CN103691414A - 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 the neutral optical catalyst sol preparation method of a kind of high stable for cement-based material.
Background technology
Cement is as one of the most widely used material in Inorganic Non-metallic Materials, in common base field, is able to large-scale application on as building and road.In recent years, the pollution of building can damage the images such as company, hotel, bank and restaurant of moving in, and therefore in exterior wall maintenance attractive in appearance, needs expensive fund.The exterior pollution of building the most obvious heavy pollutant stands in the breach and for pollutant, adheres to the dirt of generation, and carbon and the oil content of pollutant sources in the waste gas of motor vehicle emission is that main so-called urban type pollutes.
Photocatalyst is mainly with nanoscale TiO
2the semi-conducting material general name with photo-catalysis function for representative.When photocatalyst is applied to substrate surface, utilize photocatalysis and the photic super hydrophilicity of photocatalyst, can be by the organic matter degradation in attract dirt, inorganic matter 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 purifying air, and realizes without the function of manually knowing some building pollutions.
TiO
2the wet chemical methods of film is owing to having advantage on cost, and is easy to realize, and obtained research comparatively widely.Wet chemical methods mainly comprises liquid phase deposition and sol-gel processing.Liquid phase deposition only need to soak place's substrate in corresponding reactant liquor, after certain hour reaction, can on substrate, deposit the TiO that obtains crystallization
2film, however the shortcoming of this method is to be not suitable for preparing TiO in large area
2film.It is low that sol-gel processing has preparation temperature, and technique is simple, can prepare the film that multicomponent mixes, and the advantage such as film particles degree is even, purity height, thereby become preparation TiO
2the common methods of film.
But sol-gel processing needs later stage high-temperature process to make TiO conventionally
2complete crystallization, but high-temperature process may cause base material element to TiO
2film diffusion inside, and easily cause TiO
2grain growth, cause photo-quantum efficiency and photocatalytic activity to reduce, so this process has seriously limited its application at the substrate surface of poor heat resistance.
For this reason, the previously prepared TiO that is dispersed with
2nanocrystalline solution, utilizes it to film afterwards at normal temperatures, realizes and just makes and have crystalline TiO without high-temperature process
2film becomes the emphasis of people's research.Up to now, the common method of 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 is mainly to utilize inorganic titanium salt with alkali reaction, to obtain in advance Ti (OH) as predecessor
4precipitation, and then add acid to obtain TiO as degumming agent
2.As adopting titanium tetrachloride, titanyl sulfate and metatitanic acid have been 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 because the general acid resistance of cement-based material is poor, adopt the acid optical catalyst sol of this acquisition to damage base material.Therefore, need to first synthesize the efficiency light catalyst that neutral crystal property is good and then apply 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 is to introduce H
2o
2as complexing agent to Ti (OH)
4precipitation is carried 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 in dispergation process, to add the modifier of high score subclass, 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 has also introduced the neutral mixed crystal TiO of high stable
2nanocrystalline preparation method, but about the application at cement-based material, do not introduce.Glass fiber cement sill (GRC) is with a wide range of applications in as building roof, building curtain wall, wall decoration, municipal traffic engineering construction in public building field, early stage, my company reported Nano self-cleaning fiber reinforced cement product and production method thereof at Chinese patent CN102518275, but the detailed preparation of producing about photocatalyst there is no introduction.
Summary of the invention
The object of the invention is provides a kind of high stable for cement-based material neutral optical catalyst sol preparation method for above-mentioned weak point, is a kind of synthetic neutral optical catalyst sol preparation method of high stable who is applicable to cement-based material application, this TiO
2preparation method be convenient to industrialization, greatly improved nano-TiO
2application power on cement-based material surface.
A kind of high stable for cement-based material of the present invention is neutral optical catalyst sol preparation method realize by the following technical programs:
The neutral optical catalyst sol preparation method of a kind of high stable for cement-based material takes following steps:
A, titanium salt hydrolysis: 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, and the alkaline aqueous solution adding is any one of ammoniacal liquor, NaOH;
B, sedimentation and filtration washing: by centrifugal three times of above-mentioned A gained white suspension, to repeatedly washing of precipitation, until the electrical conductivity of cleaning solution is less than 50 μ S/cm;
C, acid adding dispergation: to the dilute acid solution that adds 0.1M in the precipitation of gained; 60
odispergation 4 h under C, obtain nattier blue transparent TiO
2acidic sol; Described acid is any in nitric acid, hydrochloric acid or sulfuric acid.
D, SiO
2colloidal sol is synthetic: using ethyl orthosilicate as raw material, be 1:24 according to ethyl orthosilicate and ethanol mole proportioning in ethanol, by dripping acid, as catalyst, is hydrolyzed and obtains SiO
2colloidal sol; Described acid is any in nitric acid, hydrochloric acid or sulfuric acid, and splashing into acid is 1:0.15 with mole proportioning of ethyl orthosilicate.
E, to adding in the nattier blue vitreosol obtaining in C, can improve hydrophilic SiO
2colloidal sol, continues to stir 0.5h～4h, obtains mixed sols; Nattier blue transparent TiO
2colloidal sol and SiO
2colloidal sol mole proportioning is 1:4.
F, to the NaOH solution that adds the 0.1M configuring in the resulting mixed sols of D, regulate
ph is to neutral, and its rotary evaporation, to containing the alcohol solution that is again dispersed to volume fraction 30 %～50% after a small amount of moisture content, is obtained to the neutral optical catalyst sol of high stable for cement-based material.
Because cement-based material is to nano-TiO
2colloidal sol
ph value has restriction, too low
ph value can be damaged 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 approaches 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 using in preparation process of the present invention is extensive, low price, and technique is simple, convenient operation, thereby be easy to carry out large-scale production.
2, the titania/silica hydrosol photocatalyst activity component TiO that prepared by the present invention
2colloidal sol be several nanometers, even particle distribution, stability is fine, can not assemble and form flocculent deposit after long storage time in the time of can not precipitating and dilute.
3, this nano-sized hydrosol is neutral, can be widely used in cement-based material field, almost negligible to cement-based material damage.
4, in the prepared hydrosol, contain inorganic binder, strengthened the adhesion on cement matrix surface.
When 5, the nano-sized hydrosol of preparation is coated on cement-based material surface, obtained good photocatalytic self-cleaning 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 the neutral optical catalyst sol XRD figure of powder after drying.
Fig. 2 is for forming the SEM photo of complex sol.
Fig. 3 is for forming the EDS figure of complex sol.
Fig. 4 is TiO
2spectrum over time during the neutral colloidal sol photocatalytic degradation of colloidal sol and photocatalyst rhodamine B.
Fig. 5 is that GRC cement matrix surface applies after the neutral colloidal sol of photocatalyst the rhodamine B change procedure of degrading in time.
The specific embodiment
Below with reference to embodiment, the invention will be further described:
(1) TiO
2synthesizing of acidic sol
In 100 mL water, add titanium sulfate to be configured as the aqueous solution of 0.2 M, and stir 1 h and obtain clear solution.The ammonia spirit that adds subsequently a certain amount of 0.1M, regulates
ph is about 7, after ageing a period of time, centrifugal, with the abundant sulfate (needing to remove because sulfate ion can cause precipitation) of removing for 3 times in solution of deionized water, take out filter cake, add after some deionized waters, add again a certain amount of dilute nitric acid solution, control its concentration for (10-20) wt %, regulate
ph is to 1 left and right.Then 60
ounder C, stir 4-6 h, obtain the transparent TiO with blue light
2colloidal sol.
(2) SiO
2synthesizing of colloidal sol
In cold bath, get in the ethanol that 2-4mL ethyl orthosilicate joins 40-50mL and stir 10 min, make it fully be mixed into homogeneous phase solution, add afterwards 1-3mL water, and splash into 0.3 mLHNO
3, after dropwising, reactant mixture is warming up to 70 ℃ and stirring and refluxing 2-3h, obtain SiO after cooling
2colloidal sol.
(3) photocatalyst TiO
2/ SiO
2the preparation of complex sol:
Get prepared TiO
2colloidal sol 40-60mL is placed in beaker, adds the prepared SiO of 10-30mL afterwards to it
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 be re-dispersed in the methanol aqueous solution that 500 mL volume fractions are 30%, obtain required TiO
2/ SiO
2complex sol.Fig. 1 is TiO
2colloidal sol and same SiO
2be compounded to form neutral optical catalyst sol the XRD figure of powder, the as can be seen from the figure TiO of preparation after drying
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 synthetic SiO
2for amorphous state, so still only there is TiO in optical catalyst sol
2diffraction maximum, and kept good crystallinity.Fig. 2 is for obtaining the stereoscan photograph of complex sol, and the nano particle diameter as can be seen from the figure obtaining is less, is about 10-20nm left and right.And in EDS spectrogram, show in colloidal sol and contain Na, O, Si and Ti signal, illustrate in colloidal sol except including SiO
2and TiO
2outside, also have Na
2oSiO
2, this is conducive to colloidal sol in the coating on cement matrix surface.
Embodiment 2:
In 100 mL water, add a certain amount of titanium tetrachloride to be configured to the aqueous solution of 0.2-0.5M, and stir 1 h and obtain clear solution.The ammonia spirit that adds subsequently a certain amount of 0.1M, regulates
ph is about 7.After ageing a period of time, centrifugal, with the abundant Cl removing in solution for 3 times of deionized water
-, take out filter cake, add after some deionized waters, then add a certain amount of dilute hydrochloric acid solution, controlling its concentration is 30-40wt %, regulates
ph is to 1 left and right.Then at 60 ℃, stir 4-5 h, obtain the transparent TiO with blue light
2colloidal sol.Get prepared TiO
2 colloidal sol 50 mL are placed in beaker, add the prepared SiO of 20 mL afterwards to it
2colloidal sol, after stirring 1 h, drips the NaOH aqueous solution of 1M wherein to PH=7, will after gained colloidal sol rotary evaporation, be re-dispersed in the isopropanol water solution that 200 mL volume fractions are 50%, obtains the optical catalyst sol of high stable.
Embodiment 3:
In 100 mL water, add a certain amount of titanyl sulfate to be configured to the aqueous solution of 0.2-0.4M, and stir 1 h and obtain clear solution.The ammonia spirit that adds subsequently a certain amount of 0.1M, regulates
ph is about 7.After ageing a period of time, centrifugal, with the abundant SO removing in solution for 3 times of deionized water
4 2-, take out filter cake, add after some deionized waters, then add a certain amount of dilution heat of sulfuric acid, controlling its concentration is 10-20wt %, regulates
ph is to 1 left and right.Then at 60 ℃, stir 5-6 h, obtain the transparent TiO with blue light
2colloidal sol.Get prepared TiO
2 colloidal sol 50 mL are placed in beaker, add the prepared SiO of 20 mL afterwards to it
2colloidal sol, after stirring 1 h, drips the NaOH aqueous solution of 1M wherein to PH=7, will after gained colloidal sol rotary evaporation, be re-dispersed in the ethanol water that 200 mL volume fractions are 40%, obtains the optical catalyst sol of high stable.
Embodiment 4:TiO
2the photocatalytic activity evaluation of the neutral colloidal sol of colloidal sol and photocatalyst
Configure the rhodamine B aqueous solution of 10 mg/L, get respectively the synthetic TiO of 10 mL
2colloidal sol and photocatalyst neutral water colloidal sol, join in the rhodamine B solution that 50 mL configure, and using ultraviolet light intensity is 365 nm, 2mW/cm
2, at set intervals solution is carried out to ultraviolet-visible absorption spectroscopy and tests its absorbance.Be respectively as shown in Figure 3 TiO
2spectrum over time during the neutral colloidal sol photocatalytic degradation of colloidal sol and photocatalyst rhodamine B.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
2after colloidal sol, contribute to the raising of photocatalytic activity.
Embodiment 5: optical catalyst sol is in coating and the self-cleaning performance test on glass fiber reinforced cement sill surface
The preparation of glass fiber reinforced cement based composites (GRC) sample piece: 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%) make fibre reinforced cement architectural surface mortar after stirring.
By the fibre reinforced cement architectural surface mortar configuring, adopt gunite in the mould with decorative effect, to make fibre reinforced cement architectural surface, 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%) mix, stir and make fibre reinforced cement structure sheaf slurry.After fibre reinforced cement structure sheaf slurry is configured, sprayed and be ejected in the volume mould with fibre reinforced cement architectural surface, and adopted scraper plate that slurry is struck off, and then used pressure roller to carry out roll-in closely knit, made fibre reinforced cement structure sheaf.
Alkali-resistant glass fibre felt is routed in mould, with pressure roller, carries out roll extrusion, make it to be absorbed in fibre reinforced cement structure sheaf.Maintenance 4 under above-mentioned fiber reinforced cement product normal temperature as a child, is carried out to the demoulding.Resulting fiber reinforced cement product sample piece is cut, obtain long 5cm, wide 3cm, the cement-like piece of thick 1cm.
In order to prevent the water suction of cement material, first adopt drop-coating that polyacrylic acid is carried out to film forming on GRC sample piece, natural air drying, forms separation layer.Adopt drop-coating to apply synthetic optical catalyst sol, natural air drying scribbling on the GRC sample piece of separation layer.In being coated with optical catalyst sol, drip to be coated with the rhodamine B solution having configured, and to be placed under ultraviolet etc. and to irradiate, 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 be effectively at cement flaggy surface spreading, after ultraviolet lighting degraded 24h, rhodamine B can be completely degraded, and Fig. 4 has shown under UV-irradiation that rhodamine B is in the degradation process on GRC surface.
Embodiment 6: optical catalyst sol is in coating and the self-cleaning performance test of porous concrete product
The preparation of pervious concrete material sample piece: 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 again 42.5 grades of ordinary cements, grating is 1.48 unit level artificial sand, 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, through compacting, obtaining compact dimensions is 50mm*100mm*200mm, surface thickness is the porous concrete product of 10mm.Use cutting machine that it is further cut into long 5cm, wide 3cm, the cement-like piece of thick 1cm is standby.In order to prevent the water suction of cement material, first adopt drop-coating that polyacrylic acid is carried out to film forming on pervious concrete sample piece, natural air drying, forms separation layer.Adopt drop-coating to apply synthetic optical catalyst sol, natural air drying scribbling on the pervious concrete sample piece of separation layer.In being coated with optical catalyst sol, drip to be coated with the rhodamine B solution having configured, and to be placed under ultraviolet etc. and to irradiate, 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 be effectively at cement flaggy surface spreading, and after ultraviolet lighting degraded 24h, rhodamine B can be completely degraded.
Claims (3)
1. for the neutral optical catalyst sol preparation method of high stable of cement-based material, it is characterized in that, take following steps:
A, titanium salt hydrolysis:
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, to repeatedly washing of precipitation, until the electrical conductivity of cleaning solution is less than 50 μ S/cm;
C, acid adding dispergation: to the dilute acid solution that adds 0.1M in the precipitation of gained; 60
odispergation 4 h under C, obtain nattier blue transparent TiO
2acidic sol; Described acid is any in nitric acid, hydrochloric acid or sulfuric acid;
D, SiO
2colloidal sol is synthetic: using ethyl orthosilicate as raw material, be 1:24 according to ethyl orthosilicate and ethanol mole proportioning in ethanol, by dripping acid, as catalyst, is hydrolyzed and obtains SiO
2colloidal sol; Described acid is any in nitric acid, hydrochloric acid or sulfuric acid, and splashing into acid is 1:0.15 with mole proportioning of ethyl orthosilicate;
E, to the nattier blue transparent TiO obtaining in C
2in colloidal sol, add and can improve hydrophilic SiO
2colloidal sol, continues to stir 0.5h～4h, obtains mixed sols; Nattier blue transparent TiO
2colloidal sol and SiO
2colloidal sol mole proportioning is 1:4;
F, to the NaOH solution that adds the 0.1M configuring in the resulting mixed sols of D, regulate
ph is to neutral, and its rotary evaporation, to containing the alcohol solution that is again dispersed to volume fraction 30 %～50% after a small amount of moisture content, is obtained to the neutral optical catalyst sol of high stable for cement-based material.
2. the neutral optical catalyst sol preparation method of a kind of high stable 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. the neutral optical catalyst sol preparation method of a kind of high stable for cement-based material according to claim 1, is characterized in that: the alkaline aqueous solution adding in above-mentioned steps A is any one of ammoniacal liquor, NaOH.
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| CN104209145A (en) * | 2014-06-09 | 2014-12-17 | 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 |
| CN104209146A (en) * | 2014-06-09 | 2014-12-17 | 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 |
| CN105802367A (en) * | 2016-03-16 | 2016-07-27 | 湖北格林森新型建材科技有限公司 | Composite film-coated self-cleaning inorganic ecological decorative plate 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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| CN104209145A (en) * | 2014-06-09 | 2014-12-17 | 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 |
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| CN105802367A (en) * | 2016-03-16 | 2016-07-27 | 湖北格林森新型建材科技有限公司 | Composite film-coated self-cleaning inorganic ecological decorative plate and preparation method 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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