CN105254186A - Preparation method for self-cleaning glass - Google Patents

Preparation method for self-cleaning glass Download PDF

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Publication number
CN105254186A
CN105254186A CN201510716011.4A CN201510716011A CN105254186A CN 105254186 A CN105254186 A CN 105254186A CN 201510716011 A CN201510716011 A CN 201510716011A CN 105254186 A CN105254186 A CN 105254186A
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glass
self
liquid
time
acid
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CN201510716011.4A
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Chinese (zh)
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陆志文
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Suzhou Lingtong Glass Products Co Ltd
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Suzhou Lingtong Glass Products Co Ltd
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Priority to CN201510716011.4A priority Critical patent/CN105254186A/en
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Abstract

The invention discloses a preparation method for self-cleaning glass. The preparation method comprises the steps that 1, liquid A-SiO2 sol is prepared; 2, liquid B-TiO2 sol is prepared; 3, glass to be processed through film coating is sequentially processed through acid pickling and alcohol washing, and then thermal treatment is performed to enable the temperature of the glass to be kept at 500 DEG C-580 DEG C; 4, first-time film coating is performed with the liquid A; 5, second-time film coating is performed with the liquid B. According to the preparation method, a mixed-type acid catalyst is adopted as a catalyst for preparing the sol. According to the self-cleaning glass prepared through the method, the dependency of a super-hydrophilic film formed on the surface of the self-cleaning glass on ultraviolet light is reduced, organic pollutants can be effectively removed under visible light, the anti-fog effect is good, the super good self-cleaning effect can be kept, even if the glass is placed at a dark place for a period of time, the glass still has super hydrophilicity, and the super-hydrophilic film layer is firmly bound with a glass substrate.

Description

A kind of self-cleaning glass preparation method
Technical field
The present invention relates to a kind of self-cleaning glass preparation method.
Background technology
Along with the raising that people require aesthetic and quality of the life, glass is subject to increasing welcome in the field such as buildings, automobile, but glass also brings many difficult problems while bringing people's light and beauty, and the cleaning problem as building glass curtain wall annoyings people always.
At present, be mainly divided into two kinds: one to be form hydrophobic membrane at glass surface about self-cleaning glass, make surface dust and microbial spore firmly can not stick to coatingsurface, be easy to be taken away by rainwater, thus realize automatically cleaning; Another kind forms super hydrophilic film at glass surface, because super hydrophilic film can produce electronics and hole under the irradiation of normal pressure and sunlight, and electronics and hole finally can produce superoxide radical and hydroxyl radical free radical with external environment, these free radicals can, without the organism being selectively oxidized glass surface, finally allow them allow rainwater wash away with dust etc.Be only the adhesion of decreasing pollution thing due to hydrophobic type instead of carry out oxidation explanation to pollutent, time therefore in the face of being difficult to the greasy dirt of removing, it will be felt simply helpless, so the research of the current overwhelming majority launches around wetting ability.The hydrophilic self-cleaning glass preparation method of the prior art shortcoming such as have rete strongly to rely on illumination, rete cohesive force not strong.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of self-cleaning glass preparation method.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of self-cleaning glass preparation method, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, acid catalyst and dehydrated alcohol mixing ultrasonic after, ageing at least 12 hours; Described acid catalyst is the mixing acid of valeric acid and hydrochloric acid; Preferably, in described acid catalyst, the mol ratio of valeric acid and hydrochloric acid is 1:1-1:2.
(2) B liquid TiO is prepared 2colloidal sol, by butyl (tetra) titanate, distilled water, acid catalyst and dehydrated alcohol mixing ultrasonic after, ageing at least 12 hours; Preferably, in described acid catalyst, the mol ratio of valeric acid and hydrochloric acid is 1:1-1:2.
(3) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 500-580 DEG C;
(4) first time plated film, A liquid is sprayed at the glass surface processed through step (3); Preferably, coating film thickness is 30-60nm for the first time.
(5) second time plated film, is sprayed at the glass surface after step (4) process by B liquid; Preferably, second time coating film thickness is 40-80nm.
Preferably, the ultrasonic time in step (1) and step (2) is 10-25min.
Preferably, described tetraethoxy, distilled water, valeric acid and dehydrated alcohol take mol ratio as 1:10:0.01:50.
Preferably, described butyl (tetra) titanate, distilled water, valeric acid and dehydrated alcohol are with mol ratio 1:5:0.01:40.
Preferably, the PEG2000 that massfraction is 1.2% is also added with in described B liquid.
The beneficial effect that the present invention reaches:
(1) the super hydrophilic film on the self-cleaning glass surface of the present invention's manufacture reduces the dependency of UV-light, effectively can remove organic pollutant under visible light, good antifogging effect, extraordinary automatically cleaning effect can be maintained, even be placed in dark place for some time, glass still has Superhydrophilic;
(2) super hydrophilic membrane is combined firmly with substrate of glass, and weather resistance is superior.
Embodiment
Below in conjunction with embodiment, the invention will be further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
A kind of self-cleaning glass preparation method, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, acid catalyst and dehydrated alcohol are that 1:10:0.01:50 mixes with mol ratio, ultrasonic 15min, ageing 24 hours;
(2) B liquid TiO is prepared 2colloidal sol, by butyl (tetra) titanate, distilled water, acid catalyst and dehydrated alcohol are that 1:5:0.01:40 mixes with mol ratio, after ultrasonic 15min, then add the PEG2000 that massfraction is 1.2%, ultrasonic 5min, ageing 24 hours;
Step (1) and the middle acid catalyst of step (2) are mol ratio is the valeric acid of 1:1 and the mixture of hydrochloric acid.
(3) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 550 DEG C;
(4) first time plated film, A liquid is sprayed at the glass surface processed through step (3); Coating film thickness is 60nm for the first time.
(5) second time plated film, is sprayed at the glass surface after step (4) process by B liquid; Second time coating film thickness is 50nm.
Embodiment 2
A kind of self-cleaning glass preparation method, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, acid catalyst and dehydrated alcohol are that 1:10:0.01:50 mixes with mol ratio, ultrasonic 20min, ageing 12 hours;
(2) B liquid TiO is prepared 2colloidal sol, by butyl (tetra) titanate, distilled water, acid catalyst and dehydrated alcohol are that 1:5:0.01:40 mixes with mol ratio, after ultrasonic 20min, then add the PEG2000 that massfraction is 1.2%, ultrasonic 5min, ageing 12 hours;
Step (1) and the middle acid catalyst of step (2) are mol ratio is the valeric acid of 1:1.2 and the mixture of hydrochloric acid.
(3) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 500 DEG C;
(4) first time plated film, A liquid is sprayed at the glass surface processed through step (3); Coating film thickness is 40nm for the first time.
(5) second time plated film, is sprayed at the glass surface after step (4) process by B liquid; Second time coating film thickness is 80nm.
Embodiment 3
A kind of self-cleaning glass preparation method, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, acid catalyst and dehydrated alcohol are that 1:10:0.01:50 mixes with mol ratio, ultrasonic 10min, ageing 16 hours;
(2) B liquid TiO is prepared 2colloidal sol, by butyl (tetra) titanate, distilled water, acid catalyst and dehydrated alcohol are that 1:5:0.01:40 mixes with mol ratio, after ultrasonic 20min, then add the PEG2000 that massfraction is 1.2%, ultrasonic 5min, ageing 16 hours;
(3) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 500 DEG C;
Step (1) and the middle acid catalyst of step (2) are mol ratio is the valeric acid of 1:2 and the mixture of hydrochloric acid.
(4) first time plated film, A liquid is sprayed at the glass surface processed through step (3); Coating film thickness is 40nm for the first time.
(5) second time plated film, is sprayed at the glass surface after step (4) process by B liquid; Second time coating film thickness is 80nm.
Comparative example 1
A kind of self-cleaning glass preparation method, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, hydrochloric acid and dehydrated alcohol are that 1:10:0.01:50 mixes with mol ratio, ultrasonic 20min, ageing 12 hours;
(2) B liquid TiO is prepared 2colloidal sol, by butyl (tetra) titanate, distilled water, acid catalyst and dehydrated alcohol are that 1:5:0.01:40 mixes with mol ratio, after ultrasonic 20min, then add the PEG2000 that massfraction is 1.2%, ultrasonic 5min, ageing 12 hours;
(3) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 500 DEG C;
(4) first time plated film, A liquid is sprayed at the glass surface processed through step (3); Coating film thickness is 40nm for the first time.
(5) second time plated film, is sprayed at the glass surface after step (4) process by B liquid; Second time coating film thickness is 80nm.
Comparative example 2
A kind of self-cleaning glass preparation method, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, acid catalyst and dehydrated alcohol are that 1:10:0.01:50 mixes with mol ratio, ultrasonic 20min, ageing 12 hours;
Step (1) acid catalyst is mol ratio is the valeric acid of 1:1.2 and the mixture of hydrochloric acid.
(2) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 500 DEG C;
(3) plated film, is sprayed at the glass surface processed through step (3) by A liquid; Coating film thickness is 120nm for the first time.
Measure of merit:
One, Contact-angle measurement result: embodiment 1:1.2 °, embodiment 2:0.3 °, embodiment 3:1.0 °, comparative example 1:3.1 °, comparative example 2:3.8 °, the self-cleaning glass that market is bought: 4.5 °.Can find out thus, the self-cleaning glass contact angle that the inventive method obtains is all lower than 5 °, and also have outstanding advantage compared with commercially available self-cleaning glass, contact angle is all lower than 4 °.
Two, super-hydrophilic thin film cohesive force on the glass substrate.The self-cleaning glass bought embodiment 1-4, comparative example 1-2 and market carries out adhesive force respectively to be tested, and result is as follows:
Embodiment 1:28N, embodiment 2:29N, embodiment 3:25N, comparative example 1:15N, comparative example 2:18N, available glass: 11N.Result can be found out thus, has higher bonding strength between the super hydrophilic film that the inventive method obtains and substrate of glass, and mixed-acid catalyst can the more excellent colloidal sol of processability, and then affect final film performance.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and distortion, these improve and distortion also should be considered as protection scope of the present invention.

Claims (6)

1. a self-cleaning glass preparation method, is characterized in that, comprises step:
(1) A liquid SiO is prepared 2colloidal sol, by tetraethoxy, distilled water, acid catalyst and dehydrated alcohol mixing ultrasonic after, ageing at least 12 hours; Described acid catalyst is the mixing acid of valeric acid and hydrochloric acid;
(2) B liquid TiO is prepared 2colloidal sol, by butyl (tetra) titanate, distilled water, acid catalyst and dehydrated alcohol mixing ultrasonic after, ageing at least 12 hours; Described acid catalyst is the mixing acid of valeric acid and hydrochloric acid;
(3) by glass to be coated successively through overpickling and alcohol wash, then thermal treatment makes glass temperature remain on 500-580 DEG C;
(4) first time plated film, A liquid is sprayed at the glass surface processed through step (3);
(5) second time plated film, is sprayed at the glass surface after step (4) process by B liquid.
2. a kind of self-cleaning glass preparation method according to claim 1, is characterized in that, coating film thickness is 30-60nm for the first time, and second time coating film thickness is 40-80nm.
3. a kind of self-cleaning glass preparation method according to claim 1, is characterized in that, the ultrasonic time in step (1) and step (2) is 10-25min.
4. a kind of self-cleaning glass preparation method according to claim 1, is characterized in that, described tetraethoxy, distilled water, and valeric acid and dehydrated alcohol take mol ratio as 1:10:0.01:50.
5. a kind of self-cleaning glass preparation method according to claim 1, it is characterized in that, described butyl (tetra) titanate, distilled water, valeric acid and dehydrated alcohol are with mol ratio 1:5:0.01:40.
6. a kind of self-cleaning glass preparation method according to claim 1, is characterized in that, is also added with the PEG2000 that massfraction is 1.2% in described B liquid.
CN201510716011.4A 2015-10-29 2015-10-29 Preparation method for self-cleaning glass Pending CN105254186A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474600A (en) * 2017-09-11 2017-12-15 新材料与产业技术北京研究院 Self-cleaning coating composition and its preparation method and application
CN108147677A (en) * 2017-12-06 2018-06-12 吕莉 A kind of preparation method of high efficiency photocatalysis glass with clean

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003306347A (en) * 2002-04-15 2003-10-28 Bridgestone Corp Stain-proofing glass
CN1548403A (en) * 2003-05-09 2004-11-24 山 汪 Protecting composite membrane and its prepn
CN102503554A (en) * 2011-11-02 2012-06-20 西南交通大学 Method for preparing oil-water-soaked light-operated reversible SiO2/TiO2 composite coating on silicon substrate surface
CN104711551A (en) * 2013-12-16 2015-06-17 天津森宇仕达科技发展有限公司 Preparation method for double-layer low refractive index antireflection film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003306347A (en) * 2002-04-15 2003-10-28 Bridgestone Corp Stain-proofing glass
CN1548403A (en) * 2003-05-09 2004-11-24 山 汪 Protecting composite membrane and its prepn
CN102503554A (en) * 2011-11-02 2012-06-20 西南交通大学 Method for preparing oil-water-soaked light-operated reversible SiO2/TiO2 composite coating on silicon substrate surface
CN104711551A (en) * 2013-12-16 2015-06-17 天津森宇仕达科技发展有限公司 Preparation method for double-layer low refractive index antireflection film

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474600A (en) * 2017-09-11 2017-12-15 新材料与产业技术北京研究院 Self-cleaning coating composition and its preparation method and application
CN108147677A (en) * 2017-12-06 2018-06-12 吕莉 A kind of preparation method of high efficiency photocatalysis glass with clean

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Application publication date: 20160120