CN1724354A - A kind of method that improves thermal stability of silicon dioxide deroyel - Google Patents
A kind of method that improves thermal stability of silicon dioxide deroyel Download PDFInfo
- Publication number
- CN1724354A CN1724354A CN 200510027544 CN200510027544A CN1724354A CN 1724354 A CN1724354 A CN 1724354A CN 200510027544 CN200510027544 CN 200510027544 CN 200510027544 A CN200510027544 A CN 200510027544A CN 1724354 A CN1724354 A CN 1724354A
- Authority
- CN
- China
- Prior art keywords
- aerosil
- sample
- aerogel
- concentration
- silicon dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of method that can improve the thermostability of aerosil.At first, according to silicon sol: ethanol: nitric acid=10～20: 2～15: 1～2 volume ratio is measured, and obtains alcogel after mixing thoroughly.After 50 ℃ of following constant temperature 12-24h are aging, with soaked in absolute ethyl alcohol 1-2 time, be 80% alcohol immersion 24h then with concentration, be 1: 1 tetraethoxy and alcoholic acid mixed liquid dipping 48h again with volume ratio, the gained gel places 70 ℃ of freeze-day with constant temperature 72h, promptly obtains silica aerogel.Use 0.2～1.5molL then
-1Iron nitrate solution soak 72h, be that 0.5～2% weak ammonia soaks 24h with concentration again, clean with ethanolic soln then, use soaked in absolute ethyl alcohol 12h, the sealing of gained sample places 70 ℃ of thermostat container inner drying 72h, i.e. assembling obtains nanoparticle-aerogel mesic hole compound sample.Technology of the present invention is simple, with low cost, equipment requirements and input is low, thermostability obviously improves: the mean pore size 24.7～26.5nm of the sample after 1000 ℃ of thermal treatment, pore volume is up to 0.927～0.951cm
3G
-1, specific surface area is then up to 138.0565～148.0979m
2G
-1
Description
Technical field
The present invention relates to a kind of method that can improve the thermostability of aerosil.Specifically be assembling Fe in aerogel is mesoporous
2O
3The technology of nanoparticle.The doped F e of Huo Deing in this way
2O
3The SiO of nanoparticle
2Aerogel can overcome common SiO
2Aerogel is the not high shortcoming of poor heat stability, physical strength in actual applications.
Background technology
Aerosil is coalescent mutually by Nano particles of silicon dioxide, constitute the vesicular network structure, and in the hole of vesicular network structure, be full of the solid-state material of a kind of high dispersive of air, it is at calorifics, electricity, optics, aspects such as acoustics have special performance, thereby have a wide range of applications.This aerogel has particular structure and a lot of good performances, but will further utilize its specific performance to carry out practical application the time, must improve its structure, makes it to adapt to the special requirement of Application Areas.The physical strength of pure silicon aerogel is not high, its vesicular structure easy sintering and suffer serious destruction again under hot conditions, and the high temperature heat radiation effect obviously strengthens, make its elevated temperature heat conductance increase considerably, and this has influenced its application in elevated temperature heat insulating material field.Assemble nanometer particulate in aerogel, can not only improve performances such as the structural strength of aerogel itself, heat-resisting and high temperature thermal resistance, but also might bring into play the catalysis of nanoparticle and inhale performance such as ripple, therefore, exploration assemble nanometer particulate in aerosil prepares the doping aerogel, and the research that improves the high-temperature heat-resistance performance of aerosil has practical significance.
The existing a spot of report in the preparation home and abroad of at present relevant doping aerogel.United States Patent (USP) (' Glycerol-doped aerogel coatings as biological capture media ' US20030207304) relates to a kind of polyol doping aerogel material, this aerogel is applied to the trapping of biological particle, helps analysis and evaluation to biological particle; (' Aerogel backed ultrasound transducer ' US20010014775) relates to a kind of preparation of aerogel acoustic lining, thereby covering or doping metals make aerogel possess conductive capability on the aerogel acoustic lining; (' Smart aerogel ' US 6,447,991) relate to a kind of method of the compound with particular organisms avidity of mixing in aerogel, this aerogel with particular organisms avidity that mixed is applied to surveying and identifying microorganisms such as bacterium, virus, toxin.Chinese patent application (' modified nanometer heat insulating material and production technique thereof ' CN97106652.3) relates to a kind of composition and production technique of doping vario-property nanometer foam silica aerogel heat preserving and insulating material, this invention is the very thin network that nano SiO 2 particle is cross-linked to form, among network, inlay titanium dioxide and inorganic strengthening agent again, but it is extremely inhomogeneous that the doped silicon aerogel of this method gained is formed, but also be very easy to cracking and fragmentation; (' aerogel composite that contains fiber ' CN96196880.X) relates to the matrix material that preparation contains 5-97% (volume) aerogel particle, at least a binding agent and at least a filamentary material, the skewness of filamentary material in this aerogel composite, and the binding agent of introducing decomposition easily in heat-processed, suppress its range of application greatly.So, up to now, also do not find both at home and abroad simple, the with low cost and method of the raising thermal stability of silicon dioxide deroyel that quality is higher of technology.
Summary of the invention
The method of the thermostability that can improve aerosil that the objective of the invention is to disclose that a kind of technology is simple, with low cost, equipment requirements and input is low.The SiO2 aerogel of the dopen Nano particulate of Huo Deing can overcome common SiO in this way
2Aerogel is shortcoming such as not high, poor heat stability of physical strength in actual applications, for aerosil lays the first stone in the practical application aspect the high temperature thermal insulation material.
For achieving the above object, the present invention assemble nanometer Fe in the general silica aerogel of appropriate bore structure is mesoporous
2O
3Particulate, preparation nanoparticle-aerogel mesic hole compound, thus improve the thermostability method of aerogel on calorifics.At first, selecting cheap silicon sol is main raw material, at first prepare the bulk silicon aerogel, the aqueous solution soaking of an amount of bulk silicon aerogel, soak with weak ammonia more again, clean with ethanolic soln then with metal nitrate, use soaked in absolute ethyl alcohol after removing residual solution, remove ethanol, gained sample sealed thermostat drying, i.e. assembling obtains improving the aerosil (nanoparticle-aerogel mesic hole compound) of thermostability.
Concrete technology is as follows:
The first step: the preparation of silica aerogel
At first, according to silicon dioxide gel: ethanol: nitric acid=10～20: 3～15: 1～2 volume ratio (v/v) is measured, and wherein nitric acid is 5% weight percent concentration (w/w), and ethanol is dehydrated alcohol.Earlier add nitric acid in silicon sol, under agitation, add dehydrated alcohol, after stirring, obtaining mixed solution is alcogel.Alcogel is transferred in the sealed vessel, after 50 ℃ of following constant temperature 12-24 hour (h) are aging, use soaked in absolute ethyl alcohol 1-2 time earlier, be the alcohol immersion 24h of 80% quality percentage (v/v) then with concentration, carry out exchange of solvent, be the tetraethoxy and the alcoholic acid mixed liquid dipping 48h of 1: 1 (v/v) with volume ratio again, the gained gel places 70 ℃ of freeze-day with constant temperature 72h., promptly obtain the silica aerogel sample.
Second step: the preparation of the aerosil that thermostability is high
With the silica aerogel of the first step with 0.2～1.5molL
-1Iron nitrate solution be that soak solution soaks 72h, be the weak ammonia immersion 24h of 0.5～2% quality percentage again with concentration, be that 65% aqueous ethanolic solution cleans with concentration then, remove residual solution in the sample, use soaked in absolute ethyl alcohol 12h, remove ethanol, the sealing of gained sample places 70 ℃ of thermostat container inner drying 72h, i.e. assembling obtains the aerosil (nanoparticle-aerogel mesic hole compound) that thermostability obviously improves.
The present invention has the following advantages:
1. to have selected the aerosil of appropriate bore structure be presoma in the present invention, soaks by iron nitrate solution, assembles Fe in aerosil is mesoporous
2O
3Nanoparticle, preparation nanoparticle-aerogel mesic hole compound material, its operating procedure is simple, condition is controlled easily, equipment requirements is low, with low cost.
2. the present invention has overcome doped silicon aerogel composition heterogeneity and the easy cracked shortcoming that tougheners such as inlaying inorganic fibre in the aerogel sol-gel process in early stage makes, the doping aerogel of the assemble nanometer particulate that obtains has higher intensity, and becomes piece good.
3. the present invention assemble in situ Fe in the silica aerogel hole
2O
3Nanoparticle prepares in the doping aerogel process, Fe
2O
3Nanoparticle is assembled on the inwall of aerosil hole with the form of monolayer of particles, do not need to add any additives, so technology is reliable.
4. by in silica aerogel, assembling Fe
2O
3The doping silicon dioxide aerogel that nanoparticle makes, the about 24.7nm of the mean pore size of the sample after 1000 ℃ of thermal treatment, pore volume is up to 0.951cm
3G
-1, specific surface area is then up to 148.0979m
2G
-1And the about 10nm of mean pore size of the sample of pure silicon dioxide aerogel after 1000 ℃ of thermal treatment, pore volume only is 0.004cm
3G
-1, specific surface area also has only 1.3713m
2G
-1Compare assembling Fe with the pure silicon dioxide aerogel
2O
3The thermostability of the doping silicon dioxide aerogel that makes after the nanoparticle is significantly improved.
Embodiment
Embodiment 1
The present invention at first is that catalyzer makes typical aerosil sample with the salpeter solution.The proportioning of reaction system is a silicon dioxide gel: ethanol: nitric acid=10: 3: 2 volume ratios (v/v), and silicon sol is commercially available, and nitric acid is 5% weight percent concentration (w/w), and ethanol is dehydrated alcohol.Silicon sol is placed in the beaker, adds nitric acid, under the continuous stirring of magnetic stirring apparatus, with transfer pipet dehydrated alcohol is added, after stirring, obtaining mixed solution is alcogel.The alcogel of gained is transferred in the sealed vessel at 50 ℃ of following constant temperature, carry out 12-24h aging after, use soaked in absolute ethyl alcohol 1-2 time earlier, with the alcohol immersion of alcogel,, carry out exchange of solvent then at 50 ℃ of following constant temperature 24h with 80% (v/v), use tetraethoxy and alcoholic acid mixed solution (1: 1 again, v/v) soak 48h, the gained gel places 70 ℃ of freeze-day with constant temperature 72h, promptly obtains block aerosil sample.
Then in block aerosil sample, assemble Fe
2O
3Nanoparticle.Adopt 0.2molL
-1Iron nitrate solution be soak solution, block aerosil sample put into wherein soak 72h, be the weak ammonia immersion 24h of 0.5% quality percentage again with concentration, clean with ethanolic soln at last, remove residual solution in the sample, use soaked in absolute ethyl alcohol 12h, remove ethanol, the sealing of gained sample places 70 ℃ of thermostat container inner drying 72h, i.e. assembling obtains the aerosil (nanoparticle-aerogel mesic hole compound) that thermostability obviously improves.The about 26.5nm of mean pore size of the sample of this aerosil after 1000 ℃ of thermal treatment, pore volume is up to 0.927cm
3G
-1, specific surface area is then up to 138.0565m
2G
-1
Embodiment 2
The proportioning of reaction system is a silicon sol: ethanol: nitric acid=20: 15: 1 volume ratios (v/v), all the other steps are identical with embodiment 1, make block aerosil sample.Adopt 1.5molL
-1Iron nitrate solution be soak solution, block aerosil sample is put into wherein, soak 72h, be the weak ammonia immersion 24h of 2% quality percentage with concentration again, clean with ethanolic soln then, remove residual solution in the sample, use soaked in absolute ethyl alcohol 12h, remove ethanol, the sealing of gained sample places 70 ℃ of thermostat container inner drying 72h, and assembling obtains the aerosil (nanoparticle-aerogel mesic hole compound sample) that thermostability obviously improves.The about 24.7nm of mean pore size of the sample of this aerosil after 1000 ℃ of thermal treatment, pore volume is up to 0.951cm
3G
-1, specific surface area is then up to 148.0979m
2G
-1And the about 10nm of mean pore size of the sample of pure silicon dioxide aerogel after 1000 ℃ of thermal treatment, pore volume only is 0.004cm
3G
-1, specific surface area also has only 1.3713m
2G
-1, to compare with the pure silicon dioxide aerogel, the thermostability of doping silicon dioxide aerogel is significantly improved.
Claims (1)
1. method that improves thermal stability of silicon dioxide deroyel is characterized in that:
The first step: the preparation of aerosil
At first, according to silicon dioxide gel: ethanol: nitric acid=10～20: 2～15: 1～2 volume ratio is measured, and wherein the concentration of nitric acid is 5% weight percent, and ethanol is dehydrated alcohol.Earlier add nitric acid in silicon dioxide gel, under agitation, add dehydrated alcohol, after stirring, obtaining mixed solution is alcogel; Alcogel is transferred in the sealed vessel, after 50 ℃ of following constant temperature 12-24h are aging, use soaked in absolute ethyl alcohol 1-2 time earlier, be the alcohol immersion 24h of 80% quality percentage then with concentration, carry out exchange of solvent, be 1: 1 tetraethoxy and alcoholic acid mixed liquid dipping 48h again with volume ratio, the gained gel places 70 ℃ of freeze-day with constant temperature 72h, promptly obtains the silica aerogel sample;
Second step: the preparation of the aerosil that thermostability is high
With the aerosil of the first step with 0.2～1.5molL
-1Iron nitrate solution be that soak solution soaks 72h, be the weak ammonia immersion 24h of 0.5～2% quality percentage again with concentration, be that 65% ethanolic soln cleans with concentration then, remove residual solution in the sample, use soaked in absolute ethyl alcohol 12h, remove ethanol, the sealing of gained sample places 70 ℃ of thermostat container inner drying 72h, i.e. assembling obtains the aerosil that thermostability obviously improves; Mean pore size 24.7～the 26.5nm of the sample of this aerosil after 1000 ℃ of thermal treatment, pore volume is up to 0.927～0.951cm
3G
-1, specific surface area is then up to 138.0565～148.0979m
2G
-1
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510027544 CN1724354A (en) | 2005-07-06 | 2005-07-06 | A kind of method that improves thermal stability of silicon dioxide deroyel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510027544 CN1724354A (en) | 2005-07-06 | 2005-07-06 | A kind of method that improves thermal stability of silicon dioxide deroyel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1724354A true CN1724354A (en) | 2006-01-25 |
Family
ID=35924010
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510027544 Pending CN1724354A (en) | 2005-07-06 | 2005-07-06 | A kind of method that improves thermal stability of silicon dioxide deroyel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1724354A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444737B (en) * | 2008-12-22 | 2011-07-20 | 长沙星纳气凝胶有限公司 | Nickel-based catalyst for hydrogen production by ethanol steam reforming and preparation method thereof |
| CN101638237B (en) * | 2008-07-28 | 2012-06-13 | 广东道氏技术股份有限公司 | Method for quickly preparing silicondioxlde aerogel |
| CN103043673A (en) * | 2013-01-15 | 2013-04-17 | 赵峰 | Preparation method of silicon dioxide aerogel |
| CN105692631A (en) * | 2016-04-29 | 2016-06-22 | 广东工业大学 | Normal-pressure preparation method for silicon dioxide aerogel |
| CN110760291A (en) * | 2019-10-31 | 2020-02-07 | 哈尔滨工业大学 | Preparation method of silicate high-temperature wave-absorbing composite material |
-
2005
- 2005-07-06 CN CN 200510027544 patent/CN1724354A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638237B (en) * | 2008-07-28 | 2012-06-13 | 广东道氏技术股份有限公司 | Method for quickly preparing silicondioxlde aerogel |
| CN101444737B (en) * | 2008-12-22 | 2011-07-20 | 长沙星纳气凝胶有限公司 | Nickel-based catalyst for hydrogen production by ethanol steam reforming and preparation method thereof |
| CN103043673A (en) * | 2013-01-15 | 2013-04-17 | 赵峰 | Preparation method of silicon dioxide aerogel |
| WO2014110891A1 (en) * | 2013-01-15 | 2014-07-24 | Zhao Feng | Preparation method of silica aerogel |
| CN103043673B (en) * | 2013-01-15 | 2015-11-25 | 北京博天子睿科技有限公司 | A kind of preparation method of aerosil |
| CN105692631A (en) * | 2016-04-29 | 2016-06-22 | 广东工业大学 | Normal-pressure preparation method for silicon dioxide aerogel |
| CN105692631B (en) * | 2016-04-29 | 2019-03-22 | 广东工业大学 | A kind of atmospheric preparation method of aerosil |
| CN110760291A (en) * | 2019-10-31 | 2020-02-07 | 哈尔滨工业大学 | Preparation method of silicate high-temperature wave-absorbing composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6207098B1 (en) | Method for producing porous inorganic materials | |
| CN101503195B (en) | Method for preparing hydrophobic SiO2 aerogel | |
| CN101372337B (en) | Method for preparing transparent silicon dioxide aerogel by co-precursor normal atmosphere drying | |
| DE69732758T2 (en) | Process for the preparation of an airgel | |
| CN1317187C (en) | Process for preparing stephanoporate powder doped silica aerogel heat-insulation material | |
| KR101218508B1 (en) | Ceramic-carbon composites and its process | |
| CN1724354A (en) | A kind of method that improves thermal stability of silicon dioxide deroyel | |
| CN102020285A (en) | Preparation method for hydrophobic silica aerogel | |
| CN102276235A (en) | Method for improving infrared shading performance of aerogel heat-insulation composite material | |
| CN101638757B (en) | Method for steel fiber surface anticorrosion and modified treatment | |
| CN102515181B (en) | Method for improving strength of aerogel composite material | |
| CN103342367B (en) | Hydrophilic SiO2Method for producing aerogels | |
| CN105113213A (en) | Method for preparation of antioxidant composite coating on carbon fiber surface | |
| CN104609476B (en) | Method for using single-walled carbon nanotube as axis for preparation of coaxial composite nanowires | |
| CN1654324A (en) | Method for preparing SiO2 aerogel with nanometer apertures under normal pressure | |
| CN102294179B (en) | Preparation method of inorganic mesoporous membrane | |
| CN110918008A (en) | Foam-reinforced SiO2-TiO2Preparation method of composite aerogel | |
| CN104119060B (en) | Fiber is cross-linked the preparation method of aerogel composite | |
| CN104528743A (en) | Preparation method of mesoporous one-dimensional silicon dioxide nanofiber with high specific surface area | |
| CN109052465B (en) | Glass bead-nano titanium dioxide compound and preparation process thereof | |
| CN106829972A (en) | A kind of hydrophobic aerogels and preparation method thereof, aerogel blanket | |
| CN110193378A (en) | A kind of preparation method and applications of CuM/SAPO-34 molecular sieve | |
| Molo et al. | Application of silica rice husk ash for cellulase immobilized by sol-gel entrapment | |
| Pierre et al. | Applications of sol-gel processing | |
| CN111085183A (en) | Silicon oxide and titanium oxide composite material and synthesis method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20060125 |