, high silica fiber, aluminum silicate fiber, glass fibre, mullite fiber, silicon carbide fiber, silicon nitride fiber, sapphire whisker, boron nitride fibre, basalt fibre, brucite fiber, attapulgite fiber.
Step (2) is described finely tunes with alkali after the pH value of above-mentioned acidic silicasol, is compounded to form plural gel with opalizer, and described opalizer is one or more in titanium dioxide, metatitanic acid, titanyl sulfate, zirconia titanate, zirconium dioxide, zirconium silicate, carbon black.
The described acidic substance of step (3) can be the acid that step (1) is mentioned, and can be also the mixtures of the organic solvent mentioned of the acid mentioned of step (1) and step (1).
The gel hydrophobically modified agent that step (4) is described, for the waterproofing agent of organosilicon with silicon methyl structural of chloride ion-containing and fluorion not, preferably hexamethyldisilazane, hexamethyldisiloxane, methyl trimethoxy base silane, Union carbide A-162, dimethyldiethoxysilane, dimethyldimethoxysil,ne, trimethylethoxysilane, trimethylammonium methoxy silane.
The supercritical drying that step (5) is described, drying medium comprises ethanol or carbonic acid gas; Described constant pressure and dry, comprises warm air drying and infrared drying, and the drying medium of warm air drying is air, nitrogen or carbonic acid gas, preferred nitrogen and carbonic acid gas; Described microwave vacuum drying, dry front equipment vacuum degree should be lower than 100 holders, preferably lower than 10 holders.
As previously mentioned, water glass is prepared aerogel material as silicon source, remove sodium ion or potassium ion and other impurity is the direction of researchist's unremitting effort always, the present invention utilizes most of sodium salts, sylvite, molysite and aluminium salt to be all insoluble to the characteristic of organic solvent, by forming salinity after diluted water glass is mixed with acid, in organic solvent, separate out, precipitate, filter, thereby obtain deionized acidic silicasol.
In the described organic solvent preferred molecular structure of step (1), carbonatoms is less than 8, particularly preferably methyl alcohol, ethanol, ethylene glycol, propyl alcohol, glycerol, vinylcarbinol, acetone, formaldehyde, acetaldehyde, propionic aldehyde, it is water-soluble to be preferably that above-mentioned organic solvent has, and when separating out salinity, can dissolve each other and become one with silicon sol.
For convenience of understanding, the situation of mixing with sodium silicate and sulfuric acid here describes.The main component of sodium silicate is water glass, and contains a small amount of iron ion, aluminum ion and other metal ions.After water glass mixes with sulfuric acid, can generate nano level hydrated SiO 2, silicon sol generates a large amount of sodium sulfate and a small amount of ferric sulfate, Tai-Ace S 150 simultaneously.These three kinds of vitriol are all soluble salts in water, its solubleness in 20 ℃ of water is respectively 19.5g/100g water, 440g/100g water, 36.4g/100g water, but these three kinds of salt are all dissolved in the organic solvents such as ethanol hardly, in silicon sol, ethanol content reaches more than 5% and separates out with regard to having a large amount of vitriols, even if the sodium sulfate that when alcohol concn reaches 70%, content is 200ppm also can be separated out.By organic solvents such as ethanol, just the salt of silicon sol can be analyzed like this, then remove precipitation by filtration, thereby reach the object except freshen impurity.
The silicon sol containing organic solvent of preparing in the present invention must be acid system, otherwise organic solvent may cause the rapid gel of silicon sol and cannot separate out salinity.The pH value of silicon sol is controlled at 0.1 ~ 4th, in order to obtain the silicon sol that can preserve the long period, so that the work of follow-up filtration desalination.PH value preferably 1.5 ~ 3.5th is introduced alkali when next regulating pH value to facilitate gel as far as possible less, avoids producing new impurity effect quality product.
Solvent exchange in aerogel preparation process and modifying process are often very loaded down with trivial details, consume a large amount of manpower and materials, and have seriously elongated the cycle of producing, and affect production efficiency.In the present invention, organic solvent has just been introduced in preparing the process of silicon sol, also avoided in traditional technology after desalination will be repeatedly solvent exchange.
In the present invention, the gel of acquisition is carried out in advance before hydrophobically modified to acidifying, acidization not only can play and promote the aging effect of gel, also can improve the activity of gel surface silicon hydroxyl, at silicon hydroxyl surface, forms H
+electric charge, simultaneously properties-correcting agent can generate highly active silanol (containing-OH) in sour environment, thereby has accelerated reacting of properties-correcting agent and silicon hydroxyl, and express delivery completes gel modification up hill and dale, realize efficiently high-quality production.
At most of water glass, be that prepare in the research invention and document of aerogel in silicon source, acid used mostly is hydrochloric acid or hydrofluoric acid, hydrophobically modified agent used mostly is trimethylchlorosilane, although also can prepare the aerogel of heat-proof quality excellence, but due to the impact of chlorion and fluorion, cannot obtain application in fields such as nuclear power, natural gas liquids.The acid that the present invention is used and hydrophobic modification agent do not contain chlorion and fluorion, and this has just been avoided these two kinds of element corrosion to the field devices such as nuclear power, natural gas liquids and pipeline from source, be conducive to client's safety in production.The preferred acid of the present invention is sulfuric acid and phosphoric acid, and reason is the most common and safety of this two classes acid, and price is comparatively cheap.Preferably nitric acid reason is not that nitric acid character is too active, and easy and organic solvent generation vigorous reaction is dangerous.
Pure aerogel foreign matter content prepared by the present invention is few, transparency is high, and indices is suitable with organosilicon source aerogel.In the present invention, silicon sol and filamentary material and opalizer can obtain the aerogel composite of various forms and purposes after compound.
Medium preferred nitrogen or two kinds of inert medias of carbonic acid gas when constant pressure and dry of the present invention adopts warm air drying, be to contact with oxygen for fear of the organic solvent in aerogel, raising security; The present invention adopts microwave drying can obtain higher drying efficiency, adds that vacuum combination can avoid microwave in container because point discharge effect occurs that spark brings potential safety hazard, and simultaneously under vacuum, dry efficiency further improves.
beneficial effect.
Compared with prior art, the aerogel material that prepared by the present invention has following significant advantage.
(1) utilize most salt to be all insoluble to the characteristic of organic solvent, the a large amount of sodium ions or the potassium ion that in removal water glass silicon source that can be simple and quick, contain, the a small amount of iron ion containing in water glass, aluminum ion etc. also can be removed rapidly, thereby obtain the higher aerogel material of purity.
(2) precipitation filtering out directly becomes solid materials, can be used as solid waste treatment, also can be used as technical grade industrial chemicals and sell, avoided traditional washing deionization to consume a large amount of water resourcess, the saline pollution need for environment that washes out carries out wastewater treatment again, wastewater treatment concentrated solution also needs evaporate to dryness to become the series of problems such as solid again.
(3) organic solvent is just introduced at sol phase, can save the solvent exchange link of traditional water glass silicon source technique after deionization, has saved the time, has also greatly reduced replacement solvent amount simultaneously, has reduced cost.
(4) the present invention first carries out acidification to gel before hydrophobically modified, has improved the reactive behavior of silicon gel surface, thereby has significantly improved effect and the efficiency of modification, is conducive to high efficiency production in enormous quantities.
(5) the aerogel material whole process that prepared by the present invention does not contain chlorion and fluorion, fundamentally avoided the corrosion to e-quipment and pipe of chlorion and fluorion, both the safety and reliability that had improved equipment operation in aerogel production process, makes again to obtain aerogel product and can be applied to the field to protection against corrosion requirement harshness such as nuclear power, natural gas liquids.
(6) gel that hydrophobically modified of the present invention completes can carry out supercritical drying or constant pressure and dry or microwave vacuum drying, and preparation technology has stronger adaptive faculty to different drying modes.
(7) the pure aerogel of silicon-dioxide that prepared by the present invention, density is 50 ~ 120kg/m
3, specific surface area is 530 ~ 850m
2/ g, transparency approaches pure aerogel prepared by organosilicon silicon source; Aerosil fibre composite prepared by the present invention, density is 150 ~ 360kg/m
3, thermal conductivity is 0.017 ~ 0.025w/mk, water-intake rate is less than 2%.
Embodiment
Provide the embodiment of silica aerogel material below, as the present invention is described in more detail.
Embodiment 1.
Take the sodium silicate 80g of modulus 3.3, add pure water 60g to stir, obtain dilution water glass.Taking concentration is the sulfuric acid 20g of 40%wt, then while stirring dilution water glass is joined in sulfuric acid, until pH value is 3.Continue to add while stirring the ethanol 300g of 95%wt.With centrifugal filter, remove the precipitation in colloidal sol, obtain the silicon sol of transparent clarification.In silicon sol, drip the ammoniacal liquor that concentration is 1%wt, regulate pH to 4.1, gel after 50min, the standing aging 5h of room temperature.Aging good gel is inserted to 500ml, and soaking at room temperature 3h in the 40%wt sulfuric acid that mass ratio is 2:8 and 95% alcohol mixeding liquid, carries out acidifying.The gel that completes acidifying is inserted in the hexamethyldisilazane of 500ml, under room temperature, carry out hydrophobic modification.6h post-modification completes, and gel is carried out to supercritical drying 10h, and drying medium is ethanol, and temperature is 260 ℃, and pressure is 8Mpa.Gained aerogel is translucent particle, density 60kg/m
3, specific surface area 760m
2/ g.
Embodiment 2.
Take the sodium silicate 80g of modulus 3.6, add pure water 80g to stir, obtain dilution water glass.Taking concentration is the phosphoric acid 25g of 30%wt, then while stirring dilution water glass is joined in phosphoric acid, until pH value is 2.3.Continue to add while stirring the methyl alcohol 300g of 95%wt.With vacuum filter, remove the precipitation in colloidal sol, obtain the silicon sol of transparent clarification.In silicon sol, drip the sodium hydroxide that concentration is 1%wt, regulate pH to 4.3, gel after 30min, 40 ℃ of standing aging 6h.Aging good gel is inserted to 500ml, in the 40%wt sulfuric acid that mass ratio is 3:7 and propyl alcohol mixed solution, at 35 ℃, soak 3h, carry out acidifying.The gel that completes acidifying is inserted in the dimethyldiethoxysilane of 500ml, carry out hydrophobic modification at 50 ℃.8h post-modification completes, and gel is carried out to nitrogen warm air drying 5h, and nitrogen temperature is 80 ℃.Gained aerogel is translucent particle, density 70kg/m
3, specific surface area 640m
2/ g.
Embodiment 3.
Take the potash water glass 80g of modulus 3.3, add pure water 100g to stir, obtain dilution water glass.Taking concentration is the acetic acid 10g of wt 50%, then while stirring dilution water glass is joined in acetic acid, until pH value is 3.Continue to add while stirring acetone 300g.With pressurization titanium rod filter, remove the precipitation in colloidal sol, obtain the silicon sol of transparent clarification.Toward dripping concentration in silicon sol, be 1% potassium hydroxide, regulate pH to 3.7, add titanium dioxide opacifier to stir, pour in the box that is covered with fiberglass needled mat gel after 90min, 25 ℃ of aging 7h into.Aging good gel is inserted to 500ml, in 40% oxalic acid that mass ratio is 2:8 and dehydrated alcohol mixed solution, at 25 ℃, soak 3.5h, carry out acidifying.The gel that completes acidifying is inserted in the hexamethyldisiloxane of 500ml, 50 ℃ are carried out hydrophobic modification.7h post-modification completes, and gel is carried out to microwave vacuum drying, before being dried, microwave vacuum dryer is evacuated down to 10
-below holder.Obtain aerogel glass composite felt, density 210kg/m
3, thermal conductivity 0.018w/mk, water-intake rate 1.8%.
Embodiment 4.
Take the sodium silicate 80g of modulus 2.4, add pure water 10g to stir, obtain dilution water glass.Taking concentration is the sulfuric acid 20g of 40%wt, then while stirring dilution water glass is joined in acid, until pH value is 3.Continue to add while stirring anhydrous acetaldehyde 400g.With centrifugal filter, remove the precipitation in colloidal sol, obtain the silicon sol of transparent clarification.In silicon sol, drip the ammoniacal liquor that concentration is 2%wt, regulate pH to 4.5, pour in the box that is covered with polyster fibre eedle-punched non-wovens gel after 20min into, standing aging 15h.On aging good gel, pour 100ml into, 40% acetic acid soaks 3h, carries out acidifying.The gel that completes acidifying is inserted in the trimethylammonium methoxy silane of 500ml, carry out hydrophobic modification.6h post-modification completes, and gel is carried out to supercritical drying 10h, and drying medium is carbonic acid gas, and temperature is 40 ℃, and pressure is 10Mpa.Obtain aerogel terylene composite felt, density 180kg/m
3, thermal conductivity 0.017w/mk, water-intake rate 1.2%.
Embodiment 5.
Take the sodium silicate 80g of modulus 3.3, add pure water 160g to stir, obtain dilution water glass.Taking concentration is the oxalic acid 10g of 10%wt and the sulfuric acid 20g of 40%wt, then while stirring dilution water glass is joined in acid, until pH value is 3.Continue to add while stirring the ethanol 300g of 95%wt.With vacuum filter, remove the precipitation in colloidal sol, obtain the silicon sol of transparent clarification.In silicon sol, drip the sodium hydroxide that concentration is 2%wt, regulate pH to 4.1, add titanyl sulfate opalizer to stir and pour in the box that is covered with sapphire whisker plate, gel after 50min, 90 ℃ of standing aging 10h.Aging good gel is inserted to 500ml, in the 40%wt phosphoric acid that mass ratio is 1:9 and propyl alcohol mixed solution, at 70 ℃, soak 3h, carry out acidifying.The gel that completes acidifying is inserted in the methyl trimethoxy base silane of 500ml, carry out hydrophobic modification at 60 ℃.6h post-modification completes, and gel is placed in to dry 5h under infrared lamp.Obtain aerogel sapphire whisker composition board, density 350kg/m
3, thermal conductivity 0.023w/mk, water-intake rate 1.9%.
The above, be only preferred embodiment of the present invention, not the present invention done to any type of restriction.Any simple modification, equivalent variations and modification that every foundation technology of the present invention and method essence are done above embodiment, all still belong in the scope of technology of the present invention and method scheme.
Claims (10)
1. silica aerogel material and preparation method thereof, is characterized in that, this silica aerogel material preparation process comprises the following steps:
(1) after water glass is diluted with pure water, mix with the organic solvent containing sour, then remove the precipitation of generation, obtain high-purity acidic silicasol;
(2) with alkali, finely tune the pH value of above-mentioned acidic silicasol, direct standing formation gel or be compounded to form plural gel with fiber, opalizer is standing aging;
(3) above-mentioned gel is soaked with acidic substance, carry out acidifying;
(4) with hydrophobically modified agent, the gel after to acidifying carries out hydrophobically modified;
(5) gel is dried and obtains aerogel material, comprise supercritical drying or constant pressure and dry or microwave vacuum drying.
2. silica aerogel material claimed in claim 1, is characterized in that the described water glass of step (1) dilutes with pure water, and the volume ratio of water glass and pure water is 1:0.1 ~ 20, preferably 1:0.5 ~ 10; Described water glass comprises potash water glass and sodium silicate.
3. silica aerogel material claimed in claim 1, it is characterized in that mineral acid that the described acid of step (1) is not chloride ion-containing and fluorion or organic acid one or more; Mineral acid comprises oxygen acid, oxygen-free acid, complex acid, preferably sulfuric acid and phosphoric acid; Organic acid comprises carboxylic acid (COOH), sulfonic acid (SO
3h),-sulfinic acid (RSOOH), thionothiolic acid (RCOSH), preferably oxalic acid, acetic acid, formic acid, propionic acid, butanic acid, positive valeric acid.
4. silica aerogel material claimed in claim 1, it is characterized in that the described organic solvent of step (1) is one or more in alcohol, ether, ester, ketone, aldehyde, aliphatic series or aromatic hydrocarbon, in preferred molecular structure, carbonatoms is less than 8, particularly preferably methyl alcohol, ethanol, ethylene glycol, propyl alcohol, glycerol, vinylcarbinol, acetone, formaldehyde, acetaldehyde, propionic aldehyde.
5. silica aerogel material claimed in claim 1, is characterized in that the precipitation of the described generation of step (1) adopts the mode of filtering to remove, and comprises centrifuging, vacuum filtration, pressure filtration.
6. silica aerogel material claimed in claim 1, is characterized in that after the described water glass dilution of step (1) be 0.1 ~ 4 with mix the pH value of the acidic silicasol of gained afterwards containing sour organic solvent, preferably 1.5 ~ 3.5.
7. silica aerogel material claimed in claim 1, it is characterized in that step (2) described with alkali finely tune above-mentioned acidic silicasol pH value, pH value is 3.0 ~ 7.0, and described alkali is one or more in sodium hydroxide, potassium hydroxide, calcium hydroxide and ammoniacal liquor.
8. silica aerogel material claimed in claim 1, is characterized in that the described acidic substance of step (3) can be the acid that step (1) is mentioned, and can be also the mixture of the organic solvent mentioned of the acid mentioned of step (1) and step (1).
9. silica aerogel material claimed in claim 1, it is characterized in that the gel hydrophobically modified agent that step (4) is described, for the waterproofing agent of organosilicon with silicon methyl structural of chloride ion-containing and fluorion not, preferably hexamethyldisilazane, hexamethyldisiloxane, methyl trimethoxy base silane, Union carbide A-162, dimethyldiethoxysilane, dimethyldimethoxysil,ne, trimethylethoxysilane, trimethylammonium methoxy silane.
10. silica aerogel material claimed in claim 1, is characterized in that the supercritical drying that step (5) is described, and drying medium comprises ethanol or carbonic acid gas; Described constant pressure and dry, comprises warm air drying and infrared drying, and the drying medium of warm air drying is air, nitrogen or carbonic acid gas, preferred nitrogen and carbonic acid gas; Described microwave vacuum drying, dry front equipment vacuum degree should be lower than 100 holders, preferably lower than 10 holders.
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| PCT/CN2015/081204 WO2015192731A1 (en) | 2014-06-18 | 2015-06-10 | Silicon-based monobasic or multibasic oxide aerogel material and preparation method therefor |
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Cited By (50)
| Publication number | Priority date | Publication date | Assignee | Title |
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