CN103691414B - Preparation method of high-stability neutral photocatalyst sol for cement-based material - Google Patents
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Abstract
The invention belongs to the field of material science, and relates to a preparation method of a high-stability neutral photocatalyst sol for a cement-based material. The preparation method comprises the following steps of A, hydrolyzing a titanium salt, namely, adding an inorganic titanium salt as a raw material in an alkaline water solution for hydrolysis to obtain a white suspension; B, precipitating and filtering, namely, precipitating the white suspension obtained from the step A and washing multiple times; C, adding acid for peptizing, namely, adding a 0.1M dilute acid water solution in the obtained precipitate, thereby obtaining a bluish transparent TiO2 acidic sol; D, synthesizing the SiO2 sol, namely, hydrolyzing through dropping acid as a catalyst according to a mol ratio of tetraethoxysilane to alcohol of 1:24 in the alcohol to obtain an SiO2 sol; E, adding the SiO2 sol for improving the hydrophily in the bluish transparent TiO2 acidic sol obtained in the step C to obtain a mixed solution; and F, adding a prepared NaOH solution in the mixed sol obtained in the step D, and dispersing to an alcohol-water solution with a volume percent of 30-50 percent to obtain the high-stability neutral photocatalyst sol for the cement-based material.
Description
Technical field
The invention belongs to material science, relate to a kind of high-stability neutral photocatalyst sol preparation method for cement-based material.
Background technology
Cement as one of material the most widely used in Inorganic Non-metallic Materials, in common base field as building and road are able to large-scale application.In recent years, the pollution of building can damage move in company, hotel, the image such as bank and restaurant, therefore in the maintenance that exterior wall is attractive in appearance, need expensive fund.The exterior dirt polluting the most obvious heavy pollutant and stand in the breach as pollutant attachment produces of building, and the carbon of pollutant sources in the waste gas of motor vehicle emission and oil content are that main so-called urban type pollutes.
Photocatalyst is mainly with nanoscale TiO
2for the semi-conducting material general name with photo-catalysis function of representative.When photocatalyst is applied to substrate surface, utilize the photocatalysis of photocatalyst and photic super hydrophilicity, can by the organic matter degradation in attract dirt, inorganic matter then can be clean by rain drop erosion, realizes self-cleaning surface performance.Therefore, synthesis of nano TiO
2optical catalyst sol is also sprayed at cement-based material surface construction TiO
2film, is expected to play the effect purified air, and realizes the function without the need to manually knowing some building pollutions.
TiO
2the wet chemical methods of film owing to having advantage on cost, and is easy to realize, and obtains and studies comparatively widely.Wet chemical methods mainly comprises liquid phase deposition and sol-gel processing.Liquid phase deposition only needs leaching place substrate in corresponding reactant liquor, after certain hour reaction, can obtain the TiO of crystallization at deposition on substrate
2film, but the shortcoming of this method is not suitable for preparing TiO in large area
2film.The advantages such as it is low that sol-gel processing has preparation temperature, and technique is simple, can prepare the film that multicomponent mixes, and film particles degree is even, and purity is high, thus become preparation TiO
2the most common methods of film.
But sol-gel processing needs later stage high-temperature process to make TiO usually
2complete crystallization, but high-temperature process may cause base material element to TiO
2film diffusion inside, and easily cause TiO
2grain growth, causes photo-quantum efficiency and photocatalytic activity to reduce, and therefore this process seriously limits its application at the substrate surface of poor heat resistance.
For this reason, previously preparedly TiO is dispersed with
2nanocrystalline solution, utilizes its film afterwards at normal temperatures, realizes having crystalline TiO without the need to high-temperature process is just obtained
2film becomes the emphasis of people's research.Up to now, the common method preparing TiO 2 sol photochemical catalyst has: Sol-Gel-hydro-thermal method, Sol-Gel-low temperature dispergation method, amorphous TiO
2-low temperature dispergation method.Wherein chemical precipitation-dispergation method is preparation TiO
2colloidal sol has the method for application potential most.This method mainly utilizes inorganic titanium salt to obtain Ti (OH) as predecessor in advance with alkali reaction
4precipitation, and then add acid as degumming agent acquisition TiO
2.As adopted titanium tetrachloride, titanyl sulfate and metatitanic acid have prepared TiO as predecessor people
2colloidal sol (Journal of Sol-Gel Science and Technology. 25,121-136,2002; Journal of hazardous Materials. 152,347-355,2008), but due to the general acid resistance of cement-based material poor, adopt the acid optical catalyst sol of this acquisition certainly will damage base material.Therefore, need first synthesize the good efficiency light catalyst of neutral crystal property and then carry out coating film forming on cement matrix surface.About neutral TiO
2the preparation of optical catalyst sol, also has Patents to report.Chinese patent CN101049962A discloses a kind of nano-TiO of neutrality
2colloidal sol preparation method, the method introduces H
2o
2as complexing agent to Ti (OH)
4precipitation carries out dispergation, but TiO prepared by the method
2colloidal sol crystal property is poor, and photocatalytic activity is poor.Chinese patent CN102432063A discloses a kind of preparation method of the neutral Nanometer Titanium Dioxide Hydrosol for function fabric, the method is the modifier adding high score subclass in dispergation process, obtain the neutral hydrosol, but the modifier of this technology high score subclass in actual application is easily by TiO
2light degradation.In addition, Chinese patent CN101306838A also describes the neutral mixed crystal TiO of high stable
2nanocrystalline preparation method, but do not introduce about the application at cement-based material.Glass fiber cement sill (GRC) is with a wide range of applications in public building field is as building roof, building curtain wall, wall decoration, municipal traffic engineering construction, early stage, my company reported Nano self-cleaning fiber reinforced cement product and production method thereof at Chinese patent CN102518275, but there is no introduction about the detailed preparation that photocatalyst is produced.
Summary of the invention
The object of the invention is to provide a kind of high-stability neutral photocatalyst sol preparation method for cement-based material for above-mentioned weak point, is a kind of high-stability neutral photocatalyst sol preparation method synthesizing the application of applicable cement-based material, this TiO
2preparation method be convenient to industrialization, substantially increase nano-TiO
2in the application power on cement-based material surface.
A kind of high-stability neutral photocatalyst sol preparation method for cement-based material of the present invention realizes by the following technical programs:
A kind of high-stability neutral photocatalyst sol preparation method for cement-based material takes following steps:
A, titanium salt are hydrolyzed: select inorganic titanium salt as raw material, add in alkaline aqueous solution and be hydrolyzed, make solution be adjusted to neutral pH=7, obtain white suspension; Wherein said inorganic titanium salt is any one in titanium sulfate, titanyl sulfate or titanium chloride cheap and easy to get, the alkaline aqueous solution added be ammoniacal liquor, NaOH any one;
B, sedimentation and filtration washing: by centrifugal three times of above-mentioned A gained white suspension, precipitation is repeatedly washed, until the electrical conductivity of cleaning solution is less than 50 μ S/cm;
C, acid adding dispergation: the dilute acid solution adding 0.1M in the precipitation of gained; 60
odispergation 4 h under C, obtains nattier blue transparent TiO
2acidic sol; Described acid is any one in nitric acid, hydrochloric acid or sulfuric acid.
D, SiO
2colloidal sol synthesizes: using ethyl orthosilicate as raw material, is 1:24 in ethanol according to ethyl orthosilicate and ethanol mol ratio, to be hydrolyzed acquisition SiO as catalyst by dripping acid
2colloidal sol; Described acid is any one in nitric acid, hydrochloric acid or sulfuric acid, and instillation acid is 1:0.15 with the mol ratio of ethyl orthosilicate.
Add in E, nattier blue vitreosol of obtaining in C and can improve hydrophilic SiO
2colloidal sol, Keep agitation 0.5h ~ 4h, obtains mixed sols; Nattier blue transparent TiO
2colloidal sol and SiO
2colloidal sol mol ratio is 1:4.
The NaOH solution of the 0.1M configured is added in F, the mixed sols that obtains to E, regulate pH to neutral, by its rotary evaporation to containing the alcohol solution being again dispersed to volume fraction 30 % ~ 50% after a small amount of moisture content, obtain the high-stability neutral photocatalyst sol being used for cement-based material.
Because cement-based material is to nano-TiO
2colloidal sol
ph value has restriction, too low
ph value can damage the physical and mechanical properties of cement-based material.The present invention utilize inorganic titanium salt cheap and easy to get as raw material in preparation process to nano-TiO
2the hydrosol carries out modification, successfully directly prepares
ph value is close to the nano-TiO neutral, dispersion stabilization is good, photocatalysis performance is good
2colloidal sol.The present invention prepares cement based TiO
2the production cost of optical catalyst sol is low, is nano-TiO
2photochemical catalyst brings important breakthrough in the application in cement-based material field, has following outstanding feature:
1, the inorganic titanium salt raw material used in preparation process of the present invention is extensive, low price, and technique is simple, and convenient operation, is thus easy to carry out large-scale production.
2, the titania/silica hydrosol photocatalyst activity component TiO for preparing of the present invention
2colloidal sol be a few nanometer, even particle distribution, stability is fine, can not assemble and form flocculent deposit when can not precipitate and dilute after long storage time.
3, this nano-sized hydrosol is in neutral, can be widely used in cement-based material field, almost negligible to cement-based material damage.
4, containing inorganic binder in the prepared hydrosol, the adhesion on cement matrix surface is enhanced.
5, when the nano-sized hydrosol of preparation is coated on cement-based material surface, good photocatalytic self-cleaning is obtained active.
Accompanying drawing explanation
Below with reference to accompanying drawing, the invention will be further described:
Fig. 1 is TiO
2colloidal sol and same SiO
2be compounded to form neutral optical catalyst sol after drying powder XRD figure.
Fig. 2 is the SEM photo forming complex sol.
Fig. 3 is the EDS figure forming complex sol.
Fig. 4 is TiO
2spectrum over time during the neutral colloidal sol photocatalytic degradation rhodamine B of colloidal sol and photocatalyst.
Fig. 5 is that after the neutral colloidal sol of GRC cement matrix surface coating photocatalyst, rhodamine B is degraded change procedure in time.
Detailed description of the invention
Below with reference to embodiment, the invention will be further described:
Embodiment 1 TiO
2/ SiO
2the preparation of Compound Water colloidal sol:
(1) TiO
2the synthesis of acidic sol
In 100 mL water, add the aqueous solution that titanium sulfate is configured as 0.2 M, and carry out stirring 1 h and obtain clear transparent solutions.Add the ammonia spirit of a certain amount of 0.1M subsequently, regulate
ph is about 7, after ageing a period of time, centrifugal, with the sulfate (needing to remove because sulfate ion can cause precipitation) in abundant 3 the removing solution of deionized water, take out filter cake, after adding some deionized waters, add a certain amount of dilute nitric acid solution again, control its concentration for (10-20) wt %, regulate
ph is to about 1.Then 60
ocarry out stirring 4-6 h under C, obtain the transparent TiO with blue light
2colloidal sol.
(2) SiO
2the synthesis of colloidal sol
In cold bath, get 2-4mL ethyl orthosilicate and join in the ethanol of 40-50mL and stir 10 min, make it fully be mixed into homogeneous phase solution, add 1-3mL water afterwards, and instill 0.3 mLHNO
3, after dropwising, reactant mixture is warming up to 70 DEG C and stirring and refluxing 2-3h, after cooling, obtains SiO
2colloidal sol.
(3) photocatalyst TiO
2/ SiO
2the preparation of complex sol:
Get prepared TiO
2colloidal sol 40-60mL is placed in beaker, backward its add SiO prepared by 10-30mL
2colloidal sol, after stirring 1 h, drips the NaOH aqueous solution of 1M extremely wherein
ph=7, subsequently by this colloidal sol rotary evaporation to containing a small amount of moisture content, and to be re-dispersed into 500 mL volume fractions be in the methanol aqueous solution of 30%, the TiO needed for acquisition
2/ SiO
2complex sol.Fig. 1 is TiO
2colloidal sol and same SiO
2be compounded to form neutral optical catalyst sol after drying powder XRD figure, the TiO as can be seen from the figure prepared
2colloidal sol crystal property is better, presents anatase structured.And TiO
2same SiO
2after colloidal sol is compounded to form the neutral colloidal sol of photocatalyst, due to the SiO of synthesis
2for amorphous state, therefore still only there is TiO in optical catalyst sol
2diffraction maximum, and maintain good crystallinity.Fig. 2 is the stereoscan photograph obtaining complex sol, and the nano particle diameter as can be seen from the figure obtained is less, is about about 10-20nm.And to show in colloidal sol containing Na, O, Si and Ti signal in EDS spectrogram, illustrate in colloidal sol except including SiO
2and TiO
2outside, also have Na
2oSiO
2, this is conducive to the coating of colloidal sol on cement matrix surface.
Embodiment 2:
In 100 mL water, add the aqueous solution that a certain amount of titanium tetrachloride is configured to 0.2-0.5M, and carry out stirring 1 h and obtain clear transparent solutions.Add the ammonia spirit of a certain amount of 0.1M subsequently, regulate
ph is about 7.After ageing a period of time, centrifugal, with the Cl in abundant 3 the removing solution of deionized water
-, take out filter cake, after adding some deionized waters, then add a certain amount of dilute hydrochloric acid solution, controlling its concentration is 30-40wt %, regulates
ph is to about 1.Then at 60 DEG C, carry out stirring 4-5 h, obtain the transparent TiO with blue light
2colloidal sol.Get prepared TiO
2colloidal sol 50 mL is placed in beaker, backward its add SiO prepared by 20 mL
2colloidal sol, after stirring 1 h, the NaOH aqueous solution dripping 1M wherein, to PH=7, is in the isopropanol water solution of 50% by being re-dispersed into 200 mL volume fractions after gained colloidal sol rotary evaporation, obtains the optical catalyst sol of high stable.
Embodiment 3:
In 100 mL water, add the aqueous solution that a certain amount of titanyl sulfate is configured to 0.2-0.4M, and carry out stirring 1 h and obtain clear transparent solutions.Add the ammonia spirit of a certain amount of 0.1M subsequently, regulate
ph is about 7.After ageing a period of time, centrifugal, with the SO in abundant 3 the removing solution of deionized water
4 2-, take out filter cake, after adding some deionized waters, then add a certain amount of dilution heat of sulfuric acid, controlling its concentration is 10-20wt %, regulates
ph is to about 1.Then at 60 DEG C, carry out stirring 5-6 h, obtain the transparent TiO with blue light
2colloidal sol.Get prepared TiO
2colloidal sol 50 mL is placed in beaker, backward its add SiO prepared by 20 mL
2colloidal sol, after stirring 1 h, the NaOH aqueous solution dripping 1M wherein, to PH=7, is in the ethanol water of 40% by being re-dispersed into 200 mL volume fractions after gained colloidal sol rotary evaporation, obtains the optical catalyst sol of high stable.
Embodiment 4:TiO
2the photocatalytic activity evaluation of colloidal sol and the neutral colloidal sol of photocatalyst
Configure the rhodamine B aqueous solution of 10 mg/L, get the TiO of 10 mL synthesis respectively
2colloidal sol and photocatalyst neutral water colloidal sol, join in the rhodamine B solution that 50 mL configure, use ultraviolet light intensity to be 365 nm, 2mW/cm
2, at set intervals ultraviolet-visible absorption spectroscopy is carried out to solution and tests its absorbance.Be respectively TiO as shown in Figure 3
2spectrum over time during the neutral colloidal sol photocatalytic degradation rhodamine B of colloidal sol and photocatalyst.After 4-6 h irradiates, the speed of the neutral colloidal sol rhodamine B degradation of photocatalysis can reach 10 %, and independent TiO
2colloidal sol can reach 20 %, shows to add SiO
2the raising of photocatalytic activity is contributed to after colloidal sol.
Embodiment 5: the coating of optical catalyst sol on glass fiber reinforced cement sill surface and self-cleaning performance test
The preparation of glass fiber reinforced cement based composites (GRC) sample block: by cement 25kg(25%), sand 35kg(35%), glass chip 13kg(13%), PVA fiber 1kg(1%), PP fiber 1kg(1%), pigment powder 5kg(5%), polymer dispersion powder 5kg(5%), water reducer naphthalenesulfonate formaldehyde condensation compound 0.3kg(0.3%), early strength agent sulfate 0.3kg(0.3%), antifreezing agent calcium chloride 0.2kg(0.2%), inside mix the siliceous powder waterproofing agent 0.2kg(0.2% of formula), metakaolin 2kg(2%), stone flour 1kg(1%), water 11kg(11%) stir after make fibre reinforced cement architectural surface mortar.
By the fibre reinforced cement architectural surface mortar configured, adopt gunite to make fibre reinforced cement architectural surface in the mould of decorative effect, surface thickness is 3 cm, nature 10 minutes.By cement 25kg(25%), sand 46kg(46%), alkali-resistant glass fibre 3kg(3%), basalt fibre 2kg(2%), redispersable latex powder 5kg(5%), thickener hydroxypropyl methylcellulose 0.5kg(0.5%), metakaolin 3kg(2%), breeze 2kg(2%), water 12kg(12%) mixing, stir and make fibrous cementitious structural layer slurry.After fibrous cementitious structural layer slurry is configured, sprayed to be ejected into and had in the volume mould of fibre reinforced cement architectural surface, and adopted scraper plate to be struck off by slurry, then use pressure roller to carry out roll-in closely knit, make fibrous cementitious structural layer.
Alkali-resistant glass fibre felt is routed in mould, carries out roll extrusion with pressure roller, make it to be absorbed in fibrous cementitious structural layer.Maintenance 4 under above-mentioned fiber reinforced cement product normal temperature as a child, is carried out the demoulding.Obtained fiber reinforced cement product sample block is cut, obtains long 5cm, wide 3cm, the cement-like block of thick 1cm.
In order to prevent the water suction of cement material, first adopting drop-coating that polyacrylic acid is carried out film forming, natural air drying on GRC sample block, forming separation layer.Drop-coating is adopted on the GRC sample block scribbling separation layer, to apply the optical catalyst sol of synthesis, natural air drying.Drip the rhodamine B solution that configured of painting one being coated with in optical catalyst sol, and irradiate under being placed in ultraviolet etc., ultraviolet light intensity is 365 nm, 2mW/cm
2.In experiment, optical catalyst sol is better at the filming performance of GRC plate surface, and rhodamine B pigment can effectively at cement laminates surface spreading, after ultraviolet lighting degrades 24h, rhodamine B can be completely degraded, and Fig. 4 shows the degradation process of rhodamine B on GRC surface under UV-irradiation.
Embodiment 6: optical catalyst sol is in the coating of porous concrete product and self-cleaning performance test
The preparation of pervious concrete material sample block: adopt 42.5 grades of ordinary cements, grating is the unit level natural sand of 0.3-0.6 mm, naphthalene series high-efficiency water-reducing agent and water, by aggregate: cement: water: water reducer=3:1:0.3:0.03 preparation obtains surface layer pervious concrete, adopt 42.5 grades of ordinary cements again, grating is the unit level artificial sand of 1.48, naphthalene series high-efficiency water-reducing agent and water, by aggregate: cement: water: water reducer=4:1:0.3:0.04 configuration obtains bottom pervious concrete, obtaining compact dimensions through compacting is 50mm*100mm*200mm, surface thickness is the porous concrete product of 10mm.Use cutting machine it to be cut into long 5cm further, wide 3cm, the cement-like block of thick 1cm is for subsequent use.In order to prevent the water suction of cement material, first adopting drop-coating that polyacrylic acid is carried out film forming, natural air drying on pervious concrete sample block, forming separation layer.Drop-coating is adopted on the pervious concrete sample block scribbling separation layer, to apply the optical catalyst sol of synthesis, natural air drying.Drip the rhodamine B solution that configured of painting one being coated with in optical catalyst sol, and irradiate under being placed in ultraviolet etc., ultraviolet light intensity is 365 nm, 2mW/cm
2.In experiment, optical catalyst sol is better at the filming performance of plate surface, and rhodamine B pigment can effectively at cement laminates surface spreading, and after ultraviolet lighting degraded 24h, rhodamine B can be completely degraded.
Claims (3)
1., for a high-stability neutral photocatalyst sol preparation method for cement-based material, it is characterized in that, take following steps:
A, titanium salt are hydrolyzed:
Select inorganic titanium salt as raw material, add in alkaline aqueous solution and be hydrolyzed, make solution be adjusted to neutral pH=7, obtain white suspension;
B, sedimentation and filtration washing: by centrifugal three times of above-mentioned A gained white suspension, precipitation is repeatedly washed, until the electrical conductivity of cleaning solution is less than 50 μ S/cm;
C, acid adding dispergation: the dilute acid solution adding 0.1M in the precipitation of gained; 60
odispergation 4 h under C, obtains nattier blue transparent TiO
2acidic sol; Described acid is any one in nitric acid, hydrochloric acid or sulfuric acid;
D, SiO
2colloidal sol synthesizes: using ethyl orthosilicate as raw material, is 1:24 in ethanol according to ethyl orthosilicate and ethanol mol ratio, to be hydrolyzed acquisition SiO as catalyst by dripping acid
2colloidal sol; Described acid is any one in nitric acid, hydrochloric acid or sulfuric acid, and instillation acid is 1:0.15 with the mol ratio of ethyl orthosilicate;
E, the nattier blue transparent TiO obtained in C
2add in colloidal sol and can improve hydrophilic SiO
2colloidal sol, Keep agitation 0.5h ~ 4h, obtains mixed sols; Nattier blue transparent TiO
2colloidal sol and SiO
2colloidal sol mol ratio is 1:4;
The NaOH solution of the 0.1M configured is added in F, the mixed sols that obtains to E, regulate pH to neutral, by its rotary evaporation to containing the alcohol solution being again dispersed to volume fraction 30 % ~ 50% after a small amount of moisture content, obtain the high-stability neutral photocatalyst sol being used for cement-based material.
2. a kind of high-stability neutral photocatalyst sol preparation method for cement-based material according to claim 1, is characterized in that: the inorganic titanium salt described in above-mentioned steps A is any one in titanium sulfate, titanyl sulfate or titanium chloride.
3. a kind of high-stability neutral photocatalyst sol preparation method for cement-based material according to claim 1, is characterized in that: the alkaline aqueous solution added in above-mentioned steps A be ammoniacal liquor, NaOH any one.
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| CN104209145B (en) * | 2014-06-09 | 2017-01-25 | 深圳市天得一环境科技有限公司 | Nanometer spherical porous weak light photocatalyst for degrading formaldehyde, and preparation method and application thereof |
| CN104209146B (en) * | 2014-06-09 | 2017-01-25 | 深圳市天得一环境科技有限公司 | Nanometer spherical porous weak light photocatalyst for degrading nitrogen oxide, and preparation method and application thereof |
| CN105802367B (en) * | 2016-03-16 | 2018-03-16 | 湖北格林森绿色环保材料股份有限公司 | A kind of inorganic ecological ornamental plate of Composite Coatings membranous type automatically cleaning and preparation method thereof |
| CN106431112A (en) * | 2016-09-21 | 2017-02-22 | 南京倍立达新材料系统工程股份有限公司 | Photocatalysis modified fiber composite dry-mixed mortar |
| CN111559923A (en) * | 2020-05-09 | 2020-08-21 | 东南大学 | Preparation method of cement-based material with photocatalytic performance |
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| CN1546226A (en) * | 2003-12-17 | 2004-11-17 | 同济大学 | TiO2/SiO2 aerogel and method for making same |
| CN1597810A (en) * | 2003-09-18 | 2005-03-23 | 中国科学院理化技术研究所 | Antifogging sterilization multifunctional coating and its preparation process and use |
| CN101024169A (en) * | 2007-03-26 | 2007-08-29 | 云南大学 | Method for preparing mesoporous crystal titanium dioxide using light-sensitive active matter as formboard |
| CN101306359A (en) * | 2008-07-01 | 2008-11-19 | 中国人民解放军第二炮兵工程学院 | Composite aerogel photocatalyst for recovering titanium dioxide/silicon dioxide |
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| KR101104262B1 (en) * | 2008-12-31 | 2012-01-11 | 주식회사 노루홀딩스 | Article wih self-cleaning effect and method of preparation thereof |
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| CN1597810A (en) * | 2003-09-18 | 2005-03-23 | 中国科学院理化技术研究所 | Antifogging sterilization multifunctional coating and its preparation process and use |
| CN1546226A (en) * | 2003-12-17 | 2004-11-17 | 同济大学 | TiO2/SiO2 aerogel and method for making same |
| CN101024169A (en) * | 2007-03-26 | 2007-08-29 | 云南大学 | Method for preparing mesoporous crystal titanium dioxide using light-sensitive active matter as formboard |
| CN101306359A (en) * | 2008-07-01 | 2008-11-19 | 中国人民解放军第二炮兵工程学院 | Composite aerogel photocatalyst for recovering titanium dioxide/silicon dioxide |
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