CN106675238A - Method for preparing photocatalysis glass self-cleaned coating - Google Patents
Method for preparing photocatalysis glass self-cleaned coating Download PDFInfo
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- CN106675238A CN106675238A CN201611135199.4A CN201611135199A CN106675238A CN 106675238 A CN106675238 A CN 106675238A CN 201611135199 A CN201611135199 A CN 201611135199A CN 106675238 A CN106675238 A CN 106675238A
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- Prior art keywords
- titanium dioxide
- nano titanium
- thinization
- glass self
- double
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- 239000011521 glass Substances 0.000 title claims abstract description 42
- 238000000576 coating method Methods 0.000 title claims abstract description 39
- 239000011248 coating agent Substances 0.000 title claims abstract description 38
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 20
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 18
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 8
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005642 Oleic acid Substances 0.000 claims abstract description 8
- 239000000839 emulsion Substances 0.000 claims abstract description 8
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 39
- 238000004140 cleaning Methods 0.000 claims description 22
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 19
- 235000010215 titanium dioxide Nutrition 0.000 claims description 19
- 238000001914 filtration Methods 0.000 claims description 17
- 239000003643 water by type Substances 0.000 claims description 17
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 6
- 238000010168 coupling process Methods 0.000 claims description 6
- 238000005859 coupling reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 6
- 239000002562 thickening agent Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 abstract description 9
- 231100000719 pollutant Toxicity 0.000 abstract description 9
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract 3
- 239000011593 sulfur Substances 0.000 abstract 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 abstract 1
- 239000006087 Silane Coupling Agent Substances 0.000 abstract 1
- 239000003463 adsorbent Substances 0.000 abstract 1
- 238000011109 contamination Methods 0.000 abstract 1
- 238000010336 energy treatment Methods 0.000 abstract 1
- 239000000413 hydrolysate Substances 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 abstract 1
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 239000004744 fabric Substances 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 230000003115 biocidal effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- MZZINWWGSYUHGU-UHFFFAOYSA-J ToTo-1 Chemical compound [I-].[I-].[I-].[I-].C12=CC=CC=C2C(C=C2N(C3=CC=CC=C3S2)C)=CC=[N+]1CCC[N+](C)(C)CCC[N+](C)(C)CCC[N+](C1=CC=CC=C11)=CC=C1C=C1N(C)C2=CC=CC=C2S1 MZZINWWGSYUHGU-UHFFFAOYSA-J 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical class [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000005348 self-cleaning glass Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon Alkane Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
- C09D5/1612—Non-macromolecular compounds
- C09D5/1618—Non-macromolecular compounds inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
- C09D5/1668—Vinyl-type polymers
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a method for preparing a photocatalysis glass self-cleaned coating, and belongs to the technical field of functional materials. The method comprises the following steps of: by taking cyclohexane, oleic acid and titanium tetraisopropoxide as raw materials to prepare hydrophobic nano titanium dioxide, generating active silanol from triethoxy-1H,1H,2H,2H-tridecafluoro-n-octylsilane in chloroform, performing inert low-surface energy treatment on the hydrophobic nano titanium dioxide so as to enable the hydrophobic nano titanium dioxide to have very low surface energy and very poor wettability, performing surface treatment on the double-sulfur treated modified titanium dioxide in absolute ethyl alcohol by using hydrolysate of a silane coupling agent A-186 so as to obtain modified double-sulfur nano titanium dioxide, finally dispersing the modified double-sulfur nano titanium dioxide into aqueous fluorocarbon emulsion resin, and adding other aids, uniformly mixing, thereby obtaining the photocatalysis glass self-cleaned coating. The photocatalysis glass self-cleaned coating prepared by using the method is good in filming property, good in adhesion to substrates, good in contamination resistance and free of phenomena such as ash adhesion or adsorbent oily pollutants.
Description
Technical field
The invention discloses a kind of preparation method of photocatalysis glass self-cleaning coating, belongs to the technology neck of functional material
Domain.
Background technology
Glass curtain wall is a kind of novel construction wall trailing attractive in appearance, is the notable spy in modern high-rise building epoch
Levy.The raising of progress and living standards of the people recently as society, glass curtain wall has at home and abroad been obtained widely should
With, and consumption is increasing, but its antifouling property is poor.
Self-cleaning glass coating is a kind of super-hydrophilic coating for being sprayed on glass surface, coated face and it is dirty between it is rapid
Form one layer of super hydrophilic moisture film, make dirty release-coated face, using nature rainwash, make it is dirty with moisture film gravity work
It is rinsed with, reaches self-cleaning purpose.Exploitation earliest starts from Japan, eighties of last century the mid-90, the east pottery of Japan
（TOTO）Company and Asahi Glass company are applied to glass surface using titanium dioxide optical catalyst.Develop at present variously-shaped
Tens of kinds of titania coatings.In addition to Japan, Pilkington building materials company of Britain and PPG companies of the U.S. also active development this
The TiO of one product, wherein MB Group Plc2Glass with clean exploitation marches at the forefront of the world.Scientific research institution of China is also positive
Research and development.
It is usually used in the titanium dioxide self-cleaning coating of glass surface at present, plating/painting layer of titanium dioxide thin film on glass
Afterwards, because titanium dioxide exists（Ultraviolet）Good photocatalysis characteristic can be produced in the presence of luminous energy and there is Superhydrophilic,
Using this super hydrophilic characteristic so that the water droplet of very little is converged to big water droplet, comes off under gravity, so that being stained with
Dye spot thereon can be readily washed away, makes glass have characteristic easy to clean, its low price, but must have purple
Outside line is irradiated, and poor with matrix adhesive force, easy to stick grey and absorption oiliness pollutant.
The content of the invention
The technical problem to be solved：It is necessary for the titanium dioxide self-cleaning coating currently used for glass surface
There is ultraviolet to irradiate, the defect of easy to stick ash and absorption oiliness pollutant poor with matrix adhesive force.The present invention is with hexamethylene, Oleic acid
Hydrophobic nano titanium dioxide is prepared for raw material with titanium tetraisopropylate, then tridecafluoro-n-octyltriethoxysilane is produced in chloroform
Raw activity silanol, to the process of hydrophobic nano titanium dioxide inertia low-surface-energy so as to extremely low surface energy and extreme difference
Wettability, then with the hydrolyzed solution of silane coupling A -186 to dehydrated alcohol in double thinization process modifying titanium dioxide surfaces
Process, must be modified double thinization nano titanium oxides, finally modified double thinization nano titanium oxides are dispersed in into water-base fluorocarbon emulsion
In resin, after adding other auxiliary agent mix homogeneously, photocatalysis glass self-cleaning coating is obtained.Coating film property prepared by the present invention
Good, strong with matrix adhesive force, anti-stain characteristic is good, occurs without viscous ash and absorption oiliness pollutant phenomenon.
To solve above-mentioned technical problem, the present invention is using technical scheme as described below：
（1）200~300mL hexamethylene is measured, 50~60mL Oleic acid, 30~50mL titanium tetraisopropylates add 300~400mL matter
Amount fraction is in 10% tert-butylamine aqueous solution, to be stirred after 20~30min with 300~400r/min, in proceeding to four-hole boiling flask, heating
To 170~190 DEG C, 3~5h of insulation reaction is cooled to 1~2h of standing after room temperature, collects upper oil phase and adds isopyknic ethanol
In, proceed to after mix homogeneously in centrifuge, with 5000~6000r/min, 3~5min of centrifugation, precipitation is collected, precipitation is put
In vacuum drying oven, 2~3h is dried at 70~80 DEG C, then is proceeded to crushing in pulverizer, cross 200 mesh sieves, obtain hydrophobic
Type nano titanium oxide；
（2）The above-mentioned hydrophobic nano titanium dioxide of 3~5g is weighed, it is in adding 120~240mL chloroforms and super with 300W ultrasound wave
Sound disperses 30~40min, 3~5mL tridecafluoro-n-octyltriethoxysilanes is added, under 40~50 DEG C of waters bath with thermostatic control, with 300
~400r/min stirs 10~12h, stands sucking filtration after 1~2h, and with chloroform filter cake 3~5 times, subsequently proceeds to filter cake dry
In dry case, 2~3h is dried at 70~80 DEG C, obtains double thinization and process modifying titanium dioxide；
（3）0.15~0.20g silane coupling As -186 are added in 4~5mL deionized waters, water is stirred with 300~400r/min
After 30~40min of solution, 300~320mL dehydrated alcohol is added, above-mentioned double the thinization process modifying titanium dioxides of 3~5g, 80~
Under 85 DEG C of waters bath with thermostatic control, continue to stir 30~35min, subsequently filter, and successively with dehydrated alcohol and deionized water wash filtering residue 3
~5 times, then filtering residue is placed in vacuum drying oven, it is dried to constant weight at 105~110 DEG C, must be modified double thinization nano-silicas
Change titanium；
（4）Count by weight, weigh 40~55 parts of water-base fluorocarbon emulsion resins, 3~5 parts of above-mentioned modified double thinization nano-silicas
Change titanium, 0.5~1.5 part of dispersant, 5040,20~40 parts of dehydrated alcohol, 1~2 part of 3030,0.5~1.5 part of polyurethane thickener
Levelling agent 440, is fitted into mix homogeneously in batch mixer, obtains photocatalysis glass self-cleaning coating.
The present invention application process be：First glass surface is rinsed with tap water, and wiped 1~3 time with ethanol cloth.Again with sea
It is continuous that photocatalysis glass self-cleaning coating obtained by the present invention is dipped in into full, glass surface is evenly applied to, controlling coating thickness is
0.3~0.5mm, stands 3~4min of solidification, is wiped vaporific vestige with dry and comfortable soft cloth.Jing inspections, the coating and matrix
Adhesive force is strong, ash not easy to stick and absorption oiliness pollutant, plays strength antibacterial and self-cleaning effect, antibiotic rate up to more than 99.2%,
Ultraviolet can be effectively absorbed simultaneously, the ageing resistance of coating is improved, and anti-stain characteristic is good, is reached using rear glass basal plane light transmittance
More than 90.8%.
Compared with additive method, Advantageous Effects are the present invention：
（1）The present invention prepares simple, gained coating good film-forming property, strong with matrix adhesive force, improves the antibiotic rate of glass, antibiotic rate
Up to more than 99.2%；
（2）Photocatalysis glass self-cleaning coating obtained by the present invention can effectively absorb ultraviolet, improve the ageing resistance of coating；
（3）Anti-stain characteristic is good, occurs without viscous ash and absorption oiliness pollutant phenomenon, improves the light transmittance of glass, and light transmittance reaches
More than 90.8%.
Specific embodiment
200~300mL hexamethylene is measured, 50~60mL Oleic acid, 30~50mL titanium tetraisopropylates add 300~400mL matter
Amount fraction is in 10% tert-butylamine aqueous solution, to be stirred after 20~30min with 300~400r/min, in proceeding to four-hole boiling flask, heating
To 170~190 DEG C, 3~5h of insulation reaction is cooled to 1~2h of standing after room temperature, collects upper oil phase and adds isopyknic ethanol
In, proceed to after mix homogeneously in centrifuge, with 5000~6000r/min, 3~5min of centrifugation, precipitation is collected, precipitation is put
In vacuum drying oven, 2~3h is dried at 70~80 DEG C, then is proceeded to crushing in pulverizer, cross 200 mesh sieves, obtain hydrophobic
Type nano titanium oxide；The above-mentioned hydrophobic nano titanium dioxide of 3~5g is weighed, in adding 120~240mL chloroforms, and with 300W
Ultrasonic echography disperses 30~40min, 3~5mL tridecafluoro-n-octyltriethoxysilanes is added, in 40~50 DEG C of waters bath with thermostatic control
Under, 10~12h is stirred with 300~400r/min, stand sucking filtration after 1~2h, and with chloroform filter cake 3~5 times, subsequently will filter
Cake is proceeded in drying baker, and 2~3h is dried at 70~80 DEG C, is obtained double thinization and is processed modifying titanium dioxide；By 0.15~0.20g silicon
Alkane coupling agent A-186 is added in 4~5mL deionized waters, is hydrolyzed after 30~40min with 300~400r/min stirrings, is added
300~320mL dehydrated alcohol, above-mentioned double thinization of 3~5g process modifying titanium dioxide, under 80~85 DEG C of waters bath with thermostatic control, continue
30~35min of stirring, subsequently filters, and successively with dehydrated alcohol and deionized water wash filtering residue 3~5 times, then filtering residue is placed in
In vacuum drying oven, it is dried to constant weight at 105~110 DEG C, must be modified double thinization nano titanium oxides；Count by weight,
Weigh 40~55 parts of water-base fluorocarbon emulsion resins, 3~5 parts of above-mentioned modified double thinization nano titanium oxides, 0.5~1.5 part of dispersion
5040,20~40 parts of dehydrated alcohol of agent, 1~2 part of polyurethane thickener, 3030,0.5~1.5 part of levelling agent 440 loads batch mixer
Middle mix homogeneously, obtains photocatalysis glass self-cleaning coating.
Example 1
200mL hexamethylene is measured, 50mL Oleic acid, 30mL titanium tetraisopropylates add 300mL mass fractions to be that 10% tert-butylamine is water-soluble
In liquid, stirred after 20min with 300r/min, in proceeding to four-hole boiling flask, be heated to 170 DEG C, insulation reaction 3h, after being cooled to room temperature
1h is stood, upper oil phase is collected and is added in isopyknic ethanol, proceeded to after mix homogeneously in centrifuge, with 5000r/min centrifugations
3min is separated, precipitation is collected, precipitation is placed in vacuum drying oven, 2h is dried at 70 DEG C, then proceeded to powder in pulverizer
It is broken, 200 mesh sieves are crossed, obtain hydrophobic nano titanium dioxide；The above-mentioned hydrophobic nano titanium dioxide of 3g is weighed, 120mL chloroforms are added
In, and 30min is disperseed with 300W ultrasonic echographies, 3mL tridecafluoro-n-octyltriethoxysilanes are added, in 40 DEG C of waters bath with thermostatic control
Under, 10h is stirred with 300r/min, sucking filtration after 1h is stood, and with chloroform filter cake 3 times, subsequently filter cake is proceeded in drying baker,
2h is dried at 70 DEG C, double thinization is obtained and is processed modifying titanium dioxide；0.15g silane coupling As -186 are added into 4mL deionized waters
In, hydrolyzed after 30min with 300r/min stirrings, 300mL dehydrated alcohol is added, above-mentioned double thinization of 3g process modified titanium dioxide
Titanium, under 80 DEG C of waters bath with thermostatic control, continues to stir 30min, subsequently filters, and successively with dehydrated alcohol and deionized water wash filtering residue
3 times, then filtering residue is placed in vacuum drying oven, it is dried to constant weight at 105 DEG C, must be modified double thinization nano titanium oxides；Press
Parts by weight meter, weighs 40 parts of water-base fluorocarbon emulsion resins, 3 parts of above-mentioned modified double thinization nano titanium oxides, 0.5 part of dispersant
5040,20 parts of dehydrated alcohol, 1 part of polyurethane thickener, 3030,0.5 part of levelling agent 440, are fitted into mix homogeneously in batch mixer, obtain
Photocatalysis glass self-cleaning coating.
The present invention application process be：First glass surface is rinsed with tap water, and wiped 1 time with ethanol cloth.Sponge is used again
Photocatalysis glass self-cleaning coating obtained by the present invention is dipped in into full, glass surface is evenly applied to, controlling coating thickness is
0.3mm, stands solidification 3min, is wiped vaporific vestige with dry and comfortable soft cloth.Jing inspections, the coating and matrix adhesive force
By force, it is not easy to stick ash and absorption oiliness pollutant, play strength antibacterial and self-cleaning effect, antibiotic rate up to 99.3%, while can be effective
Ultraviolet is absorbed, the ageing resistance of coating is improved, anti-stain characteristic is good, using rear glass basal plane light transmittance up to 90.9%.
Example 2
300mL hexamethylene is measured, 60mL Oleic acid, 50mL titanium tetraisopropylates add 400mL mass fractions to be that 10% tert-butylamine is water-soluble
In liquid, stirred after 30min with 400r/min, in proceeding to four-hole boiling flask, be heated to 190 DEG C, insulation reaction 5h, after being cooled to room temperature
2h is stood, upper oil phase is collected and is added in isopyknic ethanol, proceeded to after mix homogeneously in centrifuge, with 6000r/min centrifugations
5min is separated, precipitation is collected, precipitation is placed in vacuum drying oven, 3h is dried at 80 DEG C, then proceeded to powder in pulverizer
It is broken, 200 mesh sieves are crossed, obtain hydrophobic nano titanium dioxide；The above-mentioned hydrophobic nano titanium dioxide of 5g is weighed, 240mL chloroforms are added
In, and 40min is disperseed with 300W ultrasonic echographies, 5mL tridecafluoro-n-octyltriethoxysilanes are added, in 50 DEG C of waters bath with thermostatic control
Under, 12h is stirred with 400r/min, sucking filtration after 2h is stood, and with chloroform filter cake 5 times, subsequently filter cake is proceeded in drying baker,
3h is dried at 80 DEG C, double thinization is obtained and is processed modifying titanium dioxide；0.20g silane coupling As -186 are added into 5mL deionized waters
In, hydrolyzed after 40min with 300~400r/min stirrings, 320mL dehydrated alcohol is added, above-mentioned double thinization of 5g process modified two
Titanium oxide, under 85 DEG C of waters bath with thermostatic control, continues to stir 35min, subsequently filters, and successively with dehydrated alcohol and deionized water wash
Filtering residue 5 times, then filtering residue is placed in vacuum drying oven, it is dried to constant weight at 110 DEG C, must be modified double thinization nanometer titanium dioxides
Titanium；Count by weight, weigh 55 parts of water-base fluorocarbon emulsion resins, 5 parts of above-mentioned modified double thinization nano titanium oxides, 1.5 parts
5040,40 parts of dehydrated alcohol of dispersant, 2 parts of polyurethane thickeners, 3030,1.5 parts of levelling agents 440 are fitted in batch mixer and mix equal
It is even, obtain photocatalysis glass self-cleaning coating.
The present invention application process be：First glass surface is rinsed with tap water, and wiped 3 times with ethanol cloth.Sponge is used again
Photocatalysis glass self-cleaning coating obtained by the present invention is dipped in into full, glass surface is evenly applied to, controlling coating thickness is
0.5mm, stands solidification 4min, is wiped vaporific vestige with dry and comfortable soft cloth.Jing inspections, the coating and matrix adhesive force
By force, it is not easy to stick ash and absorption oiliness pollutant, play strength antibacterial and self-cleaning effect, antibiotic rate up to 99.8%, while can be effective
Ultraviolet is absorbed, the ageing resistance of coating is improved, anti-stain characteristic is good, using rear glass basal plane light transmittance up to 91.2%.
Example 3
250mL hexamethylene is measured, 55mL Oleic acid, 40mL titanium tetraisopropylates add 350mL mass fractions to be that 10% tert-butylamine is water-soluble
In liquid, stirred after 25min with 350r/min, in proceeding to four-hole boiling flask, be heated to 180 DEG C, insulation reaction 4h, after being cooled to room temperature
Stand 1.5h, collect upper oil phase and add in isopyknic ethanol, proceed to after mix homogeneously in centrifuge, with 5500r/min from
The heart separates 4min, collects precipitation, and precipitation is placed in vacuum drying oven, and 2.5h is dried at 75 DEG C, then is proceeded to pulverizer
Middle crushing, crosses 200 mesh sieves, obtains hydrophobic nano titanium dioxide；The above-mentioned hydrophobic nano titanium dioxide of 4g is weighed, 180mL is added
In chloroform, and 35min is disperseed with 300W ultrasonic echographies, 4mL tridecafluoro-n-octyltriethoxysilanes are added, in 45 DEG C of constant temperature
Under water-bath, 11h is stirred with 350r/min, stand sucking filtration after 1.5h, and with chloroform filter cake 4 times, subsequently proceeded to filter cake dry
In dry case, 2.5h is dried at 75 DEG C, obtains double thinization and process modifying titanium dioxide；0.175g silane coupling As -186 are added
In 4.5mL deionized waters, hydrolyzed after 35min with 350r/min stirrings, add 310mL dehydrated alcohol, the above-mentioned double thinization places of 4g
Reason modifying titanium dioxide, under 82.5 DEG C of waters bath with thermostatic control, continues to stir 32.5min, subsequently filters, and successively with dehydrated alcohol and
Deionized water wash filtering residue 4 times, then filtering residue is placed in vacuum drying oven, it is dried to constant weight at 107.5 DEG C, must be modified double dredging
Change nano titanium oxide；Count by weight, weigh 47.5 parts of water-base fluorocarbon emulsion resins, 4 parts of above-mentioned modified double thinization nanometers
Titanium dioxide, 1 part of dispersant, 5040,30 parts of dehydrated alcohol, 1.5 parts of polyurethane thickeners, 3030,1 part of levelling agent 440 loads mixed
Mix homogeneously in material machine, obtains photocatalysis glass self-cleaning coating.
The present invention application process be：First glass surface is rinsed with tap water, and wiped 2 times with ethanol cloth.Sponge is used again
Photocatalysis glass self-cleaning coating obtained by the present invention is dipped in into full, glass surface is evenly applied to, controlling coating thickness is
0.4mm, stands solidification 3.5min, is wiped vaporific vestige with dry and comfortable soft cloth.Jing inspections, the coating and matrix adhesive force
By force, it is not easy to stick ash and absorption oiliness pollutant, play strength antibacterial and self-cleaning effect, antibiotic rate up to 99.5%, while can be effective
Ultraviolet is absorbed, the ageing resistance of coating is improved, anti-stain characteristic is good, using rear glass basal plane light transmittance up to 91.5%.
Claims (1)
1. a kind of preparation method of photocatalysis glass self-cleaning coating, it is characterised in that concrete preparation process is：
（1）200 ~ 300mL hexamethylene is measured, 50 ~ 60mL Oleic acid, 30 ~ 50mL titanium tetraisopropylates add 300 ~ 400mL mass point
Number in 10% tert-butylamine aqueous solution, to be stirred after 20 ~ 30min with 300 ~ 400r/min, in proceeding to four-hole boiling flask, be heated to 170 ~
190 DEG C, 3 ~ 5h of insulation reaction is cooled to 1 ~ 2h of standing after room temperature, collects upper oil phase and adds in isopyknic ethanol, and mixing is equal
Proceed to after even in centrifuge, with 5000 ~ 6000r/min, 3 ~ 5min of centrifugation, collect precipitation, precipitation is placed in into vacuum drying oven
In, 2 ~ 3h is dried at 70 ~ 80 DEG C, then crushing in pulverizer is proceeded to, 200 mesh sieves are crossed, obtain hydrophobic nano titanium dioxide；
（2）The above-mentioned hydrophobic nano titanium dioxide of 3 ~ 5g is weighed, in adding 120~240mL chloroforms, and with 300W ultrasonic echographies
30~40min of dispersion, adds 3 ~ 5mL tridecafluoro-n-octyltriethoxysilanes, under 40~50 DEG C of waters bath with thermostatic control, with 300~
400r/min stirs 10~12h, stands sucking filtration after 1~2h, and with chloroform filter cake 3~5 times, subsequently filter cake is proceeded to into drying
In case, 2 ~ 3h is dried at 70 ~ 80 DEG C, obtains double thinization and process modifying titanium dioxide；
（3）0.15 ~ 0.20g silane coupling As -186 are added in 4 ~ 5mL deionized waters, is hydrolyzed with 300 ~ 400r/min stirrings
After 30 ~ 40min, 300 ~ 320mL dehydrated alcohol, the above-mentioned hydrophobic nano titanium dioxide of 3 ~ 5g, in 80 ~ 85 DEG C of thermostatted waters are added
Under bath, continue to stir 30 ~ 35min, subsequently filter, and successively with dehydrated alcohol and deionized water wash filtering residue 3 ~ 5 times, then will filter
Slag is placed in vacuum drying oven, is dried to constant weight at 105 ~ 110 DEG C, and must be modified double thinization nano titanium oxides；
（4）Count by weight, weigh 40 ~ 55 parts of water-base fluorocarbon emulsion resins, 3 ~ 5 parts of above-mentioned modified double thinization nanometer titanium dioxides
Titanium, 0.5 ~ 1.5 part of dispersant, 5040,20 ~ 40 parts of dehydrated alcohol, 1~2 part of polyurethane thickener, 3030,0.5 ~ 1.5 part of levelling agent
440, it is fitted into mix homogeneously in batch mixer, obtain photocatalysis glass self-cleaning coating.
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