CN100372765C - Hydrophobic SiO2 aerogel preparing process - Google Patents
Hydrophobic SiO2 aerogel preparing process Download PDFInfo
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- CN100372765C CN100372765C CNB2004100893525A CN200410089352A CN100372765C CN 100372765 C CN100372765 C CN 100372765C CN B2004100893525 A CNB2004100893525 A CN B2004100893525A CN 200410089352 A CN200410089352 A CN 200410089352A CN 100372765 C CN100372765 C CN 100372765C
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Abstract
The present invention relates to a method for preparing hydrophobic SiO2 aerogel, particularly to a process for preparing hydrophobic sio2 aerogel at normal pressure by a one-step method. Methyltris alkoxy silane, lower alcohol, water and silicasol are mixed in a closed container, and the ratio of the methyltris alkoxy silane to the lower alcohol to the water to the silicasol is 0.5 to 4: 2 to 16: 1 to 8: 1. The pH value is adjusted to be from 4 to 6, the mixture of the methyltris alkoxy silane, the lower alcohol, the water and the silicasol is stirred for 1 to 6 hours and is statically placed for 2 to 6 hours at room temperature, and then, the pH value is adjusted to be from 7 to 10; the mixture is sealed and is positioned in a drying oven of 30 to 60 DEG C, and SiO2 mixed alcogel in which =Si-O-Si= and =Si-O-Si-CH3 are mutually and crossly linked is made; after the SiO2 mixed alcogel is processed for 24 hours in the mode of aging, the SiO2 mixed alcogel is soaked in alcohol or acetone for three times, and the soaking of each time takes four hours; finally the SiO2 mixed alcogel is dried for 12 to 36 hours in the drying oven of 60 to 80 DEG C, and the hydrophobic SiO2 aerogel can be made. The present invention has the advantages of simple process, low cost and low equipment requirement and investment; the performance of the obtained hydrophobic SiO2 aerogel is good, the density is from 100 to 600kg m<-3>, the specific surface area is from 340.06 to 436.86m<2> g<-1>, and the contact angle to the water is from 127 degrees to 141 degrees.
Description
Technical field
The present invention relates to a kind of hydrophobic SiO
2The preparation method of aerogel specifically is that next step legal system of normal pressure is equipped with hydrophobic SiO
2The technology of aerogel.
Background technology
SiO
2Aerogel is by SiO
2Colloidal particle is coalescent mutually, constitutes the vesicular network structure, and is full of the solid-state material of a kind of high dispersive of air in the hole of vesicular network structure, and it is at calorifics, electricity, and optics, aspects such as acoustics have special performance, thereby have a wide range of applications.But, many application needs of aerogel are exposed in water or the malaria, because common aerogel material has the open pore that connects the surface, high porosity and the existence of surperficial great amount of hydroxy group, make its be very easy to absorb airborne water vapour and degenerate that this has just weakened aerogel in the coml actual application value.And hydrophobic nature SiO
2Aerogel then can overcome common SiO
2Aerogel absorbs moisture and the defective that degenerates in actual applications easily, shows great application potential in each fields such as the energy, information, environmental protection, medicine, agricultural chemicals, metallurgy, catalysis, buildings.For example, it can be used as auxiliary material and/or vehicle is used for preparation and pharmaceutically active substance; Solid support material as active substance is used in agricultural and beastly industry; Can make mixture with filamentary material,, and have the hydrophobic SiO of permanently hydrophobic surface group as thermal insulation material or directly as quieter material and resonance absorption agent with low heat conductivity
2Aerogel is used as packing material in can and storing in fluid transport.Therefore, hydrophobic SiO
2Aerogel has caused insider's very big concern.
At present, the hydrophobic nature aerogel can be divided into temporary and permanent two classes.The preparation research aspect of temporary hydrophobic aerogel, it is that raw material is produced the SiO2 hydrogel that US-5738801 (Hydrophobic silica aerogels) relates to water glass, prepare alcogel with the water in the ethanol place of water gel, obtain the temporary hydrophobic SiO that the surface connects methoxyl group behind the supercritical drying
2The method of aerogel.Human methanol steams such as Lee are to the low density bulk SiO with the supercritical drying preparation
2The water-wetted surface of aerogel carries out modification, can obtain the hydrophobic SiO of temporary (relatively in the short period of time)
2Aerogel (Lee, K.-H.; Kim, S.-Y.; Yoo, K.-P.Low-density, hydrophobic aerogels.Journal ofNon-Crystalline Solids, Vol:186: 18-22. (1995)).
But, above-mentionedly do not use chloride silylating agent can only obtain to have SiO through the hydrophobic surface group of oxygen bonding
2Aerogel, these groups are to disconnect the SiO for preparing quite easily under moisture atmosphere
2The aerogel surface only has temporary transient hydrophobic nature.
Prepare permanent hydrophobic SiO
2During aerogel, all need the gel that makes is carried out surperficial silylation reactive.Promptly adopt two steps, make SiO earlier
2Wet gel (hydrogel) needs the gel that makes is carried out surperficial silylation reactive then, and the gel after the silylanizing has just been finished after super-dry and prepared the hydrophobic SiO with permanently hydrophobic surface group
2Aerogel.For example, US-6,005,012 discloses with the trimethylchlorosilane steam as surface-modifying agent, to the block SiO that has made with supercritical drying
2Aerogel carries out surface treatment, has obtained hydrophobic SiO
2The method of aerogel.US-5,830,387th, serve as that the basis preparation has (SiO with organoalkoxysilane (methyl silicate or tetraethoxy)
2)
nThe polymkeric substance of skeleton structure, make it and have the hydrophobic group and to respond active hydrophobic reagent (hexamethyldisiloxane, trimethylchlorosilane, methyltrimethoxy silane) reaction of silanol groups (being the silicon hydroxyl), through obtaining the hydrophobic aerogel behind the supercritical drying.WO94/25149 has described a kind of method of Dried at Subcritical Condition hydrophobic aerogel, makes SiO before drying
2Gel with contain chloromethyl silane base agent (as trimethylchlorosilane) reaction, replace solvent with appropriate organic solvent, the dry SiO that obtains surface organic modification in the warm air more than 200 ℃
2Aerogel.The patent No. is that 98811584.0. (producing the method for silicon tetrachloride-based organically-modified aerogel) discloses with the silicon tetrachloride is basis preparation silica wet gel, gel after aging soaks with hexamethyldisiloxane and trimethylchlorosilane and carries out surface modification, with obtaining hydrophobic wet gel behind the organic solvent purifying, drying makes organically-modified aerosil in 200 ℃ of flow of warm nitrogen gas.The patent No. is that 97195616.2. (method for preparing organically-modified aerogel) is with acidic ion exchange resin treating water glass solution, add NaOH solution and regulate filtration back gained pH value of filtrate, make it form gel, wash through the aged gel with glycol dimethyl ether then, carry out the gel surface silylation reactive with trimethylchlorosilane, make gel surface have hydrophobic nature, make organically-modified aerogel after the drying.The patent No. is that 97181109.1. (method for preparing aerogel organically-modified, permanently hydrophobic) adopts the water glass hydrolysis method to prepare lyogel, gel with hot water and organic solvent repetitive scrubbing gained, with trimethylchlorosilane, hexamethyldisiloxane as alkylating agent, make it in gel surface generation silylation reactive, after super-dry, prepared organically-modified aerogel with permanently hydrophobic surface group.
It is quite complicated that above-mentioned two-step approach prepares technology, and quality also is difficult to guarantee.At first, the surperficial silylation reactive of silica dioxide gel can't guarantee to carry out fully; Secondly, carry out modification, unavoidably produce by products such as hydrogenchloride, make follow-up purifying process become complicated with chloride silylating agent; Some still uses raw materials such as comparatively expensive alkylsiloxane (as methyl silicate, tetraethoxy) of price and titanium tetrachloride in the preparation gel process in addition, also have among some preparation methods and need to adopt the supercritical drying drying process, this technology is to the equipment requirements height, the difficulty that this has all increased preparation bulk aerogel makes the aerogel product extremely expensive.
In a word, up to now, do not find hydrophobic SiO with low cost, that technology is simple and quality product is high both at home and abroad as yet
2The aerogel preparation method.
Summary of the invention
The objective of the invention is to disclose that a kind of technology is simple, with low cost, equipment requirements and the low hydrophobic SiO of input
2The preparation method of aerogel, the hydrophobic SiO for preparing in this way
2The excellent property of aerogel.
For achieving the above object, it is main raw material that the present invention selects cheap silicon sol, silicon sol is joined the lower alcohol (C of methyl trialkoxysilane
1-C
3Monohydroxy-alcohol) in the solution of Zu Chenging, make the wet gel that obtains after the reaction have ≡ Si-O-Si ≡ and
The spacial framework that is cross-linked with each other is because the methyl (CH that gained wet gel surface silicon atoms connects
3) have hydrophobic nature, so the contact angle θ between the two-phase can become along with the increase of methyl trialkoxysilane addition greatly in the wet gel, the additional pressure of liquid will significantly reduce in the wet gel network structure at this moment, thereby improves the frame strength of gel.Subsequently with the liquid in dehydrated alcohol or the acetone replacement gel, further reduce the additional pressure of liquid in the gel, make in the drying process of aerogel preparation, the convergent force that the gel network skeleton is subjected to is reduced to minimum, deficiency so that gel in drying process, cave in, thereby realize the synthetic hydrophobic gel of single stage method, and drying makes hydrophobic SiO under normal pressure
2Aerogel.
Concrete technology is as follows:
At first, with methyl trialkoxysilane: C
1-C
3Monohydroxy-alcohol: water: silicon sol is (0.5～4) with volume ratio: (2～16): (1～8): 1 mixed is in an encloses container, be adjusted between 4～6 with the pH value of Glacial acetic acid reaction system, simultaneously with magnetic stirrer 1～6 hour to mixing, at room temperature left standstill afterwards 2～6 hours, make the methyl trialkoxysilane hydrolysis reaction fully form colloidal sol, be adjusted between 7～10 with the pH value of strong aqua then colloidal sol, be statically placed in after the sealing in 30～60 ℃ the baking oven, promptly make after 4～42 hours ≡ Si-O-si ≡ with
The SiO that is cross-linked with each other
2The alcohol mixture gel.Then, the alcogel that makes carried out ageing after 24 hours, dehydrated alcohol or the acetone organic solvent less with surface tension soak three times, and soak cycle is each 4 hours, with the small amount of N a that is contained in the water in the removal reaction system and lower alcohol solvent and the raw materials of silica sol
+Ion.At last, with the alcogel after soaking in 60-80 ℃ baking oven dry 12-36 hour, the hydrophobic SiO that can make
2Aerogel, these hydrophobics SiO
2The density of aerogel is at 100～600kgm
-3, specific surface area is at 340.06-436.86m
2G
-1Between, to the contact angle of water between 127 °-141 °.
The pH of the silicon sol among the present invention is 7.0～10.5, and density is 1.05～1.32gcm
-3, SiO
2Content 20%～40%, Na
2The content of O=0.5～0.05%, SiO
2The particle diameter of micelle concentrates on alkaline silica sol or the neutral silicon sol between 5～40nm.
Methyl trialkoxysilane among the present invention is an industrial raw material, and content is more than 98%, and its general formula is CH
3-Si (OR)
3, wherein R is methyl (CH
3) or ethyl (C
2H
5).
The present invention has the following advantages:
1. technology of the present invention is simple, and condition is controlled easily, and is with low cost.Because the raw material that the present invention selects for use is a silicon sol, this silicon sol is the energy stable existence in 6 months to 1 year, saved use organosilicon alkoxide (as tetraethoxy, methyl silicate) feedstock production wet gel the hydrolytic process of essential experience, help the control of wet gel structure more, thereby make whole hydrophobic SiO of the present invention
2The producing to become of aerogel is more prone to.While is because the silicon sol source is very extensive, cheap, and SiO in the raw material
2Content can be up to 40%, so of the present invention be that raw material is produced hydrophobic SiO by atmosphere pressure desiccation with the silicon sol
2The technology of aerogel is compared for the technology of raw material with adopting organosilicon alkoxide (as tetraethoxy, methyl silicate) at present, and operational condition is simplified more, and preparation efficiency improves greatly, and product cost obviously reduces.
2. the initial period in reaction joins silylating agent (methyl trialkoxysilane) in the reactant of producing wet gel, make that the silylation reactive of gel surface is carried out in the gelation process of colloidal sol, guaranteed that silylation reactive completely takes place gel surface, improved working efficiency, reduced technical process, realized that single stage method synthesizes hydrophobic SiO
2The preparation method of aerogel.
3. by under the acid catalysis condition, (Union carbide A-162 is called for short MTES to make methyl trialkoxysilane; Methyltrimethoxy silane is called for short MTMS) sufficient hydrolysis reaction takes place quickly, under base catalysis, make ≡ Si-O-Si ≡ and
Polycondensation takes place rapidly make the hydrophobic wet gel, thus greatly shortening-4-producing the time of alcogel.
4. the hydrophobic SiO that method of the present invention makes
2Aerogel best in quality, analysis revealed after tested, hydrophobic SiO
2The density of aerogel is at 0.1～0.6gcm
-3, specific surface area is at 340.06-436.86m
2G
-1Between, under the room temperature, water at the contact angle on these aerogel surfaces in 127 ° of-141 ° of scopes.
Embodiment
Embodiment 1:
At first, selecting commercially available neutral silicon sol for use is the silicon source, and the pH of this silicon sol is about 7.6, and density is about 1.20gcm
-3, SiO
2Content is about 30%, Na
2The content 0.05% of O, SiO
2The particle diameter of micelle concentrates between 5～25nm, and size-grade distribution is quite even.Then, with this silicon sol strainer filtering, to remove a small amount of suspended contamination in the commercially available silicon sol.Choose commercially available density and be about 0.899gcm
-3(25 ℃), (molecular formula is CH to the water white Union carbide A-162 liquid of content 〉=98%
3Si (OC
2H
5)
3) be silylating agent.Under the room temperature, dripping silicon sol, dehydrated alcohol and deionized water to filling in the Union carbide A-162 sealable container of (being called for short MTES) under the stirring of electric blender, its typical prescription is MTES: dehydrated alcohol: water: the volume ratio of silicon sol is 1.85: 4.0: 2.84: 0.5, with acetic acid the pH value is adjusted to 4, stirs and become clarifying liquid after 2 hours.Room temperature leaves standstill and adds a certain amount of strong aqua after 4 hours, and the pH value is adjusted to 8.5, places 60 ℃ of baking ovens then, obtains alcogel after 4 hours.Ageing was carried out exchange of solvent 3 times with acetone after 24 hours then, and each about 4 hours at interval, 70 ℃ of following freeze-day with constant temperature 24 hours, remove and desolvate and moisture at last, can obtain density is 0.310gcm
-3, specific surface is 340.06m
2G
-1Hydrophobic SiO
2Liquid water under the aerogel, room temperature is 136.3 ° at the contact angle of this aerogel sample surfaces.
Embodiment 2:
Repeat embodiment 1, but do following change: the pH of the silicon sol of selecting for use is 9.96, and density is 1.050gcm
-3, SiO
2Content is about 20%, Na
2The content 0.35% of O, SiO
2The particle diameter of micelle concentrates between 12～40nm.Choose technical grade density and be about 0.899gcm
-3(25 ℃), (molecular formula is CH to the water white methyltrimethoxy silane liquid of content 〉=98%
3Si (OCH
3)
3) be silylating agent.Methyltrimethoxy silane (being called for short MTMS): dehydrated alcohol: water: silicon sol is 1.5: 2: 1 with volume ratio: 1 mixed, add a certain amount of vinegar acid for adjusting pH value 6, stir under the room temperature to become after 6 hours and show slightly milky transparent liquid, adding strong aqua then makes the pH value be adjusted in 7.0, be statically placed in 60 ℃ the baking oven, promptly make ≡ Si-O-Si ≡ and ≡ Si-O-Si-CH after 42 hours
3The hydrophobic wet gel that is cross-linked with each other.The gel ageing after 24 hours, is soaked 3 times each about 4 hours at interval with acetone solvent.Alcogel after the immersion in 60 ℃ baking oven dry 36 hours successively.Can make density is 0.287gcm
-3, specific surface is 436.86m
2G
-1Hydrophobic SiO
2Liquid water under the aerogel, room temperature is 127.5 ° at the contact angle of this aerogel sample surfaces.
Embodiment 3:
Repeat embodiment 1, but do following change: selecting commercially available alkaline silica sol for use is the silicon source, and the pH of this silicon sol is about 10.5, and density is about 1.320gcm
-3, SiO
2Content is about 40%, Na
2The content 0.5% of O, SiO
2The particle diameter of micelle concentrates between 12～40 nm.The silylating agent of choosing is that purity is not less than 98%, density is 0.950-0.954gcm
-3(molecular formula is CH to water white methyltrimethoxy silane
3Si (OCH
3)
3) liquid.Methyltrimethoxy silane (being called for short MTMS): ethanol: water: silicon sol is 4: 16: 8 with volume ratio: 1 mixed, add a certain amount of vinegar acid for adjusting pH value 5, stir under the room temperature and mixed in 1 hour, add alkali then and make the pH value, be statically placed in that constant temperature promptly obtains Si-O-Si ≡ and ≡ Si-O-Si-CH in 30 ℃ the thermostat container about 20 hours 10
3The hydrophobic wet gel that is cross-linked with each other.Ageing was soaked 3 times with anhydrous ethanol solvent after 24 hours, each about 4 hours at interval.The alcogel that obtains after the immersion is placed in 80 ℃ the thermostat container dry 12 hours, can make hydrophobic SiO
2Aerogel, the density of this sample are 0.127gcm
-3, specific surface is 382.39m
2G
-1, under the room temperature, liquid water is 140.8 ° at the contact angle of this aerogel sample surfaces.
Claims (3)
1. one kind prepares hydrophobic SiO
2The method of aerogel is characterized in that: at first, and with methyl trialkoxysilane: C
1-C
3Monohydroxy-alcohol: water: silicon sol is (0.5～4) with volume ratio: (2～16): (1～8): 1 mixed is in an encloses container, be adjusted between 4～6 with the pH value of Glacial acetic acid reaction system, simultaneously with magnetic stirrer 1～6 hour to mixing, at room temperature left standstill afterwards 2～6 hours, make the methyl trialkoxysilane hydrolysis reaction fully form colloidal sol, be adjusted between 7～10 with the pH value of strong aqua then colloidal sol, be statically placed in after the sealing in 30～60 ℃ the baking oven, promptly make after 4～42 hours ≡ Si-O-Si ≡ with
The SiO that is cross-linked with each other
2The alcohol mixture gel; Then, the above-mentioned alcogel that makes was carried out ageing after 24 hours, soak three times with dehydrated alcohol or acetone, soak cycle is each 4 hours, with the small amount of N a that is contained in the water in the removal reaction system and lower alcohol solvent and the raw materials of silica sol
+Ion; At last, with the alcogel after soaking in 60-80 ℃ baking oven dry 12-36 hour, can make hydrophobic SiO
2Aerogel.
2. a kind of preparation hydrophobic SiO according to claim 1
2The method of aerogel is characterized in that: silicon sol is that pH is 7.0～10.5, and density is 1.05～1.32gcm
-3, SiO
2Content 20%～40%, Na
2The content of O=0.5～0.05%, SiO
2The particle diameter of micelle concentrates on alkaline silica sol or the neutral silicon sol between 5～40nm.
3. a kind of preparation hydrophobic SiO according to claim 1
2The method of aerogel is characterized in that: described methyl trialkoxysilane is an industrial raw material, and content is more than 98%, and its general formula is CH
3-Si (OR)
3, wherein R is methyl or ethyl.
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|---|---|---|---|
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|---|---|---|---|
| CNB2004100893525A CN100372765C (en) | 2004-12-09 | 2004-12-09 | Hydrophobic SiO2 aerogel preparing process |
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| CN1636871A CN1636871A (en) | 2005-07-13 |
| CN100372765C true CN100372765C (en) | 2008-03-05 |
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