CN102382490A - Preparation method and use of hydrophilic automatically-cleaning coating with photocatalytic activity - Google Patents

Preparation method and use of hydrophilic automatically-cleaning coating with photocatalytic activity Download PDF

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Publication number
CN102382490A
CN102382490A CN2011102522040A CN201110252204A CN102382490A CN 102382490 A CN102382490 A CN 102382490A CN 2011102522040 A CN2011102522040 A CN 2011102522040A CN 201110252204 A CN201110252204 A CN 201110252204A CN 102382490 A CN102382490 A CN 102382490A
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photocatalytic activity
coating
preparation
sol
wetting ability
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罗志河
张安杰
陈丽丽
张先宏
张海银
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NORTH WEST YONGXIN GROUP CO Ltd
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NORTH WEST YONGXIN GROUP CO Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B10/00—Integration of renewable energy sources in buildings
    • Y02B10/10—Photovoltaic [PV]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Abstract

The invention provides a preparation method of a hydrophilic automatically-cleaning coating with photocatalytic activity, and belongs to the technical field of chemical engineering. The preparation method is characterized in that butyl titanate and ethyl orthosilicate are utilized as precursors; nanoscale TiO2/SiO2 sol is formed through a sol-gel method; and the nanoscale TiO2/SiO2 sol is coated on the surface of an object and is naturally dried at normal temperature to form an anatase nanoscale TiO2/SiO2 composite film with photocatalytic activity. When the anatase nanoscale TiO2/SiO2 composite film with photocatalytic activity is coated on a solar photovoltaic panel, a vehicle window glass plate or a building glass plate at a normal temperature, the anatase nanoscale TiO2/SiO2 composite film with photocatalytic activity can fast form a hydrophilic coating. Under natural light irradiation, the hydrophilic coating can decompose greasy dirt adhered to the hydrophilic coating into inorganic pollutants, and through rainwater flushing or artificial washing, the inorganic pollutants are removed so that the solar photovoltaic panel or the vehicle window glass plate or the building glass plate is kept as clean as a new one for a long time. The preparation method provided by the invention reduces a production management cost and improves solar photovoltaic panel generating efficiency.

Description

Preparation and application with wetting ability self-cleaning coating of photocatalytic activity
Technical field
The invention belongs to chemical technology field, relate to a kind of preparation method, also relate to the application of this coating simultaneously with wetting ability self-cleaning coating of photocatalytic activity.
Background technology
According to the planning and the encouragement policies of national energy policy, the planning of 2,000 ten thousand kW solar electrical energy generations, 1,000 ten thousand kW Industry Development Area solar electrical energy generations, come the opportunity of sun power great development.But simultaneously, occurred solar panel surface laying dust with other pollutant effect transmittances, be difficult to or need frequent cleaning, cause that handling cost rises, work difficulty strengthens, design performance is difficult to give full play to, degradation practical problems under the generating efficiency.
At present, the contamination resistance that improves coating mainly contains three kinds of methods: 1, reduce the coating surface ability, improve the contact angle of paint film and water, oil, make that pollutent is difficult to adhere to; 2, through adding the hydrophilization auxiliary agent, make coating surface produce hydrophilic radical, reduce paint film and water contact angle, it is not firm to make that oily pollutant adheres to, and is fallen by rain drop erosion easily; 3, through adding the method for photocatalyst, decompose the coating surface pollutent.Though the first method theoretical investigation is many, can realize that similar " lotus leaf effect " anti-market-oriented product that stains effect, also can keep does not for a long time also have; Second method can make the formation hydrophilization surface of filming through adding suitable hydrophilic additive, give the coating self-cleaning property, but the coating contact angle that forms is bigger, and the automatically cleaning effect is not clearly; The anti-contamination effect of the third method is apparent in view, but photocatalysis has very big destructiveness to organic binder.
Therefore, hydrophobicity is combined with photocatalytic activity with photocatalytic activity or wetting ability be very important.Because nano-TiO 2Having active height, good stability, advantage such as nontoxic, cheap, is present most popular photocatalyst material; With butyl(tetra)titanate and tetraethoxy is precursor, and hydrolysis forms nano-TiO 2/ SiO 2Laminated film makes coating have anti-stain characteristic ability preferably.But be precursor with butyl(tetra)titanate and tetraethoxy under the current ambient temperature, the nano titanium oxide that hydrolysis forms is unformed, has only through 500 oThe above pyroprocessing of C could form the titanium oxide of anatase titanium dioxide, have photocatalytic activity, and the coating hydrophilic property maintenance phase is shorter, and this becomes the bottleneck factor of practical application, is difficult to realize industrialized application.
Summary of the invention
The objective of the invention is provides a kind of preparation method with wetting ability self-cleaning coating of photocatalytic activity to the problem that exists in the prior art.
Another object of the present invention provides this wetting ability self-cleaning coating in the concrete application that applies photovoltaic electroplax surface, glass for vehicle window, building glass surface.
The present invention has the preparation method of the wetting ability self-cleaning coating of photocatalytic activity, comprises following process step:
1. the preparation of silicon sol: at 5 ~ 40 ℃, absolute ethyl alcohol is adjusted to pH=2.0～4.5 with hydrochloric acid or Glacial acetic acid min. 99.5, stirs 10～30min, add the tetraethoxy of absolute ethyl alcohol volume 7～14% again, stir 10～20min; The water that adds absolute ethyl alcohol volume 6～10% then stirs 20～40min, obtains water white silicon sol;
2. the preparation of titanium colloidal sol: under 5 ~ 40 ℃, absolute ethyl alcohol is adjusted to pH=2.0～4.5 with hydrochloric acid or Glacial acetic acid min. 99.5, stirs 10～30min, add the butyl(tetra)titanate of absolute ethyl alcohol volume 2～10% again, stir 10～20min; The water that adds absolute ethyl alcohol volume 2～10% then stirs 20～40min, obtains water white titanium colloidal sol;
3. the preparation of silicon titanium complex sol: said silicon sol is mixed with titanium colloidal sol, make TiO in the system 2And SiO 2Mass ratio is 0.25～1.5:1; Stir 1.5～2.5 h, obtain water white silicon titanium colloidal sol, be wetting ability self-cleaning coating with photocatalytic activity.
Above-mentioned stirring velocity is controlled at 500～3000rad/min.
The present invention is a precursor with butyl(tetra)titanate and tetraethoxy, adopts the sol-gel method hydrolysis to form nano-TiO 2/ SiO 2Colloidal sol, this colloidal sol is coated in body surface, forms the dichloride in anatase type TiO with photocatalytic activity at normal temperatures after the seasoning 2/ SiO 2Laminated film.This laminated film is coated on photovoltaic electroplax, glass for vehicle window or the building glass at normal temperatures; Can form one deck hydrophilic coating fast, this coating can be an inorganics with the oil stain decomposition that adheres to above that under natural light irradiation; Under rainwater or artificial flushing; Pollutent is rinsed out, make photovoltaic electroplax or sheet glass clean as new, and can keep for a long time.
Specify through the performance of experiment below the coating of the present invention's preparation.
Fig. 1 is the infrared spectrum of the wetting ability self-cleaning coating with photocatalytic activity for preparing of the present invention, can be found out TiO in this wetting ability self-cleaning coating by Fig. 1 2And SiO 2Also there is TiO in both independent one-tenth phase 2And SiO 2Mixture.With the coating of the present invention's preparation, the coating method that at room temperature adopts spraying, showering or dip-coating is in the surface of photovoltaic electroplax and glass for vehicle window, seasoning at normal temperatures.Fig. 2 is TiO 2/ SiO 2The X-ray diffraction collection of illustrative plates of the dried gel powder of laminated film.As can beappreciated from fig. 2, not only high but also wide peak occurs at 25.3 degree, this peak is anatase octahedrite (a 101) face, not only high but also narrow peak occurs at 38.1 degree, and this peak is anatase octahedrite (a 004) face, and TiO is described 2/ SiO 2TiO in the film 2Be the anatase octahedrite phase.Fig. 3 is TiO 2/ SiO 2The SEM spectrogram of laminated film.Can find out formed TiO by Fig. 3 2/ SiO 2Particle diameter about 18nm, it is nano level that the wetting ability self-cleaning coating with photocatalytic activity that the present invention preparation is described applies the back film that forms.Therefore, the coating of the present invention's preparation has photocatalytic activity.
Fig. 4 forms TiO at glass surface after glass surface applies the coating of the present invention's preparation 2/ SiO 2The light transmittance curve of laminated film and pure glass.Can find out that by Fig. 4 the transmittance of surperficial film forming glass and the transmittance of pure glass are very approaching, and the rainbow effect can not occur, the TiO that forms at glass surface is described 2/ SiO 2Laminated film influences its transmittance hardly.
TiO 2/ SiO 2The hydrophilicity test of laminated film: adopt the dip-coating mode to be coated on the sheet glass seasoning under the normal temperature coating of the present invention's preparation.Use the each 2 μ L redistilled waters of drawing of miniature pipette, drop on this sheet glass, adopt contact angle instrument to measure contact angle.Detected result: the contact angle of water droplet on film is not more than 25 degree, and the film of this moment is highly stable, and water is a circle in the surperficial one way or another uniform spreading of film, promptly on hydrophilicity, shows as isotropy.And illumination after one minute little water droplet can sprawl fully evenly, can satisfy antifog, antifouling self-cleaning demand.Fig. 5 is TiO 2/ SiO 2Contact angle figure on the laminated film.
Photocatalytic activity test: the coating of showering one deck the present invention preparation on sheet glass; After treating seasoning; Fall 10 ml methyl orange solutions (concentration is 0.02 mg/mL) at coating surface, to be dried after, continue to fall methyl orange solution up to dried tropeolin-D color comparatively obviously the time; Sheet glass is put into irradiation under the uv lamp, observe colour-change.The result finds that behind ultra violet lamp 1.5h, the tropeolin-D color disappears, and shows that the coating that the present invention prepares has photocatalytic activity preferably.
TiO 2/ SiO 2The anti-fog performance test of laminated film: 90 ℃ of hot water that in 500 mL beakers, add 200 mL; Under beaker, put a paper of writing full word; With a side scribble the wetting ability self-cleaning coating and sheet glass coating that an other side does not spray self-cleaning coating to being placed down on the beaker, see through coating downwards by sheet glass and observe the clear situation of writing.The result finds: do not spray a side of self-cleaning coating, the handwriting is blurred, and a side of spraying self-cleaning coating, writing is high-visible, explanation thus, and the coating of the present invention's preparation has anti-preferably fog effect.
TiO 2/ SiO 2The anti-contamination aptitude tests of laminated film: the paint spay-coating of the present invention preparation on the sheet glass of 60 * 70 cm, was placed two months on the experiment frame out of doors, observed its anti-contamination ability (and contrast with pure sheet glass).Discovery be coated with coating glass pane surface cleaner, and common glass pane surface has tangible dirt and rainwater vestige, this shows, the coating of the present invention's preparation has anti-preferably contamination ability.
In sum, coating of the present invention is coated on photovoltaic electroplax, glass for vehicle window or the building glass at normal temperatures, can form one deck hydrophilic coating fast; This coating is under natural light irradiation; Can be inorganics with the oil stain decomposition that sticks on photovoltaic electroplax or the sheet glass, under rainwater or artificial flushing, pollutent rinsed out; Make photovoltaic electroplax or sheet glass clean as new, and can keep for a long time.Therefore, can make it have self-cleaning function on its surface that applies the photovoltaic electroplax, influence the problem of transmittance and generating efficiency with other pollutents to overcome existing solar panel surface laying dust.Also can it be coated on vehicle window or the building glass, make it have self-cleaning function, thereby reduce the cleaning interval.
The coating of the present invention's preparation is used to apply the concrete application method of photovoltaic electroplax: be to adopt conventional coating method (spraying, showering or dip-coating), form thin film on photovoltaic electroplax surface.The thickness of film generally is controlled at 1～10 μ m.
The coating of the present invention's preparation is used to apply the concrete application method of glass for vehicle window or building glass: be to adopt conventional coating method (spraying, showering or dip-coating), form thin film on its surface.The thickness of film generally is controlled at the film of 1～10 μ m.
The present invention has the following advantages with respect to prior art:
1, the present invention is a precursor with butyl(tetra)titanate and tetraethoxy, adopts the sol-gel method hydrolysis to form nano-TiO 2/ SiO 2Colloidal sol, its production process is simple, and cost is low, energy-saving and environmental protection, pollution-free.
2, the coating of the present invention's preparation is coated in body surface, just can form the dichloride in anatase type TiO with photocatalytic activity at normal temperatures after the seasoning 2/ SiO 2Laminated film helps realizing suitability for industrialized production.
3, the coating of the present invention's preparation is coated on photovoltaic electroplax or other glass of building at normal temperatures; Have good photocatalysis performance, wetting ability, light transmission and self-cleaning performance; Reduce the production management cost, improved the generating efficiency of photovoltaic electroplax.
Description of drawings
Fig. 1 is the infrared spectrum of the coating for preparing of the present invention.
Fig. 2 be coating that the present invention prepares be coated in body surface the X-ray diffraction collection of illustrative plates of film forming dried gel powder.
Fig. 3 is that the coating that the present invention prepares is coated in the film forming SEM spectrogram of body surface.
Fig. 4 is the light transmittance curve that coating that the present invention prepares is coated in formed film of body surface and pure glass.
Fig. 5 is the contact angle figure that coating that the present invention prepares is coated in the formed film of body surface.
Embodiment
Embodiment one
(1) preparation of silicon sol: accurately measure the beaker that the 50ml absolute ethyl alcohol places 200ml, 5 oIn the water-bath of C, regulate pH=2.0, stir 30 min (speed is 3000rad/min) with the hydrochloric acid of mass concentration 36～38%; The tetraethoxy that adds 7 ml stirs 10min; Add the 5.0ml redistilled water, continue to stir 30 min, obtain water white silicon sol.
2. the preparation of titanium colloidal sol: accurately measure the beaker that the 100ml absolute ethyl alcohol places 500ml, 5 oIn the water-bath of C, regulate pH=2.0, stir 30 min (speed is 3000rad/min) with the hydrochloric acid of mass concentration 36～38%; Add 2 ml butyl(tetra)titanates, stir 10min; Add 10 ml redistilled waters, continue to stir 30min, obtain water white titanium colloidal sol.
3. the preparation of silicon titanium complex sol: the 50ml silicon sol is slowly joined in the 100ml titanium colloidal sol, behind the stirring 1.5h, obtain water white silicon titanium complex sol, be coating of the present invention.In this silicon titanium complex sol, TiO 2The content mass percent is 20 %.
Method with this coating employing showering evenly is coated in photovoltaic electroplax surface, and coating forms film about seasoning 2min at ambient temperature, and the contact angle of this film is 4.2 degree, and thickness is 1 μ m.
Embodiment two
(1) preparation of silicon sol: accurately measure the beaker that the 50ml absolute ethyl alcohol places 200ml, 10 oIn the water-bath of C, regulate pH=2.5, stir 30 min (stirring velocity 2500 rad/min) with the hydrochloric acid of mass concentration 36～38%; The tetraethoxy that under agitation adds 3.5ml stirs 30min; Add the 4.0ml redistilled water, continue to stir 30 min, obtain water white silicon sol.
(2) preparation of titanium colloidal sol: accurately measure the beaker that the 100ml absolute ethyl alcohol places 500ml, 20 oIn the water-bath of C, regulate pH=2.5, stir 20 min (speed is 2500 rad/min) with the hydrochloric acid of mass concentration 36～38%; Stir and add 2 ml butyl(tetra)titanates down, stirring 10min; Add the 8.0ml redistilled water, continue to stir 30min, obtain water white titanium colloidal sol.
(3) preparation of coating: 50 ml silicon sol are slowly added in the 100ml titanium colloidal sol, after continuing to stir 1.5h, obtain water white silicon titanium colloidal sol, be self-cleaning coating of the present invention.In this silicon titanium complex sol, TiO 2The content mass percent is 30 %.
Method with this self-cleaning coating employing showering evenly is coated in photovoltaic electroplax surface, and tectum forms film about seasoning 2min at ambient temperature.The contact angle that adopts contact angle instrument to measure this film is 7.6 degree, and thickness is 2 μ m.
Embodiment three
(1) preparation of silicon sol: accurately measure the beaker that the 50ml absolute ethyl alcohol places 200ml, 25 oIn the water-bath of C, regulate pH=3.5, stir 10 min (stirring velocity is 2000 rad/min) with the hydrochloric acid of mass concentration 36～38%; The tetraethoxy that under agitation adds 4.0ml stirs 10min; Add the 5.0ml redistilled water, continue to stir 30 min, obtain water white silicon sol.
(2) preparation of titanium colloidal sol: accurately measure the beaker that the 100ml absolute ethyl alcohol places 500ml, 25 oIn the water-bath of C, regulate pH=3.5, stir 30 min (stirring velocity is 2000rad/min) with the hydrochloric acid of mass concentration 36～38%; Under agitation add the 3.0ml butyl(tetra)titanate, stir 10min; Add the 3.0ml redistilled water, continue to stir 30min, obtain water white titanium colloidal sol.
(3) preparation of coating: the 50ml silicon sol is slowly added in the 100ml titanium colloidal sol, after continuing to stir 1.5h, obtain water white silicon titanium colloidal sol, be self-cleaning coating of the present invention.In this silicon titanium complex sol, TiO 2The content mass percent is 38 %.
Method with this coating employing dip-coating evenly is coated in photovoltaic electroplax surface, and tectum forms film about seasoning 2min at ambient temperature.The contact angle of measuring this film through contact angle instrument is 10.2 degree, and thickness is 5 μ m.
Embodiment four
(1) preparation of silicon sol: accurately measure the beaker that the 50ml absolute ethyl alcohol places 200ml, 30 oIn the water-bath of C, regulate pH=4.0, stir 30 min (stirring velocity is 1000rad/min) with the hydrochloric acid of mass concentration 36～38%; The tetraethoxy that under agitation adds 5ml stirs 10min; Add the 4.0ml redistilled water, continue to stir 20 min, obtain water white silicon sol.
(2) preparation of titanium colloidal sol: accurately measure the beaker that the 100ml absolute ethyl alcohol places 500ml, 30 oIn the water-bath of C, regulate pH=4.0, stir 30 min (stirring velocity is 1000rad/min) with the hydrochloric acid of mass concentration 36～38%; Under agitation add the 5.0ml butyl(tetra)titanate, stir 10min; Add the 2.0ml redistilled water, continue to stir 40min, obtain water white titanium colloidal sol.
3. the preparation of coating: the 50ml silicon sol is slowly added in the 100ml titanium colloidal sol, after continuing to stir 1.5h, add 150ml ethanol, continue to stir 1.5h, obtain water white silicon titanium colloidal sol, be coating of the present invention.In this silicon titanium complex sol, TiO 2The content mass percent is 46%.
This coating is adopted the method that sprays, evenly be coated on the glass for vehicle window, tectum forms film about seasoning 2min at ambient temperature.The contact angle of measuring this film through contact angle instrument is 14.8 degree, and thickness is 10 μ m.
Embodiment five:
(1) preparation of silicon sol: accurately measure the beaker that the 50ml absolute ethyl alcohol places 200ml, 40 oIn the water-bath of C, regulate pH=4.5, stir 30 min (stirring velocity 500rad/min) with the hydrochloric acid of mass concentration 36～38%; The tetraethoxy that under agitation adds 5ml stirs 10min; Add the 3.0ml redistilled water, continue to stir 20 min, obtain water white silicon sol.
(2) preparation of titanium colloidal sol: accurately measure the beaker that the 100ml absolute ethyl alcohol places 500ml, 40 oIn the water-bath of C, regulate pH=4.5, stir 20 min (stirring velocity 500rad/min) with the hydrochloric acid of mass concentration 36～38%; Under agitation drip the 8.5ml butyl(tetra)titanate, stir 10min; Add 3 ml redistilled waters, continue to stir 30min, obtain water white titanium colloidal sol.
3. the preparation of coating: the 50ml silicon sol is slowly added in the 100ml titanium colloidal sol, after continuing to stir 1.5h, obtain water white silicon titanium colloidal sol, promptly water white wetting ability self-cleaning coating with photocatalytic activity.In this silicon titanium complex sol, TiO 2The content mass percent is 60%.
Adopt the method for spraying evenly to be coated on the glass for vehicle window this coating, tectum forms film about seasoning 2min at ambient temperature.Measuring contact angle through contact angle instrument is 24.8 degree, and thickness is 8 μ m.

Claims (8)

1. preparation method with wetting ability self-cleaning coating of photocatalytic activity is characterized in that may further comprise the steps:
1. the preparation of silicon sol: at 5 ~ 40 ℃, absolute ethyl alcohol is adjusted to pH=2.0～4.5 with hydrochloric acid or Glacial acetic acid min. 99.5, stirs 10～30min, add the tetraethoxy of absolute ethyl alcohol volume 7～14% again, stir 10～20min; The water that adds absolute ethyl alcohol volume 6～10% then stirs 20～40min, obtains water white silicon sol;
2. the preparation of titanium colloidal sol: under 5 ~ 40 ℃, absolute ethyl alcohol is adjusted to pH=2.0～4.5 with hydrochloric acid or Glacial acetic acid min. 99.5, stirs 10～30min, add the butyl(tetra)titanate of absolute ethyl alcohol volume 2～10% again, stir 10～20min; The water that adds absolute ethyl alcohol volume 2～10% then stirs 20～40min, obtains water white titanium colloidal sol;
3. the preparation of silicon titanium complex sol: said silicon sol is mixed with titanium colloidal sol, make TiO in the system 2And SiO 2Mass ratio is 0.25～1.5:1; Stir 1.5～2.5 h, obtain water white silicon titanium colloidal sol, be wetting ability self-cleaning coating with photocatalytic activity.
2. have the preparation method of the wetting ability self-cleaning coating of photocatalytic activity according to claim 1, it is characterized in that: said stirring velocity is 500～3000rad/min.
3. the wetting ability self-cleaning coating that has photocatalytic activity according to claim 1 is used to apply the surface of photovoltaic electroplax.
4. be used to apply the surface of photovoltaic electroplax like the said wetting ability self-cleaning coating with photocatalytic activity of claim 3, it is characterized in that: adopt conventional coating method, making photovoltaic electroplax surface form thickness is the film of 1～10 μ m.
5. the wetting ability self-cleaning coating that has photocatalytic activity according to claim 1 is used to apply the surface of glass for vehicle window.
6. be used to apply the surface of glass for vehicle window like the said wetting ability self-cleaning coating with photocatalytic activity of claim 5, it is characterized in that: adopt conventional coating method, making the glass for vehicle window surface form a layer thickness is the film of 1～10 μ m.
7. the wetting ability self-cleaning coating that has photocatalytic activity according to claim 1 is used to apply the surface of building glass.
8. be used to apply the surface of building glass like the said wetting ability self-cleaning coating with photocatalytic activity of claim 7, it is characterized in that: adopt conventional coating method, making the building glass surface form a layer thickness is the film of 1～10 μ m.
CN2011102522040A 2011-08-30 2011-08-30 Preparation method and use of hydrophilic automatically-cleaning coating with photocatalytic activity Pending CN102382490A (en)

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