CN108854873A - A kind of preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel - Google Patents
A kind of preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel Download PDFInfo
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- CN108854873A CN108854873A CN201710331365.6A CN201710331365A CN108854873A CN 108854873 A CN108854873 A CN 108854873A CN 201710331365 A CN201710331365 A CN 201710331365A CN 108854873 A CN108854873 A CN 108854873A
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Abstract
The present invention relates to a kind of preparation methods of high temperature resistant silicon aluminum binary aeroge for a kind of preparation method abstract of high temperature oxidation resisting silicon/aluminium oxide binary aerogel of title.Using cheap inorganic aluminate and ethyl orthosilicate as presoma, deionized water and ethyl alcohol are solvent, and polyethylene glycol 2000 is dispersing agent, and the excellent blocky silicon-aluminium binary aeroge of high temperature resistance is prepared by supercritical drying process.Resulting aeroge sample rate is low, and specific surface area is high, and high temperature resistance is good, and certain exterior appearance is still kept at 1000 DEG C.The method has the advantages that preparation process is simple, manufacturing cycle is shorter, and the high temperature resistance of prepared aeroge extends the scope of application of aeroge, allows to be widely used in heat-insulated field.
Description
Technical field
The invention belongs to inorganic nano porous material preparation technical fields, and in particular to a kind of high temperature resistant silicon aluminum binary airsetting
The preparation method of glue.
Background technique
Aeroge is nano-porous materials made of a kind of nano particle is mutually assembled, the high hole that aerogel material has
Rate can reduce solid thermal conduction, and nano-porous structure can inhibit gas heat transfer, and the infrared light screening agent of introducing can reduce radiation and pass
Heat, this makes aeroge have excellent heat-proof quality, is the solid material that generally acknowledged thermal coefficient is minimum at present.It is this that there is sea
The material specific surface area of continuous shape open-celled structure is very big, and the structure of material can be controlled on the micro-scale of nanometer scale, from
And make it have many unique performances.The unique architectural characteristic of aeroge makes aeroge in calorifics, electricity, acoustics, optics
Etc. have unusual performance.
The study found that SiO2The room temperature thermal conductivity of aeroge is down to 0.012Wm-1k-1, but the temperature tolerance of the material compared with
Difference, 800 DEG C or more pore structures just occur seriously to collapse, and heat-proof quality drastically reduces.Al2O3The temperature tolerance of aeroge is higher, reachable
1000 DEG C, but the material is easy to happen crystal transfer under high temperature environment, and high-temperature heat conductivity is higher, thus by pair
Al2O3Aeroge carries out silicon doping, the SiO being prepared into2-Al2O3Composite aerogel is with higher heat resistance and lower
High-temperature heat conductivity.1993, Yasuyuki Mizushima etc. was prepared for sial composite aerogel, compared table after 1200 DEG C of processing
Area is reduced to 114.3m2/ g, but shrink situation and do not refer to.Nineteen ninety-five, R, Saliger et al. in silica aerogel by mixing
Miscellaneous alumina powder only obtains 1000 DEG C of heatproof of sial composite aerogel.Tatsuro Horiuchi in 2001 etc. is prepared for
Sial composite aerogel, although reference area is up to 150m after 1200 DEG C of processing2/ g, but shrink situation and do not refer to.Later, domestic
Many researchers also study sial composite aerogel, but prepare high temperature resistant, and the aeroge of forming still compares
It is more difficult.
Summary of the invention
The purpose of the present invention is to provide a kind of sides of the low cost preparation high temperature resistant sial composite aerogel of simple process
Method.
To achieve the above object of the invention, the technical solution adopted by the present invention is that：A kind of high temperature oxidation resisting silicon/oxidation aluminum binary
The preparation method of aeroge, is made in the steps below.
Step 1：PEG2000 is added to the in the mixed solvent of deionized water and ethyl alcohol, after stirring a period of time, makes it
It is dissolved completely in solvent.
Step 2：The chlorination aluminium salt for weighing certain mass is added to PEG2000 and dissolves in complete mixed solution, stirring
It is completely dissolved to it.
Step 3：The ethyl orthosilicate for measuring certain volume, is added in mixed solution, stirs, drips when being added dropwise
12h ~ for 24 hours is persistently stirred afterwards, is fully hydrolyzed it.
Step 4：It after hydrolyzing completely, measures a certain amount of propylene oxide and is added in mixed solution, stirred when being added dropwise
It mixes, solution is transferred in gelling vessel to its gel.
Step 5：By wet gel aging at a certain temperature, surface covers one layer of organic solvent protection.
Step 6：Wet gel is placed in alcohol solvent after aging and is replaced.
Step 7：The wet gel replaced is dried with supercritical drying process, finally obtains certain shapes
Silicon-aluminium binary aeroge.
The ratio between in the mixed solvent deionized water described in step 1 and ethyl alcohol are preferably 10ml：10ml, PEG2000 and solvent
Mass ratio is 1：80.
The middle Aluminium chloride hexahydrate salt quality and the mass ratio of solvent of being added is 1 described in step 2：3~1：10.
The ratio between mole of mole and chlorination aluminium salt that ethyl orthosilicate is added described in step 3 is 1：2~1：8.
The molar ratio of amount and chlorination aluminium salt that propylene oxide is added described in step 4 is 6：1~8：1, mixing time be 1 ~
3min takes out rapidly rotor after stirring, prevent from having little time to take out because of rapid gel.
Organic solvent described in step 5 is one kind of ethyl alcohol, methanol, and aging temperature is 20 ~ 30 DEG C, and the time is 0 ~ 2d.
The time swap of ethyl alcohol described in step 6 is 4 ~ 10d, and every 12h replaces a replacement fluid.
Dried medium selected by supercritical drying described in step 7 is alcohol vapor, the overcritical temperature being finally reached
It is 253 DEG C, air pressure 8.9MP, 6 ~ 10h of drying time.
Detailed description of the invention
Fig. 1 is 1000 DEG C of silica/alumina binary aerogel prepared by the present invention treated photomacrograph.
Fig. 2 is the nitrogen adsorption desorption curve graph for the silica/alumina binary aerogel that embodiment 4 is prepared.
Specific embodiment
Embodiment 1
It is 10ml that 0.25gPEG2000, which is added to the ratio between deionized water and ethyl alcohol,：The in the mixed solvent of 10ml, when stirring one section
Between after, make it completely dissolved in solvent；2.168g chlorination aluminium salt is weighed, PEG2000 is added to and dissolves in complete mixed solution,
It stirs to it and is completely dissolved；1ml ethyl orthosilicate is measured with pipette, is added in mixed solution, is stirred when being added dropwise, is added dropwise
12h is persistently stirred after complete, is fully hydrolyzed it, after hydrolyzing completely, is measured 8ml propylene oxide and is added in mixed solution, stir
After mixing 2min, solution is transferred in gelling vessel to its gel, wet gel is placed in organic solvent protection at a certain temperature
Wet gel, is placed in alcohol solvent after aging and replaces 6d by lower aging, replaces an ethanol solution every 12h.By what is replaced
6h is dried by supercritical drying process in wet gel, finally obtains two aeroge of silica/alumina of certain shapes.
Obtained aeroge sample rate is 0.094g/cm3, specific surface area 599m2/ g, Kong Rongwei 6.10cm3/ g,
Average pore size is 35.9nm.
Embodiment 2
It is 10ml that 0.25gPEG2000, which is added to the ratio between deionized water and ethyl alcohol,：The in the mixed solvent of 10ml, when stirring one section
Between after, make it completely dissolved in solvent；3.253g chlorination aluminium salt is weighed, PEG2000 is added to and dissolves in complete mixed solution,
It stirs to it and is completely dissolved；1ml ethyl orthosilicate is measured with pipette, is added in mixed solution, is stirred when being added dropwise, is added dropwise
12h is persistently stirred after complete, is fully hydrolyzed it, after hydrolyzing completely, is measured 8ml propylene oxide and is added in mixed solution, stir
After mixing 2min, solution is transferred in gelling vessel to its gel, wet gel is placed in organic solvent protection at a certain temperature
Wet gel, is placed in alcohol solvent after aging and replaces 6d by lower aging, replaces an ethanol solution every 12h.By what is replaced
6h is dried by supercritical drying process in wet gel, finally obtains two aeroge of silica/alumina of certain shapes.
Obtained aeroge sample rate is 0.098g/cm3, specific surface area 572m2/ g, Kong Rongwei 5.87cm3/ g,
Average pore size is 29.2nm.
Embodiment 3
It is 10ml that 0.25gPEG2000, which is added to the ratio between deionized water and ethyl alcohol,：The in the mixed solvent of 8ml, when stirring one section
Between after, make it completely dissolved in solvent；6.506g chlorination aluminium salt is weighed, PEG2000 is added to and dissolves in complete mixed solution,
It stirs to it and is completely dissolved；1ml ethyl orthosilicate is measured with pipette, is added in mixed solution, is stirred when being added dropwise, is added dropwise
12h is persistently stirred after complete, is fully hydrolyzed it, after hydrolyzing completely, is measured 10ml propylene oxide and is added in mixed solution, stir
After mixing 2min, solution is transferred in gelling vessel to its gel, wet gel is placed in organic solvent protection at a certain temperature
Wet gel, is placed in alcohol solvent after aging and replaces 6d by lower aging, replaces an ethanol solution every 12h.By what is replaced
6h is dried by supercritical drying process in wet gel, finally obtains two aeroge of silica/alumina of certain shapes.
Obtained aeroge sample rate is 0.1019g/cm3, specific surface area 563m2/ g, Kong Rongwei 5.72cm3/ g,
Average pore size is 37.4nm.
Embodiment 4
It is 10ml that 0.25gPEG2000, which is added to the ratio between deionized water and ethyl alcohol,：The in the mixed solvent of 10ml, when stirring one section
Between after, make it completely dissolved in solvent；3.253g chlorination aluminium salt is weighed, PEG2000 is added to and dissolves in complete mixed solution,
It stirs to it and is completely dissolved；1ml ethyl orthosilicate is measured with pipette, is added in mixed solution, is stirred when being added dropwise, is added dropwise
12h is persistently stirred after complete, is fully hydrolyzed it, after hydrolyzing completely, is measured 10ml propylene oxide and is added in mixed solution, stir
After mixing 2min, solution is transferred in gelling vessel to its gel, wet gel is placed in organic solvent protection at a certain temperature
Wet gel, is placed in alcohol solvent after aging and replaces 6d by lower aging, replaces an ethanol solution every 12h.By what is replaced
6h is dried by supercritical drying process in wet gel, finally obtains two aeroge of silica/alumina of certain shapes.
Obtained aeroge sample rate is 0.086g/cm3, specific surface area 845m2/ g, Kong Rongwei 7.21cm3/ g,
Average pore size is 29.5nm.
Embodiment 5
It is 10ml that 0.25gPEG2000, which is added to the ratio between deionized water and ethyl alcohol,：The in the mixed solvent of 10ml, when stirring one section
Between after, make it completely dissolved in solvent；3.253g chlorination aluminium salt is weighed, PEG2000 is added to and dissolves in complete mixed solution,
It stirs to it and is completely dissolved；1ml ethyl orthosilicate is measured with pipette, is added in mixed solution, is stirred when being added dropwise, is added dropwise
12h is persistently stirred after complete, is fully hydrolyzed it, after hydrolyzing completely, is measured 10ml propylene oxide and is added in mixed solution, stir
After mixing 2min, solution is transferred in gelling vessel to its gel, wet gel is placed in organic solvent protection at a certain temperature
Wet gel, is placed in alcohol solvent after aging and replaces 10d by lower aging, replaces an ethanol solution every 12h.By what is replaced
6h is dried by supercritical drying process in wet gel, finally obtains two aeroge of silica/alumina of certain shapes.
Obtained aeroge sample rate is 0.096g/cm3, specific surface area 864m2/ g, Kong Rongwei 7.06cm3/ g,
Average pore size is 42.7nm.
Presently preferred embodiments of the present invention is illustrated above, but the present invention is not limited to the embodiment,
Those skilled in the art can also make various equivalent variation or replacement on the premise of without prejudice to spirit of the invention,
These equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (8)
1. a kind of preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel, it is characterised in that made in the steps below
It is standby：
Step 1：PEG2000 is added to the in the mixed solvent of deionized water and ethyl alcohol, after stirring a period of time, makes it completely
It is dissolved in solvent；
Step 2：The chlorination aluminium salt for weighing certain mass is added to PEG2000 and dissolves in complete mixed solution, stirs to it
It is completely dissolved；
Step 3：The ethyl orthosilicate for measuring certain volume, is added in mixed solution, stirs when being added dropwise, holds after dripping
Continuous stirring 12h ~ for 24 hours, it is fully hydrolyzed it；
Step 4：After hydrolyzing completely, measures a certain amount of propylene oxide and be added in mixed solution, it, will after stirring 1 ~ 3min
Solution is transferred in gelling vessel to its gel；
Step 5：By wet gel, surface covers aging in one layer of organic solvent at a certain temperature；
Step 6：Wet gel is placed in alcohol solvent after aging and is replaced；
Step 7：The wet gel replaced is dried through supercritical drying process, finally obtain the silica of certain shapes/
Aluminium oxide binary aerogel.
2. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, feature exist
In the ratio between in the mixed solvent deionized water and ethyl alcohol are preferably 10ml in the step 1：10ml, PEG2000 and solvent quality
Than being 1：80.
3. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, which is characterized in that
The mass ratio of amount and solvent that chlorination aluminium salt is added in the step 2 is 1：3~1：10.
4. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, which is characterized in that
The ratio between mole of amount and chlorination aluminium salt that ethyl orthosilicate is added in the step 3 is 1：2~1：8.
5. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, which is characterized in that
The molar ratio of amount and chlorination aluminium salt that propylene oxide is added in the step 4 is 6：1~8：1.
6. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, which is characterized in that
Organic solvent is one kind of ethyl alcohol, methanol in the step 5, and aging temperature is 20 ~ 30 DEG C, and the time is 0 ~ 2d.
7. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, which is characterized in that
The time swap of ethyl alcohol is 4 ~ 10d in the step 6, and every 12h replaces a replacement fluid.
8. the preparation method of high temperature oxidation resisting silicon/aluminium oxide binary aerogel according to claim 1, which is characterized in that
Dried medium selected by supercritical drying is alcohol vapor in the step 7, and the overcritical temperature being finally reached is 253 DEG C,
Air pressure is 8. 9MP, 6 ~ 10h of drying time.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639437A (en) * | 2019-08-16 | 2020-01-03 | 航天特种材料及工艺技术研究所 | Preparation method of silicon-aluminum oxide composite aerogel based on non-hydrolytic sol-gel technology |
| CN111807810A (en) * | 2019-04-12 | 2020-10-23 | 北京化工大学 | Preparation method of nanowire/silicon-aluminum aerogel composite material |
| CN112430301A (en) * | 2020-11-12 | 2021-03-02 | 阳谷新太平洋电缆有限公司 | Low-smoke halogen-free flame-retardant heat-insulating material and application thereof in photoelectric composite rubber jacketed flexible cable of coal mining machine |
| CN116143132A (en) * | 2022-12-09 | 2023-05-23 | 中国科学院工程热物理研究所 | Method for preparing complete massive silica-alumina composite aerogel based on freeze drying |
-
2017
- 2017-05-11 CN CN201710331365.6A patent/CN108854873A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807810A (en) * | 2019-04-12 | 2020-10-23 | 北京化工大学 | Preparation method of nanowire/silicon-aluminum aerogel composite material |
| CN110639437A (en) * | 2019-08-16 | 2020-01-03 | 航天特种材料及工艺技术研究所 | Preparation method of silicon-aluminum oxide composite aerogel based on non-hydrolytic sol-gel technology |
| CN110639437B (en) * | 2019-08-16 | 2022-01-04 | 航天特种材料及工艺技术研究所 | Preparation method of silicon-aluminum oxide composite aerogel based on non-hydrolytic sol-gel technology |
| CN112430301A (en) * | 2020-11-12 | 2021-03-02 | 阳谷新太平洋电缆有限公司 | Low-smoke halogen-free flame-retardant heat-insulating material and application thereof in photoelectric composite rubber jacketed flexible cable of coal mining machine |
| CN116143132A (en) * | 2022-12-09 | 2023-05-23 | 中国科学院工程热物理研究所 | Method for preparing complete massive silica-alumina composite aerogel based on freeze drying |
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Application publication date: 20181123 |