CN101671029B - Method for preparing SiO2 aerogel in normal pressure drying condition - Google Patents
Method for preparing SiO2 aerogel in normal pressure drying condition Download PDFInfo
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- CN101671029B CN101671029B CN2009100730094A CN200910073009A CN101671029B CN 101671029 B CN101671029 B CN 101671029B CN 2009100730094 A CN2009100730094 A CN 2009100730094A CN 200910073009 A CN200910073009 A CN 200910073009A CN 101671029 B CN101671029 B CN 101671029B
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Abstract
The invention provides a method for preparing SiO2 aerogel in normal pressure drying condition, and relates to a preparation method of SiO2 aerogel. The preparation method overcomes the defects of complex devices, high production cost and high hazard existing in the method for preparing SiO2 aerogel in the supercritical drying condition and the defect that a complete SiO2 aerogel block is not easily obtained by the existing normal pressure drying technology. The preparation method of SiO2 aerogel comprises the following steps: obtaining SiO2 aerogel after sol-gel, ageing, solvent displacement, surface decoration, washing and drying processing. The method is characterized by low cost, low requirements on devices, good safety and the like. The SiO2 aerogel prepared by the method has uniformblock quality, good completeness, 90%-95% of gas hole ratio, low thermal conductivity, and is hydrophobing.
Description
Technical field
The present invention relates to a kind of SiO
2The preparation method of aerogel.
Background technology
SiO
2Aerogel prepares by supercritical drying as far back as early 1930s, is used for the stored material of liquid fuel in the sixties, is used for large-scale deep space probe at the beginning of the eighties, has after this received widely and has paid attention to.It has a series of special performances such as low density, high-specific surface area, high porosity, low thermal conductivity, infrasonic wave's velocity of propagation and low-k, all demonstrate unique value at aspects such as acoustics, mechanics, calorifics, optics, electricity and catalysis, such as substrate material, support of the catalyst, gas filter, the specific acoustic resistance coupling material of the large-scale integrated circuit of the dielectric material that is used for the Qie Lunkefu detector, high-speed computation, the still best solid material of present heat-insulating property simultaneously.
SiO
2The ordinary method of aerogel is to adopt the preparation of supercritical drying drying method.Aerogel performance by the supercritical process preparation is better, but the device systems complex and expensive, and need under High Temperature High Pressure, to work, dangerous high.And existing constant pressure and dry method is because the contraction of gel in drying process, and is cracked easily or crackle occurs, also is difficult to obtain complete SiO at present
2Aerogel block body.
Summary of the invention
The invention provides a kind of constant pressure and dry and prepare SiO
2The method of aerogel; Prepare SiO to overcome supercritical drying
2The aerogel method exists equipment complexity, production cost height, dangerous high shortcoming, and existing constant pressure and dry technology is difficult to obtain complete SiO
2The shortcoming of aerogel block body.
Constant pressure and dry of the present invention prepares SiO
2The method of aerogel is undertaken by following step:
One, will carry out hydrolysis reaction 48～60h after tetraethoxy (TEOS), dehydrated alcohol, oxalic acid and the water mixing, wherein the mol ratio of tetraethoxy and water is 1: 1, the mol ratio of tetraethoxy and dehydrated alcohol is 1: 7, and the mol ratio of tetraethoxy and oxalic acid is 1: 9 * 10
-4
Two, add entry, N again, dinethylformamide and ammoniacal liquor leave standstill 24～48h and obtain gel;
Three, after the gel that step 2 is prepared is placed 2～6h in 20～60 ℃ of loft drier, placing volumetric concentration then is the 80% alcoholic acid aqueous solution, burin-in process 12～24h under 40～60 ℃ of conditions, placing volume ratio again is 1: 5 tetraethoxy and alcohol mixeding liquid, burin-in process 12～24h under 40～60 ℃ of conditions;
Four, will the gel after burin-in process put into Virahol and carry out solvent exchange 4～8h, put into volume ratio then and be 1～4: 5 Virahol and normal hexane mixed solution and carry out solvent exchange 1～5 time, each 4～8h, put into normal hexane again and carry out solvent exchange 4～8h, be that 1: 1～50 trimethylchlorosilanes and normal hexane mixed solution carry out finishing to transparent fully with volume ratio then, be that 1: 1～50 Virahols and normal hexane mixed solution clean 4～8h with volume ratio again, clean 4～8h with normal hexane again;
Five, gel that will be after step 4 is handled is dry 6～10h under 40～80 ℃ of conditions, obtains aerogel; Wherein the mol ratio of described water of step 2 and the described tetraethoxy of step 1 is 3: 1, the described N of step 2, the mol ratio of dinethylformamide and the described tetraethoxy of step 1 is 0.8: 1, and the mol ratio of described ammoniacal liquor of step 2 and the described tetraethoxy of step 1 is 4 * 10
-3: 1.
The inventive method is carried out under normal pressure, and temperature of reaction is no more than 100 ℃, the reaction conditions gentleness, so the inventive method is not high to the requirement condition of equipment, and reduced production cost, improved security.
The SiO of the inventive method preparation
2The aerogel block body quality is even, integrity good, no cracked or crackle, and transparency is good, and void content is 90%～95%, hydrophobic, thermal conductivity is low.Above-mentioned aerogel has broad application prospects in heat preservation and insulation field such as the adiabatic windows of the saturating ripple of spacecraft.
Description of drawings
Fig. 1 is embodiment 11 prepared SiO
2The shape appearance figure of aerogel block body; Fig. 2 shows embodiment 11 prepared SiO
2The pattern of aerogel block body transparent characteristic; Fig. 3 is that water droplet drips in prepared SiO
2Non-wetted figure on the aerogel block body material surface; Fig. 4 is the prepared SiO of embodiment 11
2One piece of coin of aerogel block body heavy burden swims in figure waterborne; Fig. 5 is the prepared SiO of a hand-held embodiment 11
2The airsetting blob of viscose carries out the figure that calcination represents that thermal conductivity is low on alcohol blast burner.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.。
Embodiment one: the present embodiment constant pressure and dry prepares SiO
2The method of aerogel is undertaken by following step: carry out hydrolysis reaction 48h after one, tetraethoxy, dehydrated alcohol, oxalic acid and water being mixed, wherein the mol ratio of tetraethoxy and water is 1: 1, the mol ratio of tetraethoxy and dehydrated alcohol is 1: 7, and the mol ratio of tetraethoxy and oxalic acid is 1: 9 * 10
-4Two, add entry, N again, dinethylformamide and ammoniacal liquor leave standstill 36h and obtain gel; Three, after the gel that step 2 is prepared is placed 2～6h in 20～60 ℃ of loft drier, placing volumetric concentration then is the 80% alcoholic acid aqueous solution, burin-in process 12～24h under 40～60 ℃ of conditions, placing volume ratio again is 1: 5 tetraethoxy and alcohol mixeding liquid, burin-in process 12～24h under 40～60 ℃ of conditions; Four, will the gel after burin-in process put into Virahol and carry out solvent exchange 6h, put into volume ratio then and be 1～4: 5 Virahol and normal hexane mixed solution and carry out solvent exchange 1～5 time, each 5h (metathetical time), put into normal hexane again and carry out solvent exchange 5h, be that 1: 1～50 trimethylchlorosilanes and normal hexane mixed solution carry out finishing to transparent fully with volume ratio then, be that 1: 1～50 Virahols and normal hexane mixed solution clean 5h with volume ratio again, clean 5h with normal hexane again; Five, gel dry 8h under 40～80 ℃ of conditions that will be after step 4 is handled obtains aerogel; Wherein the mol ratio of described water of step 2 and the described tetraethoxy of step 1 is 3: 1, the described N of step 2, the mol ratio of dinethylformamide and the described tetraethoxy of step 1 is 0.8: 1, and the mol ratio of described ammoniacal liquor of step 2 and the described tetraethoxy of step 1 is 4 * 10
-3: 1.
The aerogel of present embodiment preparation has good one-tenth piece characteristic, and color be saturating a light blueness in vain, and the quality uniformity, and void content is 90%～95%.
Embodiment two: what present embodiment and embodiment one were different is: the drying temperature described in the step 3 is 30～50 ℃.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the drying temperature described in the step 3 is 40 ℃.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one to three were different is: in the step 3 in the alcoholic acid aqueous solution aging temperature be 45～55 ℃.Other step and parameter are identical with embodiment one to three.
Embodiment five: what present embodiment and embodiment one to three were different is: in the step 3 in the alcoholic acid aqueous solution aging temperature be 50 ℃.Other step and parameter are identical with embodiment one to three.
Embodiment six: what present embodiment and embodiment one to five were different is: in the step 3 in tetraethoxy and alcohol mixeding liquid aging temperature be 45～55 ℃.Other step and parameter are identical with embodiment one to five.
Embodiment seven: what present embodiment and embodiment one to five were different is: in the step 3 in tetraethoxy and alcohol mixeding liquid aging temperature be 50 ℃.Other step and parameter are identical with embodiment one to five.
Embodiment eight: what present embodiment and embodiment one to seven were different is: the drying temperature described in the step 5 is 50～70 ℃.Other step and parameter are identical with embodiment one to seven.
Embodiment nine: what present embodiment and embodiment one to seven were different is: the drying temperature described in the step 5 is 55～65 ℃.Other step and parameter are identical with embodiment one to seven.
Embodiment ten: what present embodiment and embodiment one to seven were different is: the drying temperature described in the step 5 is 55～65 ℃.Other step and parameter are identical with embodiment one to seven.
Embodiment 11: the present embodiment constant pressure and dry prepares SiO
2The method of aerogel is undertaken by following step: carry out hydrolysis reaction 48h after one, tetraethoxy, dehydrated alcohol, oxalic acid and water being mixed, wherein the mol ratio of tetraethoxy and water is 1: 1, the mol ratio of tetraethoxy and dehydrated alcohol is 1: 7, and the mol ratio of tetraethoxy and oxalic acid is 1: 9 * 10
-4Two, add entry, N again, dinethylformamide and ammoniacal liquor leave standstill 24h and obtain gel; Three, after the gel that step 2 is prepared is placed 6h in 40 ℃ of loft drier, placing volumetric concentration then is the 80% alcoholic acid aqueous solution, burin-in process 24h under 60 ℃ of conditions, placing volume ratio again is 1: 5 tetraethoxy and alcohol mixeding liquid, burin-in process 24h under 60 ℃ of conditions; Four, will the gel after burin-in process put into Virahol and carry out solvent exchange 6h, Virahol and the normal hexane mixed solution putting into volume ratio then and be 3.75: 5 carry out solvent exchange 5h, Virahol and the normal hexane mixed solution putting into volume ratio again and be 2.5: 5 carry out solvent exchange 5h, Virahol and the normal hexane mixed solution putting into volume ratio again and be 1.25: 5 carry out solvent exchange 5h, put into normal hexane again and carry out solvent exchange 5h, be that 1: 10 trimethylchlorosilane and normal hexane mixed solution carry out finishing to transparent fully with volume ratio then, be that 1: 10 Virahol and normal hexane mixed solution clean 5h with volume ratio again, clean 5h with normal hexane again; Five, gel dry 8h under 65 ℃ of conditions that will be after step 4 is handled obtains SiO
2Aerogel; Wherein the mol ratio of described water of step 2 and the described tetraethoxy of step 1 is 3: 1, the described N of step 2, the mol ratio of dinethylformamide and the described tetraethoxy of step 1 is 0.8: 1, and the mol ratio of described ammoniacal liquor of step 2 and the described tetraethoxy of step 1 is 4 * 10
-3: 1.
The aerogel of present embodiment preparation has good one-tenth piece characteristic (shown in Figure 1), and color be saturating a light blueness in vain, and the quality uniformity, transparency good (as shown in Figure 2), and void content is 94.5%.
At present existing constant pressure and dry technology is difficult to obtain the aerogel of diameter greater than 50mm; And preparing the diameter of aerogel, present embodiment equals 55mm.
On the aerogel of present embodiment preparation, water is the ellipsoid shape on the aerogel surface, aerogel not wetted (as shown in Figure 3) with water droplet.The aerogel of present embodiment preparation is put into water, put one piece of monobasic coin on aerogel, aerogel swims in (as shown in Figure 4) in the water.The above-mentioned aerogel that experimental results show that present embodiment preparation is nonwetting, do not absorb water.
Have hand-held aerogel to carry out calcination 45 seconds with alcohol blast burner, the result as shown in Figure 5, the thermal insulation and the resistance toheat of the aerogel of present embodiment preparation are good as seen from Figure 5.
Claims (9)
1. constant pressure and dry prepares SiO
2The method of aerogel is characterized in that constant pressure and dry prepares SiO
2The method of aerogel is undertaken by following step: carry out hydrolysis reaction 48～60h after one, tetraethoxy, dehydrated alcohol, oxalic acid and water being mixed, wherein the mol ratio of tetraethoxy and water is 1: 1, the mol ratio of tetraethoxy and dehydrated alcohol is 1: 7, and the mol ratio of tetraethoxy and oxalic acid is 1: 9 * 10
-4Two, add entry, N again, dinethylformamide and ammoniacal liquor leave standstill 24～48h and obtain gel; Three, after the gel that step 2 is prepared is placed 2～6h in 20～60 ℃ of loft drier, placing volumetric concentration then is the 80% alcoholic acid aqueous solution, burin-in process 12～24h under 40～60 ℃ of conditions, placing volume ratio again is 1: 5 tetraethoxy and alcohol mixeding liquid, burin-in process 12～24h under 40～60 ℃ of conditions; Four, will the gel after burin-in process put into Virahol and carry out solvent exchange 4～8h, put into volume ratio then and be 1～4: 5 Virahol and normal hexane mixed solution and carry out solvent exchange 1～5 time, each 4～8h, put into normal hexane again and carry out solvent exchange 4～8h, be that 1: 1～50 trimethylchlorosilanes and normal hexane mixed solution carry out finishing to transparent fully with volume ratio then, be that 1: 1～50 Virahols and normal hexane mixed solution clean 4～8h with volume ratio again, clean 4～8h with normal hexane again; Five, gel that will be after step 4 is handled is dry 6～10h under 40～80 ℃ of conditions, obtains aerogel; Wherein the mol ratio of described water of step 2 and the described tetraethoxy of step 1 is 3: 1, the described N of step 2, the mol ratio of dinethylformamide and the described tetraethoxy of step 1 is 0.8: 1, and the mol ratio of described ammoniacal liquor of step 2 and the described tetraethoxy of step 1 is 4 * 10
-3: 1.
2. constant pressure and dry according to claim 1 prepares SiO
2The method of aerogel is characterized in that the drying temperature described in the step 3 is 30～50 ℃.
3. constant pressure and dry according to claim 1 prepares SiO
2The method of aerogel is characterized in that the drying temperature described in the step 3 is 40 ℃.
4. prepare SiO according to claim 1,2 or 3 described constant pressure and dries
2The method of aerogel is characterized in that in the step 3 that aging temperature is 45～55 ℃ in the alcoholic acid aqueous solution.
5. prepare SiO according to claim 1,2 or 3 described constant pressure and dries
2The method of aerogel is characterized in that in the step 3 that aging temperature is 50 ℃ in the alcoholic acid aqueous solution.
6. constant pressure and dry according to claim 4 prepares SiO
2The method of aerogel is characterized in that in the step 3 that aging temperature is 45～55 ℃ in tetraethoxy and alcohol mixeding liquid.
7. constant pressure and dry according to claim 4 prepares SiO
2The method of aerogel is characterized in that in the step 3 that aging temperature is 50 ℃ in tetraethoxy and alcohol mixeding liquid.
8. prepare SiO according to claim 1,2,3,6 or 7 described constant pressure and dries
2The method of aerogel is characterized in that the drying temperature described in the step 5 is 50～70 ℃.
9. prepare SiO according to claim 1,2,3,6 or 7 described constant pressure and dries
2The method of aerogel is characterized in that the drying temperature described in the step 5 is 55～65 ℃.
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Cited By (1)
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| CN102951650A (en) * | 2012-08-31 | 2013-03-06 | 卢斌 | Ambient pressure drying method for rapidly preparing SiO2 aerogel |
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| CN102951650B (en) * | 2012-08-31 | 2015-05-20 | 卢斌 | Ambient pressure drying method for rapidly preparing SiO2 aerogel |
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