CN1417147A - Low-temperature prepn process of self-cleaning nano Tio2 glass - Google Patents
Low-temperature prepn process of self-cleaning nano Tio2 glass Download PDFInfo
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- CN1417147A CN1417147A CN 02150721 CN02150721A CN1417147A CN 1417147 A CN1417147 A CN 1417147A CN 02150721 CN02150721 CN 02150721 CN 02150721 A CN02150721 A CN 02150721A CN 1417147 A CN1417147 A CN 1417147A
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Abstract
The present invention relates to a low temperature treating process of self-cleaning TiO2 nanoglass. By using silica and anatase type nanosol as basic components and through pulling process, film is formed on the surface of glass plate. The film is dried at room temperature and cured or treated at temperature below 300 deg.c and cooled naturally. The prepared self-cleaned glass has excellent photocatalytic property, superhydrophilic property, high and homogeneous transparency. The said process is simple, low in cost and suitable for industrial production.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the method that a kind of low temperature prepares the nano titanium oxide self-cleaning glass.
Background technology
Found nano titanium oxide since splitting water into hydrogen and oxygen under the UV-irradiation since 1972, titanium dioxide is subjected to paying attention to very widely at material circle.In nano semiconductor material, Detitanium-ore-type TiO
2With its photocatalysis efficiency height, good stability, nontoxic and receive very big concern.Moreover, with Detitanium-ore-type TiO
2The film of making also has photic super hydrophilicity, has expanded its practical use more.Use Detitanium-ore-type TiO
2The film of preparation both can be used for degradation of organic substances, sterilization and disinfection, sewage disposal, purifying air etc., as made green light catalytic materials such as self-cleaning glass, sterilization ceramic tile, sewage purification material, also can be used as antifog material, was used for occasions such as automobile rearview mirror.At present, nano-TiO
2Research become a very active problem of nanometer novel material exploitation.
Preparation TiO
2The method of film is a lot, and its relative merits are respectively arranged.As with physics method depositing Ti O such as direct current reaction magnetron sputterings
2The glass of film has the good transparency, stronger photocatalysis performance and photic Superhydrophilic, film evenly, controllable thickness, but must vacuum system, the equipment price costliness, sputter rate also is a big bottleneck of its development of restriction in addition; The film of sol-gel method preparation has the purity height, reaction conditions is easy to advantages such as control, but need toast under comparatively high temps; And there is certain degree of difficulty in chemical Vapor deposition process in preparation large area film fashion.Just because of the various limitation that exist in various film-forming methods and the means, thereby seriously restricted nano-TiO
2The practicalization of thin-film material.
Summary of the invention
The objective of the invention is to propose that a kind of equipment is simple, investment is little, be easy to suitability for industrialized production, low-temperature curable prepares the method for nano-titanium dioxide film self-cleaning glass.Self-cleaning glass with this method preparation has good photochemical catalysis and super hydrophilicity, and transmittance is higher, and evenly.
The low-temperature curing that the present invention proposes prepares nano-titanium dioxide film self-cleaning glass method, with silicon-dioxide, Detitanium-ore-type TiO
2The colloidal sol nano material is basic composition, adopts crystal pulling method to form film at glass baseplate surface, and is at room temperature dry, solidify, or handles the back naturally cooling under less than 300 ℃ of temperature and get final product.
Among the present invention, silicon-dioxide derives from water-soluble silicon colloidal sol or tetraethoxysilance hydrolysis, Detitanium-ore-type TiO
2Colloidal sol is by TiCl
4Or other titanium salt hydrolysis preparation and obtaining, the relative content of each component is (is 1 unit with total volume): tetraethoxysilance or water-soluble silicon colloidal sol 0.1~10%, Detitanium-ore-type TiO
2Colloidal sol 1~30% (TiO
2Net content is 0.065%~1.948%), all the other are deionized water or deionized water and HCl.Membrane structure such as Fig. 1 show.
The concrete steps of preparation are: above-mentioned basic component is diluted with dehydrated alcohol, add deionized water, perhaps directly add deionized water, be stirred into colloid, glass substrate vertically is put in the colloid, at the uniform velocity lifts then, at room temperature dry, curing, or under less than 300 ℃ of temperature, handle the back naturally cooling, promptly get the nano titanium oxide self-cleaning glass.
Experiment showed, that the self-cleaning glass by the present invention's preparation has good Superhydrophilic and photocatalysis performance:
1. wetting ability experiment.In power density is 200 μ W/cm2, and wavelength is to shine under the UV-light of 254nm, measures the variation of the contact angle of water droplet (1 μ l) and film surface with the UV-irradiation time.Through after the irradiation of 40min time, contact angle is less than 1 degree, as shown in Figure 2.Has good anti-fog function.
2. photochemical catalysis experiment.Be about 100 μ W/cm2 in power density, wavelength is to shine under the UV-light of 254nm, to the decomposition of dyestuff methylene blue, as shown in Figure 3.
With half glass that is coated with nano-titanium dioxide film on March 26th, 2002 to being positioned between 10 days November in 2002 on outdoor windowsill, after water dashes as a result, this nano-TiO is arranged
2The part of film cleaning is bright, and the part dirt that does not have a film is still on its surface.
The inventive method, equipment is simple, invests for a short time, is easy to suitability for industrialized production.
This self-cleaning glass can be widely used in the window glass of buildings, auto mirror etc.
Description of drawings
Fig. 1 is this nano titanium oxide self-cleaning glass membrane structure diagram.
Fig. 2 is in the hydrophilic experiment, the diagram that contact angle changed with the UV-irradiation time.Wherein, Fig. 2 (a) is (6 °) diagram before the illumination, and Fig. 2 (b) illustrates for (0 °) after the illumination, and Fig. 2 (c) is a change curve.
Fig. 3 is in the photochemical catalysis experiment, to the decomposition diagram of dyestuff methylene blue.
Number in the figure: 1 is glass substrate, and 2 is film.
Embodiment
The invention is further illustrated by the following examples.
Embodiment 1: with 9.2ml Detitanium-ore-type TiO
2Colloid, 3ml water-soluble silicon colloidal sol and 47.8ml deionized water mix and stir; The glass substrate of previously prepd cleaning is vertically put into colloid, then it is at the uniform velocity lifted, place clean environment, and at room temperature dry, solidify or handling the back naturally cooling down smaller or equal to 300 ℃.Zhi Bei self-cleaning glass is that 254nm, optical power density are 200 μ W/cm at wavelength thus
2UV-light under the irradiation 40 minutes after, contact angle is reduced to below 1 ° by 54 °, approaches 0 °, has tangible anti-fog function.
Embodiment 2: the tetraethoxysilance of 4ml was mixed stirring after 4 hours with 50ml dehydrated alcohol (〉=99.7%), add the mixed solution of deionized water (4ml) and HCl (0.12ml), and stirred 2 hours; Again will be with the Detitanium-ore-type TiO of dehydrated alcohol (50ml) dilution
2Colloid (20ml) adds wherein, mixes with ultrasonic device.The clean glass substrate of previously prepd is inserted wherein, and vertically at the uniform velocity lift, place it in seasoning in the clean environment, curing or descending processing back naturally cooling getting final product smaller or equal to 300 ℃.Zhi Bei self-cleaning glass is that 254nm, optical power density are 160 μ W/cm at wavelength thus
2UV-light under the irradiation 40 minutes after, the contact angle of water is reduced to below 1 ° by 13 °.
Claims (4)
1, a kind of nano titanium oxide self-cleaning glass low temperature preparation method is characterized in that with silicon-dioxide and Detitanium-ore-type TiO
2Nano material is basic composition, makes colloid, adopts crystal pulling method to form film at glass baseplate surface, at room temperature dry, curing, or under less than 300 ℃ temperature, handle cooling then.
2, preparation method according to claim 1 is characterized in that silicon-dioxide derives from water-soluble silicon colloidal sol or tetraethoxy, Detitanium-ore-type TiO
2Colloidal sol is by TiCl
4Or other titanium salt hydrolysis preparation and obtaining.
3, preparation method according to claim 2, the content that it is characterized in that each component in the colloid is tetraethoxy or water-soluble silicon colloidal sol 0.1-10%, Detitanium-ore-type TiO
2Colloidal sol 1-30%, Detitanium-ore-type TiO
2Middle TiO
2Molten net content is 0.065-1.948%.
4, preparation method according to claim 3, it is characterized in that the concrete steps that prepare are as follows: basic component is diluted with dehydrated alcohol, add deionized water again, perhaps directly add ionized water, be stirred into colloid, glass substrate vertically is put in the colloid, at the uniform velocity lift then, at room temperature dry, curing are perhaps handled the back naturally cooling under less than 300 ℃ of temperature.
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CN 02150721 CN1228267C (en) | 2002-11-26 | 2002-11-26 | Low-temperature prepn process of self-cleaning nano Tio2 glass |
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CN 02150721 CN1228267C (en) | 2002-11-26 | 2002-11-26 | Low-temperature prepn process of self-cleaning nano Tio2 glass |
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Cited By (15)
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WO2004062795A1 (en) * | 2003-01-08 | 2004-07-29 | The Chinese University Of Hong Kong | Optically transparent tio2 thin films on glass having anti-bacterial and anti-virus activities and method for preparing the same |
CN1331794C (en) * | 2005-08-15 | 2007-08-15 | 上海耀华皮尔金顿玻璃股份有限公司 | Rutile phase based TiO2 low radiation filming glass capable of toughening and its technics |
CN100348335C (en) * | 2004-04-16 | 2007-11-14 | 天津理工学院 | Device and process for producing nano TiO2 film by supersonic atomization |
CN1911846B (en) * | 2006-08-15 | 2010-05-12 | 福耀玻璃工业集团股份有限公司 | Nanometer self-cleaning composition |
CN102046553A (en) * | 2008-05-26 | 2011-05-04 | 法国圣戈班玻璃厂 | Temporary protection of glass |
CN101372394B (en) * | 2007-08-21 | 2011-12-07 | 黑龙江大学 | Method for synthesizing ultra-hydrophilic film using surfactant modified titania |
CN102503156A (en) * | 2011-10-20 | 2012-06-20 | 北京工业大学 | Preparation method for super hydrophilic membranes |
CN1898173B (en) * | 2003-10-23 | 2012-11-14 | 法国圣戈班玻璃厂 | Substrate, in particular glass substrate, supporting at least one stack of a photocatalytic layer and a sublayer for the heteroepitaxial growth of said layer |
CN102817021A (en) * | 2012-08-28 | 2012-12-12 | 南昌大学 | Method for preparing novel visible light-responded N-TiO2/SiO2 composite file on surface of fluorine-carbon aluminum single sheet |
CN103086613A (en) * | 2013-03-05 | 2013-05-08 | 福建圣元电子科技有限公司 | Preparation method of anti-reflection self-cleaning coated glass |
CN103482883A (en) * | 2013-09-18 | 2014-01-01 | 苏州大学 | Preparation method of super hydrophilic glass surface |
CN103923501A (en) * | 2014-04-10 | 2014-07-16 | 上海理工大学 | Nano-sol for forming anti-aging and stain-resistant nano-coating and preparation method and application thereof |
CN104785232A (en) * | 2015-03-17 | 2015-07-22 | 珠海全程科技有限公司 | Low-temperature preparation method for high-activity nano titanium dioxide thin film loaded on ceramic |
CN108892369A (en) * | 2018-07-26 | 2018-11-27 | 安徽朗旭玻璃器皿有限公司 | A kind of self-cleaning glass and production technology |
CN110922060A (en) * | 2019-11-27 | 2020-03-27 | 江苏捷斯安环保科技有限公司 | Preparation method and application method of nano titanium dioxide photocatalytic sol |
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2002
- 2002-11-26 CN CN 02150721 patent/CN1228267C/en not_active Expired - Fee Related
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WO2004062795A1 (en) * | 2003-01-08 | 2004-07-29 | The Chinese University Of Hong Kong | Optically transparent tio2 thin films on glass having anti-bacterial and anti-virus activities and method for preparing the same |
CN1898173B (en) * | 2003-10-23 | 2012-11-14 | 法国圣戈班玻璃厂 | Substrate, in particular glass substrate, supporting at least one stack of a photocatalytic layer and a sublayer for the heteroepitaxial growth of said layer |
CN100348335C (en) * | 2004-04-16 | 2007-11-14 | 天津理工学院 | Device and process for producing nano TiO2 film by supersonic atomization |
CN1331794C (en) * | 2005-08-15 | 2007-08-15 | 上海耀华皮尔金顿玻璃股份有限公司 | Rutile phase based TiO2 low radiation filming glass capable of toughening and its technics |
CN1911846B (en) * | 2006-08-15 | 2010-05-12 | 福耀玻璃工业集团股份有限公司 | Nanometer self-cleaning composition |
CN101372394B (en) * | 2007-08-21 | 2011-12-07 | 黑龙江大学 | Method for synthesizing ultra-hydrophilic film using surfactant modified titania |
CN102046553A (en) * | 2008-05-26 | 2011-05-04 | 法国圣戈班玻璃厂 | Temporary protection of glass |
CN102046553B (en) * | 2008-05-26 | 2016-03-30 | 法国圣戈班玻璃厂 | The temporary protection of glass |
CN102503156A (en) * | 2011-10-20 | 2012-06-20 | 北京工业大学 | Preparation method for super hydrophilic membranes |
CN102817021A (en) * | 2012-08-28 | 2012-12-12 | 南昌大学 | Method for preparing novel visible light-responded N-TiO2/SiO2 composite file on surface of fluorine-carbon aluminum single sheet |
CN103086613B (en) * | 2013-03-05 | 2015-06-24 | 福建圣元电子科技有限公司 | Preparation method of anti-reflection self-cleaning coated glass |
CN103086613A (en) * | 2013-03-05 | 2013-05-08 | 福建圣元电子科技有限公司 | Preparation method of anti-reflection self-cleaning coated glass |
CN103482883A (en) * | 2013-09-18 | 2014-01-01 | 苏州大学 | Preparation method of super hydrophilic glass surface |
CN103482883B (en) * | 2013-09-18 | 2015-10-28 | 苏州大学 | A kind of preparation method of super hydrophilic glass surface |
CN103923501B (en) * | 2014-04-10 | 2016-02-10 | 上海理工大学 | A kind of Nano sol for the formation of anti-aging, stain resistant nano coating and preparation method and application |
CN103923501A (en) * | 2014-04-10 | 2014-07-16 | 上海理工大学 | Nano-sol for forming anti-aging and stain-resistant nano-coating and preparation method and application thereof |
CN104785232A (en) * | 2015-03-17 | 2015-07-22 | 珠海全程科技有限公司 | Low-temperature preparation method for high-activity nano titanium dioxide thin film loaded on ceramic |
CN108892369A (en) * | 2018-07-26 | 2018-11-27 | 安徽朗旭玻璃器皿有限公司 | A kind of self-cleaning glass and production technology |
CN108892369B (en) * | 2018-07-26 | 2021-04-16 | 安徽朗旭玻璃器皿有限公司 | Self-cleaning glass and production process thereof |
CN110922060A (en) * | 2019-11-27 | 2020-03-27 | 江苏捷斯安环保科技有限公司 | Preparation method and application method of nano titanium dioxide photocatalytic sol |
CN110922060B (en) * | 2019-11-27 | 2022-04-26 | 江苏捷斯安环保科技有限公司 | Preparation method and application method of nano titanium dioxide photocatalytic sol |
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