CN105254186A - Preparation method of self-cleaning glass - Google Patents
Preparation method of self-cleaning glass Download PDFInfo
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- 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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- self
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- liquid
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- 239000005348 self-cleaning glass Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 28
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000003377 acid catalyst Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 17
- 239000012153 distilled water Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 230000032683 aging Effects 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 13
- 229940005605 valeric acid Drugs 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000007669 thermal treatment Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 2
- 238000007747 plating Methods 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- -1 hydroxyl radical free radical Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Landscapes
- Catalysts (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a preparation method of self-cleaning glass. The method comprises the following steps: 1. preparation of solution A SiO2Sol, 2. preparation of TiO solution B2Sol, 3, acid washing and alcohol washing the glass to be coated, then heat treating to keep the glass temperature at 500-580 deg.C, 4, plating the first film with A solution, 5, plating the second film with B solution, the catalyst for preparing sol is mixedAnd (3) an acid combination catalyst. The super-hydrophilic film on the surface of the self-cleaning glass manufactured by the invention has the advantages of reduced dependence on ultraviolet light, effective removal of organic pollutants under visible light, good antifogging effect, and capability of maintaining a very good self-cleaning effect, and even if the self-cleaning glass is placed in a dark place for a period of time, the super-hydrophilic film still has super-hydrophilicity and is firmly combined with the glass substrate.
Description
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510716011.4A CN105254186A (en) | 2015-10-29 | 2015-10-29 | Preparation method of self-cleaning glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510716011.4A CN105254186A (en) | 2015-10-29 | 2015-10-29 | Preparation method of self-cleaning glass |
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| CN105254186A true CN105254186A (en) | 2016-01-20 |
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| CN201510716011.4A Pending CN105254186A (en) | 2015-10-29 | 2015-10-29 | Preparation method of self-cleaning glass |
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Cited By (2)
| 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)
| 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 |
-
2015
- 2015-10-29 CN CN201510716011.4A patent/CN105254186A/en active Pending
Patent Citations (4)
| 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)
| 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 |