CN104649280A - Preparation method of aerosil - Google Patents
Preparation method of aerosil Download PDFInfo
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- CN104649280A CN104649280A CN201310575844.4A CN201310575844A CN104649280A CN 104649280 A CN104649280 A CN 104649280A CN 201310575844 A CN201310575844 A CN 201310575844A CN 104649280 A CN104649280 A CN 104649280A
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- alcogel
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Abstract
A preparation method of aerosil belongs to the chemical field, and the invention specifically relates to the preparation method of the aerosil. The preparation method of the aerosil provided by the invention is low in cost, simple in reaction condition and high in yield. The preparation method of aerosil provided by the invention is characterized by comprising the following steps: mixing tetraethyl orthosilicate, water and ethanol by the ratio of 1:1, adjusting the mixture to acidic conditions by using hydrochloric acid, conducting refluxing at 40-80 DEG C for full hydrolysis, then adjusting the obtained product to alkaline conditions with a pH value of 8-10 by using ammonia, then transferring the uniform mixed liquid into a closed container, and forming alcogel at room temperature, wherein the time required by the sol to be still in the angle of inclination in a container is calculated as the gelation time; soaking the alcogel with ethanol in 60-80 DEG C, then soaking the alcogel with mother liquor of tetraethyl orthosilicate ethanol solution with certain composition, aging for 36-48 h, then soaking the alcogel in absolute ethyl alcohol at 40-45 DEG C for 48-64 h, and finally drying at 50-100 DEG C to obtain the aerogel.
Description
Technical field
The invention belongs to chemical field, specifically, the present invention relates to a kind of preparation method of aerosil.
Background technology
Aerosil makes it have the character of many uniquenesses by coalescent light porous its distinctive nano-sized particles of property nano structural material that forms of ultrafine particulate and nano aperture structure, thus at extremely-low density high temperature resistant heat insulation material, efficient high energy electrode, specific acoustic resistance lotus root condensation material gas adsorption and separatory membrane, the application prospect that the aspect such as effective catalyst and carrier thereof is wide, the preparation of current aerogel comprises so-gel and supercritical drying two processes usually, in colloidal sol one glue process, organosilicon alkoxide is formed with the gel of fine network pore space structure by hydrolysis and polycondensation, utilize supercritical drying process then can remove quantity of fluid in gel and obtained aerogel under the prerequisite keeping original structure but supercritical drying process needs high-tension apparatus and condition controls very harsh, thus the preparation cost of aerogel is expensive, limit the large-scale promotion application of Monolithic aerogel.
Summary of the invention
The present invention is exactly for above-mentioned technical problem, and provide a kind of with low cost, reaction conditions is simple, the preparation method of the aerosil that productive rate is high.
For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme: the preparation method of aerosil of the present invention, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 40-80 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8-10, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; After obtaining alcogel, alcogel ethanol is soaked at 60-80 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soak, ageing 36-48h, then with dehydrated alcohol 40-45 DEG C soak 48-64h, last dry at 50-100 DEG C, can aerogel be obtained.
Beneficial effect of the present invention: reaction conditions of the present invention is simple, and temperature of reaction is low, is all less than 100 DEG C.Environmental requirement is advised, and can carry out in factory.Its raw material obtains easily, and with low cost, productive rate is high, obtains good product quality.
The aerogel outward appearance obtained by context of methods is milky light porous block, and density is generally 500-800kgm3.As can be seen from stereoscan photograph, gained aerogel is the porous material with contiguous network structure.Observed result is carried out to the statistical study of size of particles, can obtain the diameter of the constituent particle of this aerogel sample about, particle is spherical substantially and size-grade distribution is more even.
Embodiment
The preparation method of aerosil of the present invention, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 40-80 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8-10, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; After obtaining alcogel, alcogel ethanol is soaked at 60-80 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soak, ageing 36-48h, then with dehydrated alcohol 40-45 DEG C soak 48-64h, last dry at 50-100 DEG C, can aerogel be obtained.
Embodiment 1: the preparation method of aerosil of the present invention, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 45 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 55 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 45h, then use dehydrated alcohol is at 45 DEG C of immersion 48h, and finally drying at 60 DEG C, can obtain aerogel.
Embodiment 2: the preparation method of aerosil of the present invention, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 80 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 10, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 80 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 48h, then use dehydrated alcohol is at 45 DEG C of immersion 64h, and finally drying at 100 DEG C, can obtain aerogel.
Embodiment 3: the preparation method of aerosil of the present invention, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 40 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 67 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 36-48h, then use dehydrated alcohol is at 44 DEG C of immersion 60h, and finally drying at 80 DEG C, can obtain aerogel.
Embodiment 4: the preparation method of aerosil of the present invention, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 70 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 9, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 72 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 48h, then use dehydrated alcohol is at 49 DEG C of immersion 60h, and finally drying at 99 DEG C, can obtain aerogel.
Claims (5)
1. the preparation method of aerosil, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 40-80 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8-10, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; After obtaining alcogel, alcogel ethanol is soaked at 60-80 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soak, ageing 36-48h, then with dehydrated alcohol 40-45 DEG C soak 48-64h, last dry at 50-100 DEG C, can aerogel be obtained.
2. the preparation method of aerosil according to claim 1, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 45 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 55 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 45h, then use dehydrated alcohol is at 45 DEG C of immersion 48h, and finally drying at 60 DEG C, can obtain aerogel.
3. the preparation method of aerosil according to claim 1, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 80 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 10, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 80 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 48h, then use dehydrated alcohol is at 45 DEG C of immersion 64h, and finally drying at 100 DEG C, can obtain aerogel.
4. the preparation method of aerosil according to claim 1, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 40 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 8, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 67 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 36-48h, then use dehydrated alcohol is at 44 DEG C of immersion 60h, and finally drying at 80 DEG C, can obtain aerogel.
5. the preparation method of aerosil according to claim 1, it is characterized in that: positive silicic acid second vinegar, water are mixed in 1:1 ratio with ethanol, under first adopting hydrochloric acid that this mixed solution is adjusted to acidic conditions, at 70 DEG C, backflow makes it fully be hydrolyzed, then being adjusted to pH value under alkaline condition with ammoniacal liquor is 9, transfer in encloses container by Homogeneous phase mixing liquid again, the time at room temperature forming alcogel required when do not flow in pitch angle in a reservoir with colloidal sol is gel time; Obtain after alcogel, alcogel ethanol soaked at 72 DEG C, then with the mother liquor of the positive silicic acid second vinegar ethanol of definite composition soaks, ageing 48h, then use dehydrated alcohol is at 49 DEG C of immersion 60h, and finally drying at 99 DEG C, can obtain aerogel.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310575844.4A CN104649280A (en) | 2013-11-18 | 2013-11-18 | Preparation method of aerosil |
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| CN201310575844.4A CN104649280A (en) | 2013-11-18 | 2013-11-18 | Preparation method of aerosil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664933A (en) * | 2015-12-31 | 2016-06-15 | 东华大学 | Method for preparing continuous SiO2/nano-metal aerogel fibers with catalysis performance through finally loading nano-metal |
| CN105671687A (en) * | 2015-12-31 | 2016-06-15 | 东华大学 | Preparation method of continuous SiO2 aerogel fibers |
| CN108483934A (en) * | 2018-03-29 | 2018-09-04 | 东南大学 | A kind of tungsten bronze/silica dioxide gel heat-insulation functional material and preparation method thereof |
-
2013
- 2013-11-18 CN CN201310575844.4A patent/CN104649280A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664933A (en) * | 2015-12-31 | 2016-06-15 | 东华大学 | Method for preparing continuous SiO2/nano-metal aerogel fibers with catalysis performance through finally loading nano-metal |
| CN105671687A (en) * | 2015-12-31 | 2016-06-15 | 东华大学 | Preparation method of continuous SiO2 aerogel fibers |
| CN105664933B (en) * | 2015-12-31 | 2018-09-25 | 东华大学 | A kind of continuous SiO of back loading nano metal preparation with catalytic performance2The method of/nano metal airsetting glue fiber |
| CN108483934A (en) * | 2018-03-29 | 2018-09-04 | 东南大学 | A kind of tungsten bronze/silica dioxide gel heat-insulation functional material and preparation method thereof |
| CN108483934B (en) * | 2018-03-29 | 2021-02-02 | 东南大学 | Tungsten bronze/silica gel heat insulation functional material and preparation method thereof |
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Application publication date: 20150527 |