CN102964055A - Ultra-fast preparation method for highly transparent aerogel glass - Google Patents
Ultra-fast preparation method for highly transparent aerogel glass Download PDFInfo
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- CN102964055A CN102964055A CN201210396792XA CN201210396792A CN102964055A CN 102964055 A CN102964055 A CN 102964055A CN 201210396792X A CN201210396792X A CN 201210396792XA CN 201210396792 A CN201210396792 A CN 201210396792A CN 102964055 A CN102964055 A CN 102964055A
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Abstract
The invention aims to provide an ultra-fast preparation method for highly transparent aerogel glass. The method comprises using tetraethyl orthosilicate and other silicon source precursors as well as ethanol and other solvents to prepared silica sol; putting the silica sol into a supercritical drying kettle, or pouring the silica sol into a die and putting the die into the supercritical drying kettle; rapidly heating, maintaining pressure and rapidly decompressing to prepare the aerogel glass with good completion. A whole preparation process can be completed in 2 hours, while traditional preparation processes need dozens of hours, and therefore the method greatly shortens time of the preparation process, increases production efficiency and improves yield of the aerogel glass. The aerogel glass prepared by the method has a visible light transmittance of more than 76 %, a density of less than 0.09 g/cm<3>, a thermal conductivity of less than 0.018 W / m*K, and a specific surface area of 800 to 1100 m<2>/g. The aerogel glass is resistant to high temperature, acid and alkali, is a new type of energy-efficient glass, and can be widely used in the fields of building energy efficiency, automobile and high temperature.
Description
Technical field
The present invention relates to that a kind of low density, good heat-insulation effect, light transmission are strong, hydrophobic, the method for the supper-fast preparation of aerogel glass of acid-alkali-corrosive-resisting, be specifically related to sol-gel technique and the quick Supercritical Drying Technology good aerogel glass of incompatible quick preparation integrity that matches.
Background technology
Aerogel is a kind of " the changing the magical material in the world " that newly rises nearest decades.Aerogel, english name aerogel sloughs most of solvent when gel, makes in the gel content liquid than solids content much less, or the medium that is full of in the space reticulated structure of gel is gas, and appearance is solid state, is aerogel.Aerogel includes a large amount of air, and typical hole dimension is in l ~ l00nm scope, and porosity is a kind of porous material with nanostructure more than 80%, all shows its peculiar property at aspects such as mechanics, acoustics, calorifics, optics.They obviously are different from pore space structure at the porous material of micron and millimeter magnitude, the nanostructure that it is very thin is so that the thermal conductivity of material is extremely low, has great specific surface area, scattering to light, sound is all much smaller than traditional porous material, these unique character are not only so that this material causes people's interest in fundamental research, and are containing in a lot of fields widely application prospect.
Aerogel glass is a kind of special aerogel, is the lightest and best glass material of effect of heat insulation in the world.The special structure of aerogel is given its good heat insulation, optics, hydrophobic, corrosion resistance nature.From outward appearance and transparency, aerogel glass is similar with simple glass, but its other glass has higher heat-insulating property, and thermotolerance is high, and fire-retardant, radioresistance radiation and ultraviolet radiation are gone back color-adjustable.In addition, aerogel is sound absorption qualities best material in all known inorganic materials, so that it becomes desirable architectural lighting material and civilian glass material.This novel glass can be used in translucent building enclosure and needs the place of high quality thermal insulation, such as thermal glass, fire door member, sun condensor roofing, the energy saving building window is heat insulation and the aspect such as air conditioning system member.
2011, the building energy consumption of China accounted for 27.5% of its total energy consumption, and covil construction and public building unit consumption of energy level are four times of Europe, three times of the U.S., and not energy-conservation building accounts for 95%." energy-saving and emission-reduction " 12 " planning " has been decided to be building energy conservation one of ten priority projects of " 12 energy-saving and emission-reduction ".Building energy consumption mainly refers to the energy, especially warming and the summer air-conditioning refrigeration that buildings winter heating, summer air-conditioning refrigeration, normal lighting, indoor and outdoor ventilation, household electrical appliances, cooking consume.Affecting the most direct factor of building energy consumption is the thermal and insulating performance of building maintenance structure, and door and window is the weak part of heat insulating in the building enclosure, is one of principal element that affects building energy conservation.With regard to the typical building maintenance structure of present China, the energy consumption of door and window more accounts for 40%～50% of building maintenance structure total energy consumption.Lagging material is applied in door and window, is considered to building energy conservation the most effective the most present direct mode.Aerogel glass is because its good character necessarily has vast application prospect on door and window.
It is the traditional method of preparation aerogel glass that sol-gel method cooperates supercritical drying, and the method is to adopt first sol method to prepare colloidal sol, and colloidal sol is poured in the mould, behind the collosol and gel, it is aging to add ethanol, and then the demoulding puts into autoclave and carry out drying, obtains aerogel glass.The method need to be passed through collosol and gel and gel weathering process, and two processes generally need respectively 2h and 48h, and in drying process, because colloidal sol has become gel, the too fast meeting of temperature rise rate causes decrease in yield, so drying process needs 22h, whole flow process generally needs 72h.Patent 200710050974.0 has been introduced the preparation of ultra-low density silicon dioxide aerogel, and it utilizes acidic silicasol to prepare density at 3 ~ 30mg/cm
3Aerogel, but preparation cycle at 3 ~ 15d, preparation be aerogel powder.Patent 201120048483.4 has been introduced the standby transparent thermal insulation SiO of integration system
2Aerogel composite glass is filled in the aerogel in the glass, and preparation process is two-step catalysis, and total preparation cycle also is at 2d.Secondly, existing preparation technology carries out drying again behind gel, because there is surface tension in the solvent of gel skeleton inside, even if the strict control of drying conditions, the yield rate of monoblock aerogel glass is still very low.
It is long that traditional method prepares the aerogel glass block cycle, and power consumption is high, and it is expensive to cause aerogel to prepare.This patent provides a kind of quick method for preparing the aerogel monolithic glass, gel and the gel weathering process of colloidal sol is saved, and adopted supper-fast intensification, whole aerogel preparation process is finished at 2h, greatly shorten preparation time, improved production efficiency, reduced production cost.
Summary of the invention
The object of the present invention is to provide a kind of supper-fast method for preparing aerogel glass.Realize whole preparation process in 2h, the aerogel glass visible light transmissivity of preparation is greater than 76%, and density is less than 0.080g/cm
3, specific surface area 800 ~ 1100m
2/ g, thermal conductivity is less than 0.021W/(mK).This aerogel glass density is little, is easy to the processing transportation, has good heat-proof quality, is desirable architectural lighting, vehicle glass material.
2, to prepare fast aerogel glass step as follows in the present invention:
(1) preparation of colloidal sol: with tetraethoxy (TEOS), methyl silicate (TMOS), trimethylchlorosilane (TMCS), acidic silicasol, in the silicon such as alkaline silica sol, the water glass source one or several are precursor, with ethanol (EtOH), methyl alcohol (MeOH), in Virahol, the acetone etc. one or several are solvent, with precursor, solvent, the distilled water of getting suitable proportion, behind the stirring 10min, add the ammoniacal liquor of an amount of 0.03～0.3mol/L, obtain silicon dioxide gel, pour colloidal sol into mould.
(2) formation of the drying of colloidal sol and glass: container or mould that colloidal sol will be housed are put into autoclave, pouring an amount of solvent into (separates with mould) in autoclave again, nitrogen is filled to that pressure is 2～6MPa in the autoclave, be warming up to 250～280 ℃ with 5～15 ℃/min, control pressure is between 8～20MPa.This moment, autoclave was filled by supercutical fluid, kept this state 10min, made transparency aerogel glass.
(3) again with the speed constant temperature pressure release of 0.2～0.6MPa/min to 0MPa, 5～10min is swept in the nitrogen punching, allows autoclave be cooled to room temperature, takes out aerogel glass.
Description of drawings
Fig. 1 is take TEOS as example, and the schema of traditional Supercritical Drying Technology and supper-fast supercritical technology contrasts.
[embodiment]
The present invention will be further described by reference to the accompanying drawings below by examples of implementation, but protection domain is not subjected to the restriction of these examples of implementation:
Embodiment 1
Take tetraethoxy: ethanol: the mol ratio of distilled water is got tetraethoxy 44ml as 1:6:3, ethanol 72ml, distilled water 10.8ml adds in the container successively, stirs 10min, the weak ammonia 15ml that adds 0.03mol/L continues to stir 10min and takes out, and pours mould into.
Mould is put into autoclave, in autoclave, adds again 100ml ethanol, be evacuated to-0.03MPa after, rush nitrogen to 4MPa, with the heat-up rate electrically heated 30min of 8 ℃/min, at this moment, pressure is 12MPa, after keeping 10min, take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave in as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling, obtain the aerogel glass of good moldability, whole flow process is 90min, and glass is circular.
Embodiment 2
Take tetraethoxy: ethanol: the mol ratio of distilled water is got tetraethoxy 88ml as 1:8:3, ethanol 192ml, distilled water 21.6ml adds in the container electric stirring 10min successively, the weak ammonia 30ml that adds 0.03mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, adds again 100ml ethanol, be evacuated to-0.03MPa after, rush nitrogen to 3MPa, with the heat-up rate electrically heated 30min of 8 ℃/min, at this moment, pressure is 15MPa, after keeping 10min, as 0MPa, be that the nitrogen of 0.6L/min rushes 10min, opening high pressure still after the cooling soon with flow velocity again in take the pressure release speed fast constant temperature pressure release of 0.5MPa/min to autoclave, obtain the aerogel glass of good moldability, whole flow process is 90min.
Embodiment 3
Take tetraethoxy: ethanol: the mol ratio of distilled water is got tetraethoxy 44ml as 1:12:3, ethanol 144ml, distilled water 14.4ml adds in the container electric stirring 10min successively, the weak ammonia 15ml that adds 0.1mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 100ml ethanol, be evacuated to-0.03MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 25min with 10 ℃/min, at this moment, pressure is 13MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 75min.
Embodiment 4
Take tetraethoxy: ethanol: the mol ratio of distilled water is got tetraethoxy 44ml as 1:6:4, ethanol 72ml, distilled water 14.4ml adds in the container electric stirring 10min successively, the weak ammonia 15ml that adds 0.1mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 150ml ethanol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 5
Take tetraethoxy: ethanol: the mol ratio of distilled water is got each tetraethoxy 44ml, ethanol 72ml as 1:8:4, distilled water 14.4ml adds in the container electric stirring 10min successively, the weak ammonia 15ml that adds 0.03mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 120ml ethanol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.6MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 85min.
Embodiment 6
Take tetraethoxy: ethanol: the mol ratio of distilled water is got tetraethoxy 44ml as 1:12:4, ethanol 144ml, distilled water 14.4ml adds in the container electric stirring 10min successively, the weak ammonia 6.3ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 90ml ethanol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 7
Take methyl silicate: methyl alcohol: the mol ratio of distilled water is got methyl silicate 60ml as 1:4:3, methyl alcohol 93ml, distilled water 22ml adds in the container electric stirring 10min successively, the weak ammonia 6.3ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 90ml methyl alcohol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 8
Take methyl silicate: methyl alcohol: the mol ratio of distilled water is got methyl silicate 30ml as 1:12:3, methyl alcohol 93ml, distilled water 11ml adds in the container electric stirring 10min successively, the weak ammonia 6.3ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 120ml methyl alcohol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 9
Take trimethylchlorosilane: ethanol: the mol ratio of distilled water is got trimethylchlorosilane 42ml as 1:4:3, ethanol 78ml, distilled water 18ml adds in the container electric stirring 10min successively, the weak ammonia 6.3ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again 120ml ethanol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 10
Take tetraethoxy: Virahol: the mol ratio of distilled water is got tetraethoxy 44ml as 1:6:4, Virahol 92ml, distilled water 10.8ml adds in the container electric stirring 10min successively, the weak ammonia 6.3ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again the 140ml Virahol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 15MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 11
Take tetraethoxy: Virahol: the mol ratio of distilled water is got tetraethoxy 22ml as 1:12:4, Virahol 92ml, distilled water 5.4ml adds in the container electric stirring 10min successively, the weak ammonia 4ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again the 150ml Virahol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 14MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.45MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Embodiment 12
Take tetraethoxy: Virahol: the mol ratio of distilled water is got tetraethoxy 44ml as 1:8:3, Virahol 120ml, distilled water 8.1ml adds in the container electric stirring 10min successively, the weak ammonia 5ml that adds 0.3mol/L continues to stir 10min and takes out, and pours in the mould.
Mould is put into autoclave, in autoclave, add again the 140ml Virahol, be evacuated to-0.04MPa after, rush nitrogen to 4MPa, heat-up rate electrically heated 30min with 8 ℃/min, at this moment, pressure is 15MPa, behind the maintenance 10min, in take the pressure release speed fast constant temperature pressure release of 0.6MPa/min to autoclave as 0MPa, be that the nitrogen of 0.5L/min rushes 10min soon with flow velocity again, opening high pressure still after the cooling obtains the aerogel glass of good moldability.Whole flow process is 95min.
Claims (10)
1. the method for the high transparency aerogel glass of supper-fast preparation is characterized in that, comprises following steps:
(1) preparation of silicon dioxide gel: take the silicon source as precursor, add solvent, obtain silicon dioxide gel through hydrolytic process;
(2) cast of colloidal sol: silicon dioxide gel without gelation process, is put into the supercritical drying still, or pour in the mould and mould to be put into the supercritical drying still;
(3) overcritical rapid drying: add an amount of solvent in autoclave, pre-inflated with nitrogen to 2～5MPa is rapidly heated to the super critical point of solvent, keeps supercritical state 8～15min, makes high transparency aerogel glass.
2. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 characterized by further comprising following step:
(4) quick pressure releasing: with the speed pressure release of 0.3～0.6MPa/min, the pressure release of autoclave internal pressure is to 0MPa, and then nitrogen wash autoclave 5～15min makes the autoclave cool to room temperature, takes out glass.
3. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that whole preparation process is less than 2h.
4. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2, it is characterized in that, the silicon source is tetraethoxy (TEOS), methyl silicate (TMOS), trimethylchlorosilane (TMCS), acidic silicasol, one or several of alkaline silica sol, water glass.
5. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that, configuration colloidal sol solvent for use is ethanol (EtOH), methyl alcohol (MeOH), one or several of Virahol, acetone.
6. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that, does not need through acid catalysis, and a direct step base catalysis obtains colloidal sol.
7. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that glass directly carries out supercritical drying without weathering process.
8. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that in its supercritical drying heat-processed, heat-up rate reaches 8 ℃/min.
9. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that the supercritical constant-pressure time is 8～15min.
10. the method for the high transparency aerogel glass of a kind of supper-fast preparation described in according to claim 1 and 2 is characterized in that the aerogel glass specific surface area 1100m of preparation
2/ g.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105536655A (en) * | 2015-12-11 | 2016-05-04 | 中国科学院兰州化学物理研究所 | Rapid preparation method for aerogel material |
| CN106699216A (en) * | 2016-12-29 | 2017-05-24 | 北京华夏特材科技发展有限公司 | Preparation method of non-shedding elastic-aerogel-coated long fiber composite material |
| CN107032582A (en) * | 2017-06-13 | 2017-08-11 | 合肥钢骨玻璃制品有限公司 | A kind of production technology of silica dioxide gel glass |
| CN107824129A (en) * | 2017-12-04 | 2018-03-23 | 陕西盟创纳米新型材料股份有限公司 | A kind of drying system of alcohol supercritical methanol technology production aeroge |
| CN110627383A (en) * | 2019-10-30 | 2019-12-31 | 应急管理部天津消防研究所 | Preparation method of transparent fireproof gel and composite fireproof glass |
| CN110862220A (en) * | 2019-11-28 | 2020-03-06 | 福建工程学院 | Preparation method of two-dimensional material doped multicomponent gel glass |
| CN114477193A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Anisotropic silicon dioxide aerogel with birefringence effect and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105536655A (en) * | 2015-12-11 | 2016-05-04 | 中国科学院兰州化学物理研究所 | Rapid preparation method for aerogel material |
| CN106699216A (en) * | 2016-12-29 | 2017-05-24 | 北京华夏特材科技发展有限公司 | Preparation method of non-shedding elastic-aerogel-coated long fiber composite material |
| CN107032582A (en) * | 2017-06-13 | 2017-08-11 | 合肥钢骨玻璃制品有限公司 | A kind of production technology of silica dioxide gel glass |
| CN107824129A (en) * | 2017-12-04 | 2018-03-23 | 陕西盟创纳米新型材料股份有限公司 | A kind of drying system of alcohol supercritical methanol technology production aeroge |
| CN107824129B (en) * | 2017-12-04 | 2024-03-12 | 陕西盟创纳米新型材料股份有限公司 | Drying system for producing aerogel by alcohol supercritical method |
| CN110627383A (en) * | 2019-10-30 | 2019-12-31 | 应急管理部天津消防研究所 | Preparation method of transparent fireproof gel and composite fireproof glass |
| CN110862220A (en) * | 2019-11-28 | 2020-03-06 | 福建工程学院 | Preparation method of two-dimensional material doped multicomponent gel glass |
| CN114477193A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Anisotropic silicon dioxide aerogel with birefringence effect and preparation method thereof |
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