CN101264891B - A kind of preparation method of high strength, low density silica airgel - Google Patents
A kind of preparation method of high strength, low density silica airgel Download PDFInfo
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- CN101264891B CN101264891B CN2008101040195A CN200810104019A CN101264891B CN 101264891 B CN101264891 B CN 101264891B CN 2008101040195 A CN2008101040195 A CN 2008101040195A CN 200810104019 A CN200810104019 A CN 200810104019A CN 101264891 B CN101264891 B CN 101264891B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 13
- 239000011240 wet gel Substances 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 13
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000004964 aerogel Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 239000012686 silicon precursor Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000000352 supercritical drying Methods 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 2
- 235000011089 carbon dioxide Nutrition 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 25
- 238000009413 insulation Methods 0.000 abstract description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000178 monomer Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 10
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 239000011800 void material Substances 0.000 description 6
- 239000012467 final product Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
本发明提出了一种制备高强度、低密度二氧化硅气凝胶的新方法，属于无机多孔材料技术领域。制备的具体步骤如下：将正硅酸甲酯或者正硅酸乙酯在pH＝1.5～4.5条件下于50～80℃水解2～6h；之后滴加氨水，并注入到模具中，使之在空气中成为湿凝胶单体；将所得的湿凝胶放在高压罐中，在一定配比的老化液中于80～150℃下老化3～10天；最后进行干燥，即可得到具有强度高并且密度低的二氧化硅气凝胶定型材料。本发明的优点在于：操作简便，工艺简单，在提高了传统二氧化硅气凝胶材料强度的同时，保证了其密度低的优点，促进了二氧化硅气凝胶在定型绝热制品领域的应用。The invention proposes a new method for preparing high-strength and low-density silica airgel, which belongs to the technical field of inorganic porous materials. The specific steps of preparation are as follows: hydrolyze methyl orthosilicate or ethyl orthosilicate at 50-80°C for 2-6 hours at pH = 1.5-4.5; then add ammonia water dropwise and inject it into the mold to make it Become a wet gel monomer in the air; put the obtained wet gel in a high-pressure tank, and age it in a certain proportion of aging solution at 80-150°C for 3-10 days; finally dry it to get a strong High and low density silica airgel setting material. The invention has the advantages of simple operation and simple process, while improving the strength of the traditional silica airgel material, it also ensures the advantage of low density, and promotes the application of silica airgel in the field of shaped heat insulation products .
Description
Technical field
The invention belongs to the inorganic porous material technical field, proposed a kind of method for preparing high strength, low-density silicon dioxide aerogel.
Background technology
Along with The development in society and economy and human living standard's raising, increasing to the demand of the energy, traditional Mineral resources such as coal, oil, Sweet natural gas will be faced with exhaustion in the near future.For alleviating energy crisis, except exploitation, research and utilization novel energy such as sun power etc., save energy, reducing power loss also is an importance.Therefore, research and develop porous material and just seem very necessary with excellent heat preservation and insulation.
Aerosil is a kind of special nano-porous materials, has the big (800～1000m of specific surface area
2/ g), the low (0.002～0.8g/cm of density
3), many premium propertiess, particularly its void content very high (up to 99%) such as unreactiveness, thermal conductivity very low (only be air 1/3) is the minimum solid material of present known thermal conductivity.Thereby have great using value in fields such as heat-insulation and heat-preservation, sound insulation, support of the catalyst, particularly in the typing thermal insulation that requires to have definite shape, sound insulation goods Application Areas, as heat-intercepting glass etc.But because the high porosity of this material causes SiO
2The structural strength of aerogel is relatively low, thereby has limited its application aspect typing thermal insulation, sound insulation goods, therefore, improves SiO
2The intensity of aerogel material becomes the focus that Many researchers is paid close attention to.
A.Katti etc. (A.Katti, N.Shimpi, S.Roy, et al.Chem.Mater, 2006,18:285-296) by coating amine-modified SiO with poly-urea
2The skeleton of aerogel has increased particle neck contact area, when having kept the aerogel meso-hole structure, has improved the intensity of material.Studies show that of R.Takahashi etc. (R.Takahashi, S.Sato, T.Sodesawa, et al.Materials Research Bulletin, 2005,40:1148-1156), under the similar situation of macropore content, reduce SiO
2Mesoporous volume content in the aerogel, intensity also can increase.With the crosslinked SiO of poly-hexamethylene vulcabond
2Nano particle in the hydrogel can improve intensity, but the material still very crisp and become opaque (N.Leventis, C.Sotiriou-Leventis, G.Zhang, et al.Nano Letters, 2002,2 (9): 957-960) that obtain.Deng Zhongsheng etc. (Z.S.Deng, J.Wang, A.M Wu.J.Non-Cryst.Solids, 1998, TiO is added in studies show that 225:101-104)
2Powder and mineral binder bond, the intensity of material increases to some extent.K.E.Parmenter etc. add ceramic fiber under lower volume density, can reduce shrinking percentage and can improve material intensity (K.E.Parmenter, F.Milstein.J.Non-Cryst.Solids, 1981,223:179-189).In addition, aging for a long time in all kinds of SOLVENTS under the normal pressure, also can improve material frame strength (G.Reichenauer.J.Non-Crystl.Solids, 2004,350:189-195).
Yet, these methods have also been brought a series of problem when having improved the strength of materials, or have reduced the void content of material, and perhaps the intensity of material improves not obvious, perhaps need the long aging work period, perhaps need miscellaneous exchange of solvent process etc.Therefore seek and both can improve intensity, the preparation method that can not have much impact to the porosity characteristic of material is particularly important again.
Aging condition is to SiO
2The structure of aerogel and performance important influence.Structure and performance that the composition of temperature, pressure and aging liquid when adjustment is aging can be regulated material.
Summary of the invention
The object of the present invention is to provide a kind of at raising SiO
2In the time of aerogel intensity, keep the method for its high porosity, low density advantage, by adopting with SiO
2Wet gel is High Temperature High Pressure aged method in the mother liquor of certain proportioning, the SiO of preparation high strength, high porosity
2Aerogel.
This method is the SiO that will obtain
2The wet gel monomer before the drying in the aging liquid of certain proportioning High Temperature High Pressure aging, concrete processing step is as follows:
With silicon precursor at silicon precursor: dehydrated alcohol: deionized water: the mol ratio of hydrolyst is 1: 2.5～8.5: 3.0～6.0: 3.0～9.0 * 10
-4Mixing solutions in hydrolysis; (1～5wt.%) also stirs dropping ammonia, and this moment, the pH of solution was 7.5～9.0, injects mould and leaves standstill, and makes its gel under air at room temperature then.In dehydrated alcohol, soak the demoulding behind 6～48h, take out silica wet gel; Silica wet gel put into 5～40vol.% silicon precursor is housed, 59～94vol.% dehydrated alcohol, 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor (in 1～5wt.%) the pressure pan, then 80～150 ℃ aging 3～10 days down; Carry out drying afterwards, obtain the aerosil shaping material.
Hydrolysising condition is that pH is controlled at 1.5～4.5,50～80 ℃ of water-baths, insulation 1～6h.
Described silicon precursor is methyl silicate (TMOS) or tetraethoxy (TEOS).
Described hydrolyst is the hydrochloric acid of 0.1～3.0mol/l or the sulfuric acid of 0.1～8.0mol/l.
Drying process is room temperature constant pressure and dry or supercritical drying.The solvent of supercritical drying is any in carbonic acid gas, ethanol, acetone, methyl alcohol, n-propyl alcohol, benzene, butanols, amylalcohol, the octane.
The present invention is with SiO
2Wet gel is aging in the mother liquor of High Temperature High Pressure, and tetramethoxysilance in the mother liquor or tetraethoxy turn into grafting in SiO by hydrolysis-esterification
2The small curvature radius place of wet gel network skeleton as the contact neck between offspring, thereby strengthens skeleton.On the other hand, with respect to the particle of long radius bigger solubleness will be arranged according to the offspring of minor radius, under certain conditions, small-particle will dissolve and under the neck of macroparticle surface or offspring deposition, thereby improves material frame strength (dissolving-PRECIPITATION MECHANISM).The environment of High Temperature High Pressure will quicken the carrying out of these processes, thereby has shortened digestion period.Because two kinds of strengthening mechanisms work at the same time, thereby the raising of the strength of materials is very obvious.Void content height, intensity height, block materials that specific surface area is high are easy to get when aerogel is dry.The ultimate compression strength of gained aerogel block body material has improved 3～5 times at 0.45～0.6MPa than the intensity without the High Temperature High Pressure aged samples.This moment, void content was 88～95%, and density is 0.17～0.28g/cm
3, be 70～85% without the void content of High Temperature High Pressure aged samples, density is 0.30～0.65g/cm
3
The present invention is under the situation of not introducing extraneous hotchpotch, and is only that the wet gel monomer is aging under the High Temperature High Pressure in mother liquor, relies on the variation of himself can obviously improve the strength of materials.This method is easy and simple to handle, and technology is simple, and cost is low, and when especially producing in enormous quantities, benefit is particularly evident.It efficiently solves long-term puzzlement silica aerogel material when improving the strength of materials, the series of negative effect problem of being brought, as reduced the void content of material and performance decrease such as the material heat-insulation and heat-preservation that causes, sound insulation.The present invention has also shortened the aging work period simultaneously.Adopt the present invention will make SiO
2Aerogel becomes possibility in the application aspect heat-intercepting glass, typing insulating product, the typing sound insulation goods, can make building energy-saving and cost-reducing on the one hand, can improve the performance characteristics of high-temperature service device on the other hand.
Embodiment
Embodiment one:
Methyl silicate (TMOS): deionized water: dehydrated alcohol: the vitriolic mol ratio is 1: 2.6: 5.8: 3.05 * 10
-4After the sulfuric acid of TMOS, deionized water, dehydrated alcohol and 0.35mol/l mixed, place 80 ℃ of water-baths, insulation 1h hydrolysis.Dropping ammonia (1.0wt.%) and stirring then, the pH ≈ 8 of this moment.Be injected in the mould afterwards and leave standstill, under air at room temperature, become glue.In dehydrated alcohol, soak 24h (at this moment, room temperature is 20 ℃) the back demoulding, take out wet gel, put into the pressure pan that 10vol.%TMOS, 89vol.% dehydrated alcohol, 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor (1.0wt.%) are housed, wore out 10 days down at 80 ℃ then.Carry out supercritical CO afterwards
2Dry (temperature: 45 ℃, pressure: 12MPa) get final product.
The volume density of gained sample is 0.23g/cm
3The sample size of compressive strength test is φ 16 * 20mm, tests on the RGM electronic universal tester, and loading rate is 0.5mm/min.Compressive strength is 0.54MPa.
Embodiment two:
Methyl silicate (TMOS): deionized water: dehydrated alcohol: the mol ratio of hydrochloric acid is 1: 2.6: 5.8: 6.1 * 10
-4With the mixed in hydrochloric acid of TMOS, deionized water, dehydrated alcohol and 0.35mol/l evenly after, place 60 ℃ of water-baths, insulation 2h hydrolysis.Dropping ammonia (1.5wt.%) and stirring then, the pH ≈ 8 of this moment.Be injected in the mould afterwards and leave standstill, under air at room temperature, become glue.In dehydrated alcohol, soak 24h (at this moment, room temperature is 20 ℃) the back demoulding, take out wet gel, put into 20vol.%TMOS is housed, the 79vol.% dehydrated alcohol in the pressure pan of 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor (1.5wt.%), wore out 3 days down at 150 ℃ then.Dry (temperature: 20 ℃) gets final product at normal temperatures and pressures afterwards.
The volume density of gained sample is 0.26g/cm
3The sample size of compressive strength test is φ 16 * 20mm, tests on the RGM electronic universal tester, and loading rate is 0.5mm/min.Compressive strength is 0.48MPa.
Embodiment three:
Tetraethoxy (TEOS): deionized water: dehydrated alcohol: the vitriolic mol ratio is 1: 8.0: 4.5: 4.2 * 10
-4After the sulfuric acid of TEOS, deionized water, dehydrated alcohol and 0.35mol/l mixed, place 80 ℃ of water-baths, insulation 1.5h hydrolysis.Dropping ammonia (1.0wt.%) and stirring then, the pH ≈ 8 of this moment.Be injected in the mould afterwards and leave standstill, under air at room temperature, become glue.In dehydrated alcohol, soak the 89vol.% demoulding of 36h (at this moment, room temperature is 15 ℃) back, take out wet gel, put into 10vol.%TEOS is housed, the 89vol.% dehydrated alcohol in the pressure pan of 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor (1.0wt.%), wore out 8 days down at 90 ℃ then.Normal temperature and pressure drying (temperature: 15 ℃) gets final product afterwards.
The volume density of gained sample is 0.25g/cm
3The sample size of compressive strength test is φ 16 * 20mm, tests on the RGM electronic universal tester, and loading rate is 0.5mm/min.Compressive strength is 0.50MPa.
Embodiment four:
Tetraethoxy (TEOS): deionized water: dehydrated alcohol: the mol ratio of hydrochloric acid is 1: 8.0: 3.5: 8.4 * 10
-4With the mixed in hydrochloric acid of TEOS, deionized water, dehydrated alcohol and 0.35mol/l evenly after, place 60 ℃ of water-baths, insulation 2h hydrolysis.Dropping ammonia (1.5wt.%) and stirring then, the pH ≈ 8 of this moment.Be injected in the mould afterwards and leave standstill, under air at room temperature, become glue.In dehydrated alcohol, soak 36h (15 ℃ of room temperatures) the back demoulding, take out wet gel, put into 20vol.%TEOS is housed, the 79vol.% dehydrated alcohol, in the pressure pan of 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor (1.5wt.%), wore out 5 days down at 100 ℃ then.Carry out supercritical CO afterwards
2Dry (temperature: 45 ℃, pressure: 12MPa) get final product.
The volume density of gained sample is 0.18g/cm
3The sample size of compressive strength test is φ 16 * 20mm, tests on the RGM electronic universal tester, and loading rate is 0.5mm/min.Compressive strength is 0.60MPa.
Embodiment five:
Tetraethoxy (TEOS): deionized water: dehydrated alcohol: the mol ratio of hydrochloric acid is 1: 6.0: 3.5: 8.4 * 10
-4With the mixed in hydrochloric acid of TEOS, deionized water, dehydrated alcohol and 0.35mol/l evenly after, place 50 ℃ of water-baths, insulation 6h hydrolysis.Dropping ammonia (1.5wt.%) and stirring afterwards, the pH ≈ 8 of this moment.Be injected in the mould afterwards and leave standstill, under air at room temperature, become glue.In dehydrated alcohol, soak 36h (15 ℃ of room temperatures) the back demoulding, take out wet gel, put into 20vol.%TEOS is housed, the 79vol.% dehydrated alcohol, in the pressure pan of 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor (1.5wt.%), wore out 3 days down at 120 ℃ then.Carry out afterwards the Supercritical Ethanol drying (temperature: 260 ℃, pressure: 7.5MPa) get final product.
The volume density of gained sample is 0.17g/cm
3The sample size of compressive strength test is φ 16 * 20mm, tests on the RGM electronic universal tester, and loading rate is 0.5mm/min.Compressive strength is 0.56MPa.
Claims (6)
1. the preparation method of a high strength, low-density silicon dioxide aerogel is characterized in that, with the silica wet gel of preparation before the drying in mother liquor burin-in process under the high-temperature and high-pressure conditions, concrete preparation process is as follows:
A, with silicon precursor at silicon precursor: dehydrated alcohol: deionized water: the mol ratio of hydrolyst is 1: 2.5～8.5: 3.0～6.0: 3.0～9.0 * 10
-4Mixing solutions in hydrolysis;
B, dropping ammonia also stir, and form colloidal sol, inject mould, leave standstill, make its gel under air at room temperature, in alcohol, soak the demoulding behind 6～48h, take out silica wet gel, the concentration of ammoniacal liquor is 1～5wt.%, and the pH of solution is 7.5～9.0 after the dropping ammonia.
C, silica wet gel put into 5～40vol.% silicon precursor is housed, 59～94vol.% dehydrated alcohol, in the pressure pan of 0.5vol.% deionized water and 0.5vol.% ammoniacal liquor, then 80～150 ℃ aging 3～10 days down;
D, the sample drying after will wearing out.
2. preparation method as claimed in claim 1 is characterized in that, described silicon precursor is methyl silicate or tetraethoxy.
3. preparation method as claimed in claim 1 is characterized in that, described hydrolyst is the sulfuric acid of 0.1～3.0mol/L hydrochloric acid or 0.1～8.0mol/L.
4. preparation method as claimed in claim 1 is characterized in that the pH of hydrolysis is controlled at 1.5～4.5 among the step a, and temperature is 50～80 ℃, and soaking time is 1～6h.
5. preparation method as claimed in claim 1 is characterized in that, the drying in the steps d is room temperature constant pressure and dry or supercritical drying.
6. preparation method as claimed in claim 6 is characterized in that, the solvent of supercritical drying is any in carbonic acid gas, ethanol, acetone, methyl alcohol, n-propyl alcohol, benzene, butanols, amylalcohol, the octane.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE112017001567T5 (en) | 2016-09-14 | 2018-12-20 | Nano Technology Co., Ltd. | A rapid production process for an airgel with a microemulsion precursor |
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| CN102515181B (en) * | 2011-11-25 | 2015-04-22 | 航天特种材料及工艺技术研究所 | Method for improving strength of aerogel composite material |
| CN102583407B (en) * | 2012-03-22 | 2013-09-04 | 陕西盟创纳米新型材料股份有限公司 | Preparation method of silica aerogel |
| CN102646756B (en) * | 2012-04-26 | 2015-02-18 | 深圳市科聚新材料有限公司 | Preparation method for silicon dioxide block layer used for I-III-IV compound solar cell |
| CN102765725B (en) * | 2012-08-10 | 2014-03-05 | 蓝烟（北京）科技有限公司 | Method for preparing hydrophobic silica aerogel with low cost |
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| CN104108720B (en) * | 2014-07-08 | 2016-11-02 | 同济大学 | A kind of preparation method of silicon dioxide airgel particles with high lighting rate |
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-
2008
- 2008-04-14 CN CN2008101040195A patent/CN101264891B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE112017001567T5 (en) | 2016-09-14 | 2018-12-20 | Nano Technology Co., Ltd. | A rapid production process for an airgel with a microemulsion precursor |
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