CN102613245B - Preparation method of nano-silica aerogels - Google Patents
Preparation method of nano-silica aerogels Download PDFInfo
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- CN102613245B CN102613245B CN201210078274.3A CN201210078274A CN102613245B CN 102613245 B CN102613245 B CN 102613245B CN 201210078274 A CN201210078274 A CN 201210078274A CN 102613245 B CN102613245 B CN 102613245B
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Abstract
The invention discloses a preparation method of nano-silica aerogels. The preparation method comprises the following steps of: (1) mixing ethyl orthosilicate with a titanium compound; (2) mixing an alcohol solvent with a mixture and diluting the mixture to get a mixed solution; (3) slowly dripping dilute ammonia water till the pH value of the solution is 7-10, continuing stirring, enabling the solution to form sols and aging to gels; and (4) performing supercritical drying processing on the obtained gels to get silica-titanium dioxide composite aerogels. According to the method, nano-scale titanium dioxide is attached on the silica aerogels with high specific surface, so that the aggregation of nano-titanium oxide is effectively prevented and the activity of the titanium oxide is enhanced.
Description
Technical field
The present invention relates to a preparation about nanometer titanium dioxide silica aerogel, particularly make to be attached to the preparation method of a kind of nanometer titanium dioxide silica aerogel of the increased activity of titanium oxide on the aerosil of high-ratio surface.
Background technology
Nano-titanium oxide, because it has high activity, has special purposes at aspects such as antibacterial, self-cleaning, solar cell, water purification.But because titanium oxide is in the process of preparation, often easily produces and reunite, make the material particle size prepared bigger than normal, its usefulness is also unsatisfactory.Having now a kind of method is in the process of preparing titanium dioxide nano material, to adopt surface coating technology to reduce the reunion between particle, and titanium oxide activity is increased greatly.But so still can not meet the needs of titanium oxide in association area.Its light degradation ability of nano rutile-type titania aeroge that known prior art is produced is that staphylococcus aureus degradation rate is 90.5%, and Escherichia coli degradation rate is 89.9%, and in photoactivate battery material, optoelectronic transformation efficiency is in 7% left and right.
Summary of the invention
For problems of the prior art and deficiency, the object of the present invention is to provide a kind of preparation method of nanometer titanium dioxide silica aerogel, the method is attached to Nano titanium dioxide on the aerosil of high-ratio surface, effectively stop the reunion of nano-titanium oxide, made the increased activity of titanium oxide.
The object of the invention is to realize by following technical proposals:
A preparation method for high-activity nano aerosil, the method comprises the steps:
1) raw material is prepared: ethyl orthosilicate is mixed according to mass ratio with titanium compound be 1: 0.4-2 ratio is mixed;
2) raw material dilution: be 10 with mixture according to mass ratio by alcoholic solvent: 1.4-3 ratio is mixed, and is mixed liquor by mixture diluted;
3) sol-gel: slowly drip the ammoniacal liquor of 5%-10% until pH is 7-10, continue to stir 30-60 minute, until white depositions disappears, in the time that elementary cell concentration is increasing in colloidal sol, just possess the basis of condensation reaction, slowly form gel; It is gel that solution forms colloidal sol extremely aging;
4) dry processing: just can carry out the preparation of aeroge after gel is aging, select Supercritical Drying Technology to process alcogel.By step 3) gained gel carries out supercritical drying in 243-290 ℃, pressure 8-20Mpa and processes 6-12 hour, obtains silica-titania composite aerogel.
Its product detects and uses biological antibiotic to detect and photoactivate cell photoelectric conversion ratio.
Further aspect of the present invention is:
On the basis of preparing high specific surface silica aerogel, need the compound of titaniferous to do meticulous selection, generally selecting titanium compound is one or more in common titanium dioxide powder, titanium tetrachloride, butyl titanate or titanyl sulfate.
In the time selecting titania powder as titanium compound, add a kind of siliceous emulsifier if silicone emulsion is as solvent simultaneously.
Described alcoholic solvent is the one in ethanol, methyl alcohol or propyl alcohol.
The present invention utilize aeroge high-ratio surface and and the duct of aeroge be perforate UNICOM state, TiOx nano particle is attached to the open cell channels of aeroge or forms titanium silicate nanostructured hole wall together with silica, most of titanium oxide are embedded among aeroge structure with molecular architecture.
Its light degradation ability of nano rutile-type titania aeroge that known prior art is produced is that staphylococcus aureus degradation rate is 90.5%, and Escherichia coli degradation rate is 89.9%, and in photoactivate battery material, optoelectronic transformation efficiency is in 7% left and right.The nano-titanium oxide aeroge most optimum materials of preparing by the present invention is 99.5% to staphylococcus aureus degradation rate, and Escherichia coli degradation rate is 99.9%, and in photoactivate battery material, optoelectronic transformation efficiency is 11%.
Embodiment
Below in conjunction with specific embodiment, the performance of nano-titanium oxide aeroge is described.
Embodiment 1
Taking 1000 grams of 40# ethyl orthosilicates mixes with 400 grams of high-purity titanium dioxide powder, add while stirring 10 liters of ethanol and 50 grams of silicone emulsions, high speed shear stirs 5 minutes, changing 80 revs/min of constant speed into stirs, slowly the ammoniacal liquor of dropping 5% is until pH is 9, continuation is stirred until solution viscosity reaches 5000 centipoises, continues to stir 30 minutes, and it is gel that solution forms colloidal sol extremely aging; Stop stirring, treat the formation of gel, carry out supercritical drying processing after gel is aging, drying condition is 290 ℃ of temperature; Pressure 20Mpa; Processing time is 12 hours, must adsorb the silica-titania composite aerogel of titanium dioxide.
Take 5 grams, prepared sample, porphyrize in mortar, respectively gets respectively 1 gram and does antibacterial experiment, separately get 2 grams with do photoactivate test, be consequently 97.1% to staphylococcus aureus degradation rate, Escherichia coli degradation rate is 97.9%, and in photoactivate battery material, optoelectronic transformation efficiency is 9%.
Embodiment 2
Take 1000 grams of 40# ethyl orthosilicates and mix with 2000 grams of titanium tetrachlorides, add while stirring 10 liters of propyl alcohol, 80 revs/min of constant speed stir, and slowly drip 5% ammoniacal liquor until pH is 10, continue to stir 50 minutes, and it is gel that solution forms colloidal sol extremely aging; Stop stirring, treat the formation of gel, carry out supercritical drying processing after gel is aging, drying condition is 260 ℃ of temperature; Pressure 15Mpa; Processing time is 12 hours, must adsorb silica-titania composite aerogel.
Take 5 grams, prepared sample, porphyrize in mortar, respectively gets respectively 1 gram and does antibacterial experiment, separately get 2 grams with do photoactivate test, be consequently 99.1% to staphylococcus aureus degradation rate, Escherichia coli degradation rate is 98.7%, and in photoactivate battery material, optoelectronic transformation efficiency is 10%.
Embodiment 3
Taking 1000 grams of 40# ethyl orthosilicates mixes with 1000 grams of butyl titanates, add while stirring 10 liters of ethanol, 80 revs/min of constant speed stir, slowly the ammoniacal liquor of dropping 8% is until pH is 7, continue to stir until solution viscosity reaches 5000 centipoises, continue to stir 60 minutes, it is gel that solution forms colloidal sol extremely aging; Stop stirring, treat the formation of gel, carry out supercritical drying processing after gel is aging, drying condition is 280 ℃ of temperature; Pressure 8Mpa; Processing time is 10 hours, obtains silica-titania composite aerogel.
Take 5 grams, prepared sample, porphyrize in mortar, respectively gets respectively 1 gram and does antibacterial experiment, separately get 2 grams with do photoactivate test, be consequently 99.7% to staphylococcus aureus degradation rate, Escherichia coli degradation rate is 99.9%, and in photoactivate battery material, optoelectronic transformation efficiency is 11%.
Embodiment 4
Take 1000 grams of 40# ethyl orthosilicates and mix with 2000 grams of titanyl sulfates, add while stirring 10 liters of methyl alcohol, 80 revs/min of constant speed stir, and slowly drip 10% ammoniacal liquor until pH is 7, continue to stir 40 minutes, and it is gel that solution forms colloidal sol extremely aging; Stop stirring, treat the formation of gel, carry out supercritical drying processing after gel is aging, drying condition is 243 ℃ of temperature; Pressure 20Mpa; Processing time is 6 hours, must adsorb silica-titania composite aerogel.
Take 5 grams, prepared sample, porphyrize in mortar, respectively gets respectively 1 gram and does antibacterial experiment, separately get 2 grams with do photoactivate test, be consequently 99% to staphylococcus aureus degradation rate, Escherichia coli degradation rate is 98.7%, and in photoactivate battery material, optoelectronic transformation efficiency is 10%.
The above; only for preferably embodiment of the present invention, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.
Claims (1)
1. a preparation method for nanometer titanium dioxide silica aerogel, is characterized in that, the method comprises the steps:
1) be that 1:0.4-2 ratio mix with titanium compound according to mass ratio by ethyl orthosilicate;
2) being that 10:1.4-3 ratio mix with the mixture of step 1) according to mass ratio by alcoholic solvent, is mixed liquor by mixture diluted;
3) slowly drip the ammoniacal liquor of 5-10% until pH is 7-10, continue to stir 30-60 minute, it is gel that solution forms colloidal sol extremely aging;
4) step 3) gained gel is carried out to supercritical drying in 243-290 ℃, pressure 8-20Mpa and process 6-12 hour, obtain silica-titania composite aerogel;
Described alcoholic solvent is the one in ethanol, methyl alcohol or propyl alcohol;
Described titanium compound is titania powder, when described selection titania powder, adds silicone emulsion as solvent simultaneously.
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| CN107523198A (en) * | 2017-07-26 | 2017-12-29 | 贵州省漆彩金州涂料有限公司 | A kind of aerosil coating manufacture craft |
| CN111362664B (en) * | 2020-02-18 | 2022-04-22 | 江苏泛亚微透科技股份有限公司 | Preparation method of aluminum-titanium doped silicon dioxide aerogel/fiber composite material |
| CN111528229A (en) * | 2020-04-16 | 2020-08-14 | 江苏斯迪克新材料科技股份有限公司 | Long-acting antibacterial agent |
| CN114261986B (en) * | 2022-01-18 | 2023-10-13 | 中国科学技术大学先进技术研究院 | Preparation method of aerogel material and application of aerogel material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1214319A (en) * | 1997-10-10 | 1999-04-21 | 同济大学 | Modified nanometer heat insulating material and its production process |
| CN1224047A (en) * | 1998-01-23 | 1999-07-28 | 中国科学院山西煤炭化学研究所 | Catalyst for combustion of natural gas and preparing process thereof |
| CN1546225A (en) * | 2003-12-17 | 2004-11-17 | 同济大学 | TiO2/SiO2 aerogel globule and method for making same |
| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| CN101288835A (en) * | 2008-06-02 | 2008-10-22 | 大连工业大学 | TiO2-SiO2 compound aerogel and its preparation method |
| US20090123985A1 (en) * | 2007-11-10 | 2009-05-14 | Chung Yuan Christian University | Method for fabricating aerogels and their application in biocomposites |
-
2012
- 2012-03-22 CN CN201210078274.3A patent/CN102613245B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1214319A (en) * | 1997-10-10 | 1999-04-21 | 同济大学 | Modified nanometer heat insulating material and its production process |
| CN1224047A (en) * | 1998-01-23 | 1999-07-28 | 中国科学院山西煤炭化学研究所 | Catalyst for combustion of natural gas and preparing process thereof |
| CN1546225A (en) * | 2003-12-17 | 2004-11-17 | 同济大学 | TiO2/SiO2 aerogel globule and method for making same |
| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| US20090123985A1 (en) * | 2007-11-10 | 2009-05-14 | Chung Yuan Christian University | Method for fabricating aerogels and their application in biocomposites |
| CN101288835A (en) * | 2008-06-02 | 2008-10-22 | 大连工业大学 | TiO2-SiO2 compound aerogel and its preparation method |
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