CN103641512B - In the method for building material surface dispersion nanometer anatase titania - Google Patents
In the method for building material surface dispersion nanometer anatase titania Download PDFInfo
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- CN103641512B CN103641512B CN201310692627.3A CN201310692627A CN103641512B CN 103641512 B CN103641512 B CN 103641512B CN 201310692627 A CN201310692627 A CN 201310692627A CN 103641512 B CN103641512 B CN 103641512B
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Abstract
The invention provides a kind of method at building material surface dispersion nanometer anatase titania, comprising: by tetrabutyl titanate and Virahol mixing, obtain the tetrabutyl titanate aqueous isopropanol that mass concentration is 4-6%; Obtain the PVP aqueous solution that mass concentration is 2%; Under whipped state, described tetrabutyl titanate aqueous isopropanol is added the described PVP aqueous solution, simultaneously control PH≤2, make tetrabutyl titanate hydrolysis obtain nanometer anatase titania colloidal sol; By the klining at the temperature of 400-550 DEG C after material surface of described nanometer anatase titania colloidal dispersion.The making method of nanometer anatase titania can improve the bonding force of nanometer anatase titania and material.
Description
Technical field
The invention belongs to environment-friendly materials field, relate to a kind of method at building material surface dispersion nanometer anatase titania.
Background technology
There is the performances such as photocatalysis Decomposition organic compound, antibacterial and Superhydrophilic in nanometer anatase titania, is a kind of available environment-friendly materials.Research finds that nanometer anatase titania photocatalyst is under near-ultraviolet light (such as sunlight or luminescent lamp etc.) irradiates, and the electronics in molecule is excited, and generates electron-hole pair.Wherein, the hole of positively charged has very strong oxidation capacity, and the water molecules in air can be made to generate the strong oxidizer of hydroxyl free radical (OH); Electronegative electronic energy makes the oxygen (O in air
2) reduction, generate another kind of strong living radical O
2-.OH and O
2-the energy that energy equivalence contained by living radical produces in the heat energy of 3600K high temperature, is enough to most of organic substance " burning " is decomposed.Its organic molecule such as energy Decomposition of benzene, formaldehyde etc., anti-bacteria, and to human body fanout free region.
On the other hand, the stable performance of nanometer anatase titania, under lower than 600 DEG C and non-strong alkali environment, it undergoes no deterioration and loses photocatalysis performance, and namely in usual environment, it is all stable have the value generally used.If nanometer anatase titania to be formed at the surface of sheet material (as ceramic tile, stone material and glass), its photocatalysis characteristic under the exciting of light, the organic pollutant in environment and kill touched bacterium of can degrading.
If cover dispersion nanometer anatase titania nanometer anatase titania powder at building material surface, then because the particle diameter of nanometer anatase titania powder comparatively greatly, can affect the performances such as photocatalysis Decomposition organic compound, antibacterial and Superhydrophilic.Because nanometer anatase titania particle diameter is comparatively large and between sheet material in conjunction with poor and to no effect.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of method at building material surface dispersion nanometer anatase titania, it can improve the bonding force of nanometer anatase titania and material, and the performance such as photocatalysis Decomposition organic compound, antibacterial and Superhydrophilic.
The technical scheme adopted solved the problems of the technologies described above is to provide a kind of method at building material surface dispersion nanometer anatase titania, comprising:
By tetrabutyl titanate and Virahol mixing, obtain the tetrabutyl titanate aqueous isopropanol that weight concentration is 4 ~ 6%;
Obtain the PVP aqueous solution that weight concentration is 2%;
Described tetrabutyl titanate aqueous isopropanol is added the described PVP aqueous solution when stirring, simultaneously will control PH≤2, make described tetrabutyl titanate hydrolysis acquisition nanometer anatase titania colloidal sol;
By the klining at the temperature of 400-500 DEG C after material surface of described nanometer anatase titania colloidal dispersion.
Wherein, by spraying method by described nanometer anatase titania colloidal dispersion in material surface; Or, in described nanometer anatase titania colloidal sol, add Vltra tears, then by typography by described nanometer anatase titania colloidal dispersion in material surface.
Wherein, nitric acid or hydrochloric acid control PH≤2 are utilized.
Wherein, by described nanometer anatase titania colloidal dispersion after material surface at the temperature of 400-550 DEG C klining 15-25 minute.
Wherein, be cooled to room temperature after being processed at the temperature of 400-500 DEG C by described material, then obtain described nanometer anatase titania colloidal sol at material surface.
Wherein, described material is ceramic tile, stone material or glass.
Wherein, in electrical kiln or gas-combustion kiln, klining Dispersion on surface has the described material of described nanometer anatase titania colloidal sol.
The present invention has following beneficial effect:
First tetrabutyl titanate and Virahol mixing are obtained tetrabutyl titanate aqueous isopropanol by a kind of method at building material surface dispersion nanometer anatase titania provided by the invention; Then, when stirring by tetrabutyl titanate aqueous isopropanol and PVP aqueous solution, obtaining nanometer anatase titania colloidal sol, there is the nano titanium oxide that hydrolysis produces particle diameter about 10nm in tetrabutyl titanate; By nanometer anatase titania colloidal dispersion after material surface, and klining at the temperature of 400-500 DEG C, remove other compound in colloidal sol and only retain nanometer anatase titania, thus be the nanometer anatase titania of about 10nm at material surface formation particle diameter, make the bonding force of nanometer anatase titania and material strong, and the performance such as photocatalysis Decomposition organic compound, antibacterial and Superhydrophilic.
Accompanying drawing explanation
Fig. 1 is the method flow diagram that the present invention makes containing nanometer anatase titania colloidal sol;
Fig. 2 makes according to the present embodiment the XRD figure containing nanometer anatase titania sample obtained;
Fig. 3 is the graphic representation of the decomposed sample benzene containing nanometer anatase titania.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the making method at building material surface making nanometer anatase titania provided by the invention is described in detail.
As shown in Figure 1, the method at building material surface making nanometer anatase titania provided by the invention comprises the following steps:
Step S1, by tetrabutyl titanate and Virahol mixing, obtain tetrabutyl titanate aqueous isopropanol, in this tetrabutyl titanate aqueous isopropanol, the mass concentration of tetrabutyl titanate is 4-6%.
Tetrabutyl titanate and Virahol all adopt technical pure tetrabutyl titanate and Virahol, and tetrabutyl titanate and Virahol mixing are obtained tetrabutyl titanate aqueous isopropanol.In this tetrabutyl titanate aqueous isopropanol, the concentration of tetrabutyl titanate is 4-6%.
Step S2, obtains the PVP aqueous solution that mass concentration is 1-2%.
In step s 2, polyvinylpyrrolidone (Polycinylpyrrolidone the is called for short PVP) aqueous solution is mixed with pure water by technical pure polyvinylpyrrolidone, obtains the PVP aqueous solution that concentration is 2%.
Step S3, under the high-speed stirring of 2500 ~ 3000r/min, adds the described PVP aqueous solution by described tetrabutyl titanate aqueous isopropanol, and control PH≤2, obtain nanometer anatase titania colloidal sol to make described tetrabutyl titanate hydrolysis.
Under whipped state, the tetrabutyl titanate aqueous isopropanol that step S1 obtains slowly is added in the PVP aqueous solution that step S2 obtains, simultaneously will control PH≤2, make tetrabutyl titanate hydrolysis, acquisition nanometer anatase titania colloidal sol.Utilize nitric acid or salt solution to regulate pH value.
Step S4, by described nanometer anatase titania colloidal dispersion after material surface at the temperature of 400-550 DEG C klining 10-20 minute.
In step s 4 which, by spraying coating process by nanometer anatase titania colloidal dispersion in material surface.Here material can adopt ceramic tile, stone material or glass.Then, material is placed on klining at the temperature of 400-550 DEG C.During klining, klining can be carried out in electrical kiln or gas-combustion kiln.The klining time is 15-25 minute.
In step s 4 which, Vltra tears can also be added in nanometer anatase titania colloidal sol, then by typography by nanometer anatase titania colloidal dispersion in material surface.Vltra tears adopts technical pure Vltra tears.
There is the pollutents such as greasy dirt, the bonding force of these pollutant effect materials and nanometer anatase titania in the material surface before dispersion nanometer anatase titania colloidal sol.Therefore, in preferably implementing at one, before implementation step S4, the making method of nanometer anatase titania also comprises: step S31 is cooled to room temperature (25-30 DEG C) after material is processed 10-20 minute at the temperature of 400-500 DEG C, then obtains nanometer anatase titania colloidal sol on its surface.Removed dust and the greasy dirt of material surface by pyroprocessing, thus improve the bonding force of material and nanometer anatase titania.Material can process in electrical kiln or gas-combustion kiln.
Be the nanometer anatase titania of about 15nm by the above-mentioned nanometer anatase titania major part granularity obtained in the method for building material surface dispersion nanometer anatase titania, only have a small amount of particle diameter to be the nanometer anatase titania of 20-30nm.But the nanometer anatase titania that particle diameter is larger is removed in klining process, thus acquisition granularity is the nanometer anatase titania of about 15nm.Produce the effect of similar intermolecular attraction between the nanometer anatase titania of this granularity and material and mortise, obtain stronger bonding force.
Embodiment one
By tetrabutyl titanate and Virahol mixing, obtain tetrabutyl titanate aqueous isopropanol.In tetrabutyl titanate aqueous isopropanol, the mass concentration of tetrabutyl titanate is 4%.Obtain the PVP aqueous solution that weight concentration is 2%.Under whipped state, tetrabutyl titanate aqueous isopropanol is added the PVP aqueous solution, simultaneously control PH≤2, make tetrabutyl titanate hydrolysis obtain nanometer anatase titania colloidal sol.By ceramic tile at the temperature of 400 DEG C klining 10 minutes to remove dust and the greasy dirt of ceramic tile surface, then by spraying coating process by nanometer anatase titania colloidal dispersion in material surface, klining 15 minutes at the temperature of 400 DEG C again, other compounds in nanometer anatase titania colloidal sol are removed and retains nanometer anatase titania, thus nanometer anatase titania is scattered in the surface of ceramic tile.
Embodiment two
By tetrabutyl titanate and Virahol mixing, obtain tetrabutyl titanate aqueous isopropanol.In tetrabutyl titanate aqueous isopropanol, the mass concentration of tetrabutyl titanate is 5%.Obtain the PVP aqueous solution that weight concentration is 2%.Under whipped state, tetrabutyl titanate aqueous isopropanol is added the PVP aqueous solution, control pH value is 1.8 simultaneously, makes tetrabutyl titanate hydrolysis obtain nanometer anatase titania colloidal sol; Then in nanometer anatase titania colloidal sol, Vltra tears is added.By ceramic tile at the temperature of 450 DEG C klining 15 minutes to remove dust and the greasy dirt of ceramic tile surface, then by screen-printing machine by nanometer anatase titania colloidal dispersion in material surface, then klining 20 minutes at the temperature of 450 DEG C.
Embodiment three
By tetrabutyl titanate and Virahol mixing, obtain tetrabutyl titanate aqueous isopropanol.In tetrabutyl titanate aqueous isopropanol, the mass concentration of tetrabutyl titanate is 6%.Obtain the PVP aqueous solution that mass concentration is 2%.Under whipped state, tetrabutyl titanate aqueous isopropanol is added the PVP aqueous solution, control pH value is 1.5 simultaneously, makes tetrabutyl titanate hydrolysis obtain nanometer anatase titania colloidal sol.Ceramic tile klining at the temperature of 500 DEG C is removed dust and the greasy dirt of ceramic tile surface for 20 minutes, then by spraying coating process by nanometer anatase titania colloidal dispersion in material surface, then klining 25 minutes at the temperature of 550 DEG C, other compounds in nanometer anatase titania colloidal sol are removed and retains nanometer anatase titania, thus nanometer anatase titania is scattered in the surface of ceramic tile.
XRD, photocatalysis Decomposition organism benzene, antibacterial (evaluation of reference GB GB-T23763-2009 photocatalysis antibacterial material and goods anti-microbial property) and wetting ability (with reference to GB GB-T23764-2009 photocatalytic self-cleaning material performance test method) four inspections are carried out to the ceramic tile that above-described embodiment obtains.
Wherein, whether XRD is the nano titanium oxide in order to prove ceramic tile surface is anatase titanium dioxide (just only having anatase crystal type to have photocatalysis performance).Detection method is that the nanometer anatase titania colloidal sol configured directly is fired the nano titanium dioxide powder obtained, the condition firing nano titanium dioxide powder is identical with the method that ceramic tile surface obtains nanometer anatase titania, therefore, the crystal formation detecting nano titanium dioxide powder is identical with detection ceramic tile surface nanometer anatase titania.Fig. 2 is the XRD figure of the nanometer anatase titania obtained according to the making method of the present embodiment nanometer anatase titania.In fig. 2, transverse axis represents angle (degree), and the longitudinal axis represents diffracted intensity (Cps).As can be seen from Figure 2, the titanium dioxide obtained by aforesaid method is nanometer anatase titania.
There is conjugated structure in organism benzene, Decomposition of benzene needs larger energy.The hydroxyl free radical that nanometer anatase titania absorption luminous energy produces and benzene molecular react, and therefore use organism benzene as the organic ability of inspection photocatalysis Decomposition.The inspection of photocatalysis Decomposition organism benzene is size ceramic tile being cut into 200 × 200mm, is placed in the closed reactor being of a size of 220 × 220 × 30mm, reactor is placed in the thermostat of 100 DEG C ± 1 DEG C, balances and starts irradiation after 14 hours.The wavelength of light is 385nm, light intensity 0.15mW/cm
2.Illumination starts after 1 hour to sample (C
0), afterwards every one hour sampling once (C
t), get three parallel sample at every turn, and by the concentration of benzene in GC-9800 spectrograph analysis reactor.Light-catalyzed reaction is that ceramic tile surface nanometer anatase titania particle interface carries out, and when reaction conditions is fixed, in reactor, organic molecule is that the important factor of carrying out is reacted in impact to ceramic tile surface velocity of diffusion.When benzene molecular start cracking will produce cracking after small molecules, small molecules and benzene molecular exist simultaneously.At this moment be the gas of a mixing in reactor, because benzene molecular quality is relatively large, so and nmTi0
2interracial contact probability reduces, and benzene decomposition rate also must be slow by easing up.Therefore, this inspection can only illustrate that the experiment sheet material of coating nanometer anatase titania has the function of decomposing organic matter, and the speed of decomposing organic matter can not be described.Utilize blank sample to contrast, to obtain the ability of nanometer anatase titania decomposing organic matter exactly simultaneously.Fig. 3 is the graphic representation of nanometer anatase titania decomposing organic matter benzene.In figure, transverse axis represents light application time (hour), and the longitudinal axis represents the relative concentration of organism benzene gas, the curve that "-■-" is blank sample, "-zero-" have the curve of nanometer anatase titania sample for Dispersion on surface.
Superhydrophilic inspection requires by contact angle measurement (JC200C1) measure sample surface water contact angle with reference to GB GB-T23764-2009 photocatalytic self-cleaning material performance test method.Detecting instrument adopts contact angle measurement PowerReachJC2000C1.Checking procedure: get the ceramic tile polylith that size is the coating nanometer anatase titania of 50 × 50 × 8mm, be positioned over wavelength 385nm respectively, light intensity 0.15mW/cm
2illumination 90,180,270 minutes under condition.Then ceramic tile surface water droplet contact angle is measured with contact angle measurement.
Antibacterial inspection requires inspection with reference to the evaluation of GB GB-T23763-2009 photocatalysis antibacterial material and goods anti-microbial property.
Tetrabutyl titanate and Virahol mixing are obtained tetrabutyl titanate aqueous isopropanol by the making method of the nanometer anatase titania that the present embodiment provides; Then, when stirring by tetrabutyl titanate aqueous isopropanol and PVP aqueous solution, obtaining nanometer anatase titania colloidal sol, there is the nano titanium oxide that hydrolysis produces particle diameter about 10nm in tetrabutyl titanate; By nanometer anatase titania colloidal dispersion after material surface, and klining at the temperature of 400-500 DEG C, remove other compound in colloidal sol and only retain nanometer anatase titania, thus be the nanometer anatase titania of about 10nm at material surface formation particle diameter, the bonding force of this nanometer anatase titania and material is strong.Adopt the 7th part in standard GB/T/T3810.7-2006 " ceramic tile test method ": after the mensuration of glazed tile surface abrasion resistance carries out scrubbing experiment, nanometer anatase titania still intactly can be retained in the surface of material.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (7)
1., in a method for building material surface dispersion nanometer anatase titania, it is characterized in that, comprising:
Step S1, by tetrabutyl titanate and Virahol mixing, obtains the tetrabutyl titanate aqueous isopropanol that weight concentration is 4-6%;
Step S2, obtains the PVP aqueous solution that weight concentration is 2%;
Step S3, adds the described PVP aqueous solution by described tetrabutyl titanate aqueous isopropanol when stirring, simultaneously will control pH≤2, makes described tetrabutyl titanate hydrolysis acquisition nanometer anatase titania colloidal sol;
Step S4, by the klining at the temperature of 400-500 DEG C after material surface of described nanometer anatase titania colloidal dispersion.
2. according to claim 1 building material surface dispersion nanometer anatase titania method, it is characterized in that, in step s 4 which, by spraying method by described nanometer anatase titania colloidal dispersion in material surface; Or, in described nanometer anatase titania colloidal sol, add Vltra tears, then by typography by described nanometer anatase titania colloidal dispersion in material surface.
3. the method at building material surface dispersion nanometer anatase titania according to claim 1, is characterized in that, in step s3, utilize nitric acid or hydrochloric acid control pH≤2.
4. the method at building material surface dispersion nanometer anatase titania according to claim 1, it is characterized in that, in step s 4 which, by described nanometer anatase titania colloidal dispersion after material surface at the temperature of 400-500 DEG C klining 15-25 minute.
5. the method at building material surface dispersion nanometer anatase titania according to claim 1, it is characterized in that, in step s 4 which, be cooled to room temperature after being processed at the temperature of 400-500 DEG C by described material, then obtain described nanometer anatase titania colloidal sol at material surface.
6., according to the arbitrary described method at building material surface dispersion nanometer anatase titania of claim 1-5, it is characterized in that, described material is ceramic tile, stone material or glass.
7. the method at building material surface dispersion nanometer anatase titania according to claim 1, it is characterized in that, in step s 4 which, in electrical kiln or gas-combustion kiln, klining Dispersion on surface has the described material of described nanometer anatase titania colloidal sol.
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| RU2190583C2 (en) * | 1997-12-15 | 2002-10-10 | Жозеф Е. ДУМЕ | Method of preparing water-repellent substance, substance and method of making waterproofness to surface of building material |
| CN102343259A (en) * | 2011-04-13 | 2012-02-08 | 浙江大学 | Method for preparing titanium dioxide nanofilm at low temperature |
| CN102491781A (en) * | 2011-11-04 | 2012-06-13 | 云南大学 | Nanometer photocatalysis surface protection material for stones and stone cultural relic and preparation method of same |
| CN102586948A (en) * | 2011-12-15 | 2012-07-18 | 江南大学 | Anatase type titanium dioxide nano-fiber photocatalyst and preparation method thereof |
| CN102628213A (en) * | 2012-04-09 | 2012-08-08 | 徐雨来 | Method for dispersing anatase nano titanium dioxide on surface of textile fabric |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2190583C2 (en) * | 1997-12-15 | 2002-10-10 | Жозеф Е. ДУМЕ | Method of preparing water-repellent substance, substance and method of making waterproofness to surface of building material |
| CN102343259A (en) * | 2011-04-13 | 2012-02-08 | 浙江大学 | Method for preparing titanium dioxide nanofilm at low temperature |
| CN102491781A (en) * | 2011-11-04 | 2012-06-13 | 云南大学 | Nanometer photocatalysis surface protection material for stones and stone cultural relic and preparation method of same |
| CN102586948A (en) * | 2011-12-15 | 2012-07-18 | 江南大学 | Anatase type titanium dioxide nano-fiber photocatalyst and preparation method thereof |
| CN102628213A (en) * | 2012-04-09 | 2012-08-08 | 徐雨来 | Method for dispersing anatase nano titanium dioxide on surface of textile fabric |
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