CN107417132A - A kind of preparation method of the antifouling antifog film of glass - Google Patents
A kind of preparation method of the antifouling antifog film of glass Download PDFInfo
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- CN107417132A CN107417132A CN201710424445.6A CN201710424445A CN107417132A CN 107417132 A CN107417132 A CN 107417132A CN 201710424445 A CN201710424445 A CN 201710424445A CN 107417132 A CN107417132 A CN 107417132A
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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
- 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
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—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 an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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
- C09D5/1625—Non-macromolecular compounds organic
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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
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
- C09D5/1675—Polyorganosiloxane-containing compositions
-
- 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
- C09D5/1687—Use of special additives
-
- 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
- C03C2217/73—Anti-reflective coatings with specific characteristics
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/114—Deposition methods from solutions or suspensions by brushing, pouring or doctorblading
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
Abstract
A kind of preparation method the present invention relates to glass with antifouling antifog film, belongs to glass-film preparing technical field.The present invention is using donaxine as anti-fouling agent, after silane coupler modified modified nano titanium oxide compounding is dredged with double, and it is embedded in polystyrene microsphere, the compounded mix of the sustainable antifouling anti-fog particles of release is made, finally it is stirred with materials such as VTES, tetraethyl orthosilicates after mixing and coating liquid smearing is made on the glass substrate, the antifouling antifog film of persistent form glass is made.The antifouling antifog time length of the present invention, effect is good, can be widely applied to a variety of matrix surfaces such as vehicle glass.
Description
Technical field
A kind of preparation method the present invention relates to glass with antifouling antifog film, belongs to glass-film preparing technical field.
Background technology
Transparent material（Such as glass, plastics）It is people's daily life, work, produces indispensable material.However, work as it
There is certain temperature difference in both sides spaced apart from each other, and steam is just assembled to body surface, form small dewdrop and form diffusion to light,
So as to significantly reduce the light transmittance of glass.Such as in cold winter because windshield surface fogging can largely effect on energy
The probability of traffic accident occurs for degree of opinion, increase；In the summer swimming of sweltering heat, the contact lens of wearing are due to the condensation of vapor
Would generally be in eyeglass upper fogging, just as " looking at flowers in a fog ".Fogging problem brings inconvenience to the work and life of people, therefore
Huge Social benefit and economic benefit will be brought by developing the antifog application product of glass surface, with important theory and in fact
Border meaning.
Antifog glass is divided into coating antifog glass, Electrothermic fog prevention glass and nano combined antifog.It is wherein nano combined antifog
Glass is mutually firmly combined together with glass using physics and chemistry using nano-glass antifog film, treated glass
Surface has hydrophile function, because water can not form the globule in substrate surface, but forms uniform moisture film, antifog so as to reach
Effect.
Nano-glass antifog film can be divided into hydrophily, water imbibition and hydrophobicity antifog film again by hydrophilic and hydrophobic point, wherein parent
There is easily absorption inorganic dirt in water-based antifog film, it is difficult to maintain hydrophily for a long time so that its antifog duration is shorter
The shortcomings that, there is the shortcomings that losing anti-fog function after water absorption saturation in water imbibition antifog film, hydrophobicity antifog film requires that diameter exists
Below 1mm water droplet can also slide.Therefore, developing a kind of antifouling antifog film for possessing long-term effect is highly desirable.
The content of the invention
The technical problems to be solved by the invention：Inorganic dirt is easily adsorbed for traditional hydrophilic antifogging film, it is difficult to long
Phase maintains hydrophily, and anti-fog duration is shorter, and water imbibition antifog film loses anti-fog function after water absorption saturation being present,
A kind of preparation method the invention provides glass with antifouling antifog film.
To solve technical problem, the technical solution adopted by the present invention is：
（1）Take reed catkins alkali and Silane coupling reagent KH-570 to add and 15~20h stirred in absolute ethyl alcohol, be centrifuged rear alcohol wash it is dry
It is dry, obtain modified donaxine；
（2）Hexamethylene, leukotrienes and titanium tetraisopropylate are taken, it is to be well mixed in the 10% tert-butylamine aqueous solution to add mass fraction, and
3~5h of insulation reaction at 180~200 DEG C, upper oil phase is collected after standing 1~2h, is dried after upper oil phase alcohol precipitation is centrifuged,
Obtain hydrophobic nano titanium dioxide；
（3）Hydrophobic nano titanium dioxide is scattered in chloroform, adds tridecafluoro-n-octyltriethoxysilane, 40~50
10~12h is stirred at DEG C, filtration washing is dried after standing 1~2h, obtains double thinization processing modifying titanium dioxides；
（4）Will modified donaxine, double thinization processing modifying titanium dioxide, styrene, divinylbenzene, azo-bis-isobutyl cyanide and ten
40~50 DEG C are heated to after six alkane are well mixed, 1~2h of insulation reaction, adds dodecyl sodium sulfate, polyvinyl alcohol, emulsification
Agent OP-10 and deionized water, 80~90 DEG C are heated under nitrogen protection, is filtered after 5~6h of stirring reaction, obtains compounded mix；
（5）VTES, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are fitted into reactor, 30~
1~2h of stirring reaction under 40 DEG C of waters bath with thermostatic control, mass fraction is added as 20% Ludox, sodium sulfosuccinate dioctyl ester and is answered
Filler is closed, 1~2h of stirring reaction, obtains coating liquid under 40~50 DEG C of waters bath with thermostatic control；（6）Coating liquid is applied to glass substrate
On, it is 0.1~0.5mm to control smearing thickness, and is dried up with nitrogen, then the glass substrate after film is placed in drying box,
30~40min is dried at 105~110 DEG C, room temperature is naturally cooled to, obtains glass with antifouling antifog film.
The step（1）In reed catkins alkali and Silane coupling reagent KH-570 mass ratio be 1.5：1~3.0：1.
The step（2）In hexamethylene, leukotrienes, the parts by volume of titanium tetraisopropylate and the tert-butylamine aqueous solution for 200~
300 parts of hexamethylenes, 60~80 parts of leukotrienes, 30~50 parts of titanium tetraisopropylates, 300~400 parts of mass fractions are 10% tert-butylamine water
Solution.
The step（3）In tridecafluoro-n-octyltriethoxysilane for hydrophobic nano titanium dioxide quality 0.5~
2.5 again.
The step（4）In modification donaxine, double thinization processing modifying titanium dioxide, styrene, divinylbenzene, idol
The isobutyl cyanogen of nitrogen two, hexadecane, dodecyl sodium sulfate, polyvinyl alcohol, the parts by weight of emulsifier op-10 and deionized water are 1~2
The modified donaxine of part, 1~2 part of double thinization processing modifying titanium dioxide, 10~20 parts of styrene, 0.5~1.0 part of divinyl
Benzene, 0.1~0.2 part of azo-bis-isobutyl cyanide, 0.1~0.2 part of hexadecane, 0.05~0.10 part of dodecyl sodium sulfate, 0.2~
0.4 part of polyvinyl alcohol, 1~2 part of emulsifier op-10 and 40~80 parts of deionized waters.
The step（5）In VTES, tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, silicon it is molten
The parts by weight of glue, sodium sulfosuccinate dioctyl ester and compounded mix are 10~20 parts of VTESs, 11~22 parts
Tetraethyl orthosilicate, 45~90 parts of absolute ethyl alcohols, 4~8 parts of deionized waters, 30~50 parts of mass fractions are 20% Ludox, 3~4 parts
Sodium sulfosuccinate dioctyl ester and 2~3 parts of compounded mixs.
The method have the benefit that：
The present invention compounds using donaxine as anti-fouling agent after silane coupler modified with double nano titanium oxides for dredging modification, and
By mini-emulsion polymerization method, reed catkins alkali is embedded in double polystyrene microspheres for dredging crosslinking, finally with the ethoxy of vinyl three
Coating liquid smearing is made on the glass substrate after being stirred mixing in the materials such as base silane, tetraethyl orthosilicate, and double thinization films are made
Layer, the present invention the antifouling anti-fog particles of sustained release, are extended antifouling by the sustained release performance of the polystyrene microsphere in compounded mix
The antifog time, it can be widely applied to a variety of matrix surfaces such as vehicle glass.
Embodiment
3.0~4.5g donaxines are weighed, 1.5~2.0g Silane coupling reagent KH-570s, add 100~200mL absolute ethyl alcohols
In, 15~20h is stirred with 300~400r/min, mixed liquor is obtained, mixed liquor is fitted into centrifuge and centrifuged, must precipitate, is used
Absolute ethyl alcohol washing precipitation 3~5 times, then the precipitation after washing is placed in drying box, 3~4h is dried at 60~70 DEG C, is obtained
Modified donaxine, measures 200~300mL hexamethylenes, 60~80mL leukotrienes, 30~50mL titanium tetraisopropylates, add 300~
400mL mass fractions are in the 10% tert-butylamine aqueous solution, stir 20~30min with 300~400r/min, material liquid are obtained, by raw material
Liquid is fitted into reactor, at 180~200 DEG C, 3~5h of insulation reaction, 1~2h is stood after being cooled to room temperature, collects upper strata oil
Phase, isometric absolute ethyl alcohol is added into upper oil phase, 3~5min of centrifugation in centrifuge is transferred to after well mixed, is obtained
Sediment, put the precipitate in vacuum drying chamber, 2~3h is dried at 70~80 DEG C, obtains hydrophobic nano titanium dioxide, claim
3~5g hydrophobic nano titanium dioxide is taken, is added in 120~240mL chloroforms, 30~40min is disperseed with 300W ultrasonic echographies,
3~5mL tridecafluoro-n-octyltriethoxysilanes are added, under 40~50 DEG C of waters bath with thermostatic control, 10 are stirred with 300~400r/min
~12h, filtered after standing 1~2h, obtain filter cake, be transferred to chloroform filter cake 3~5 times, then by filter cake in drying box, 70~
2~3h is dried at 80 DEG C, obtains double thinization processing modifying titanium dioxides, takes 1~2g to be modified donaxine, the double thinization processing of 1~2g change
Property titanium dioxide, 10~20g styrene, 0.5~1.0g divinylbenzenes, 0.1~0.2g azo-bis-isobutyl cyanides, 0.1~0.2g
Hexadecane is fitted into flask, stirs 20~30min with 300~400r/min, is again heated to 40~50 DEG C, 1~2h of insulation reaction,
Reaction solution is obtained, 0.05~0.10g dodecyl sodium sulfates, 0.2~0.4g polyvinyl alcohol, 1~2g emulsifications are added into reaction solution
Agent OP-10,40~80mL deionized water, 30~50min is stirred with 600~800r/min, then be heated to 80 under nitrogen protection
~90 DEG C, continue 5~6h of stirring reaction, filtered after being cooled to room temperature, obtain filter residue, obtain compounded mix, take 10~20g vinyl three
Ethoxysilane, 11~22g tetraethyl orthosilicates, 45~90g absolute ethyl alcohols, 4~8mL deionized waters are fitted into reactor, 30
Under~40 DEG C of waters bath with thermostatic control, with 300~400r/min, 1~2h of stirring reaction, it is molten for 20% silicon to add 30~50g mass fractions
Glue, 3~4g sodium sulfosuccinate dioctyl esters, 2~3g compounded mixs, under 40~50 DEG C of waters bath with thermostatic control, with 400~500r/min
1~2h of stirring reaction, obtains coating liquid, and coating liquid is uniformly smeared on the glass substrate, control smearing thickness be 0.1~
0.5mm, and dried up with nitrogen, then the glass substrate after film is placed in drying box, dry 30 at 105~110 DEG C~
40min, room temperature is naturally cooled to, obtain glass with antifouling antifog film.
Example 1
3.0g donaxines are weighed, 1.5g Silane coupling reagent KH-570s, adds in 100mL absolute ethyl alcohols, is stirred with 300r/min
15h, mixed liquor is obtained, mixed liquor is fitted into centrifuge and centrifuged, must precipitated, wash precipitation 3 times with absolute ethyl alcohol, then will wash
Precipitation after washing is placed in drying box, and 3h is dried at 60 DEG C, modified donaxine is obtained, measures 200mL hexamethylenes, 60mL flax
Acid, 30mL titanium tetraisopropylates, adding 300mL mass fractions is in the 10% tert-butylamine aqueous solution, with 300r/min stirrings 20~
30min, material liquid is obtained, material liquid is fitted into reactor, at 180 DEG C, insulation reaction 3h, 1h is stood after being cooled to room temperature,
Upper oil phase is collected, isometric absolute ethyl alcohol is added into upper oil phase, is transferred in centrifuge and centrifuges after well mixed
3min, sediment is obtained, put the precipitate in vacuum drying chamber, 2h is dried at 70 DEG C, obtains hydrophobic nano titanium dioxide, claimed
3g hydrophobic nano titanium dioxide is taken, is added in 120mL chloroforms, 30min is disperseed with 300W ultrasonic echographies, adds 3mL ten
Trifluoro octyltri-ethoxysilane, under 40 DEG C of water bath with thermostatic control, 10h is stirred with 300r/min, is filtered after standing 1h, obtains filter cake,
It is transferred to chloroform filter cake 3 times, then by filter cake in drying box, 2h is dried at 70 DEG C, double thinization is obtained and handles modification titanium dioxides
Titanium, 1g is taken to be modified donaxine, the double thinization processing modifying titanium dioxides of 1g, 10g styrene, 0.5g divinylbenzenes, 0.1g azos
Two isobutyl cyanogen, 0.1g hexadecanes are fitted into flask, stir 20min with 300r/min, are again heated to 40 DEG C, insulation reaction 1h, obtain
Reaction solution, into reaction solution add 0.05g dodecyl sodium sulfates, 0.2g polyvinyl alcohol, 1g emulsifier op-10s, 40mL go from
Sub- water, 30min is stirred with 600r/min, then be heated to 80 DEG C under nitrogen protection, continue stirring reaction 5h, after being cooled to room temperature
Filtering, obtains filter residue, obtains compounded mix, take 10g VTESs, 11g tetraethyl orthosilicates, 45g absolute ethyl alcohols, 4mL
Deionized water is fitted into reactor, under 30 DEG C of waters bath with thermostatic control, with 300r/min stirring reaction 1h, adds 30g mass fractions
It is anti-with 400r/min stirrings under 40 DEG C of waters bath with thermostatic control for 20% Ludox, 3g sodium sulfosuccinate dioctyl esters, 2g compounded mixs
1h is answered, obtains coating liquid, coating liquid is uniformly smeared on the glass substrate, it is 0.1mm to control smearing thickness, and is dried up with nitrogen,
The glass substrate after film is placed in drying box again, 30min is dried at 105 DEG C, naturally cools to room temperature, glass is obtained and uses and prevent
Dirty antifog film.
Example 2
3.8g donaxines are weighed, 1.8g Silane coupling reagent KH-570s, adds in 150mL absolute ethyl alcohols, is stirred with 350r/min
18h, mixed liquor is obtained, mixed liquor is fitted into centrifuge and centrifuged, must precipitated, wash precipitation 4 times with absolute ethyl alcohol, then will wash
Precipitation after washing is placed in drying box, and 3h is dried at 65 DEG C, modified donaxine is obtained, measures 250mL hexamethylenes, 70mL flax
Acid, 40mL titanium tetraisopropylates, it is in the 10% tert-butylamine aqueous solution to add 350mL mass fractions, stirs 25min with 350r/min, obtains
Material liquid, material liquid is fitted into reactor, at 190 DEG C, insulation reaction 4h, stands 1h after being cooled to room temperature, collect upper strata
Oil phase, isometric absolute ethyl alcohol is added into upper oil phase, be transferred to after well mixed in centrifuge and centrifuge 4min, it is heavy to obtain
Starch, put the precipitate in vacuum drying chamber, 2h is dried at 75 DEG C, hydrophobic nano titanium dioxide is obtained, it is hydrophobic to weigh 4g
Type nano titanium oxide, add in 180mL chloroforms, 35min is disperseed with 300W ultrasonic echographies, adds the trifluoro octyl groups of 4mL ten
Triethoxysilane, under 45 DEG C of waters bath with thermostatic control, 11h is stirred with 350r/min, is filtered after standing 1h, is obtained filter cake, washed with chloroform
Wash filter cake 4 times, then filter cake is transferred in drying box, 2h is dried at 75 DEG C, obtain double thinization processing modifying titanium dioxides, take 1g to change
Property donaxine, double thinization of 1g handle modifying titanium dioxides, 15g styrene, 0.8g divinylbenzenes, 0.1g azo-bis-isobutyl cyanides,
0.1g hexadecanes are fitted into flask, stir 25min with 350r/min, are again heated to 45 DEG C, insulation reaction 1h, obtain reaction solution, to
Addition 0.08g dodecyl sodium sulfates in reaction solution, 0.3g polyvinyl alcohol, 1g emulsifier op-10s, 60mL deionized waters, with
700r/min stirs 40min, then is heated to 85 DEG C under nitrogen protection, continues stirring reaction 5h, filters, obtain after being cooled to room temperature
Filter residue, compounded mix is obtained, take 15g VTESs, 16g tetraethyl orthosilicates, 68g absolute ethyl alcohols, 6mL deionized waters
It is fitted into reactor, under 35 DEG C of waters bath with thermostatic control, with 350r/min stirring reaction 1h, it is molten for 20% silicon adds 40g mass fractions
Glue, 3g sodium sulfosuccinate dioctyl esters, 2g compounded mixs, under 45 DEG C of waters bath with thermostatic control, with 450r/min stirring reaction 1h, it must apply
Film liquid, coating liquid is uniformly smeared on the glass substrate, it is 0.3mm to control smearing thickness, and is dried up with nitrogen, then by film
Glass substrate afterwards is placed in drying box, and 35min is dried at 108 DEG C, naturally cools to room temperature, obtains glass with antifouling antifog
Film.
Example 3
4.5g donaxines are weighed, 2.0g Silane coupling reagent KH-570s, adds in 200mL absolute ethyl alcohols, is stirred with 400r/min
20h, mixed liquor is obtained, mixed liquor is fitted into centrifuge and centrifuged, must precipitated, wash precipitation 5 times with absolute ethyl alcohol, then will wash
Precipitation after washing is placed in drying box, and 4h is dried at 70 DEG C, modified donaxine is obtained, measures 300mL hexamethylenes, 80mL flax
Acid, 50mL titanium tetraisopropylates, it is in the 10% tert-butylamine aqueous solution to add 400mL mass fractions, stirs 30min with 400r/min, obtains
Material liquid, material liquid is fitted into reactor, at 200 DEG C, insulation reaction 5h, stands 2h after being cooled to room temperature, collect upper strata
Oil phase, isometric absolute ethyl alcohol is added into upper oil phase, be transferred to after well mixed in centrifuge and centrifuge 5min, it is heavy to obtain
Starch, put the precipitate in vacuum drying chamber, 3h is dried at 80 DEG C, hydrophobic nano titanium dioxide is obtained, it is hydrophobic to weigh 5g
Type nano titanium oxide, add in 240mL chloroforms, 40min is disperseed with 300W ultrasonic echographies, adds the trifluoro octyl groups of 5mL ten
Triethoxysilane, under 50 DEG C of waters bath with thermostatic control, 12h is stirred with 400r/min, is filtered after standing 2h, is obtained filter cake, washed with chloroform
Wash filter cake 5 times, then filter cake is transferred in drying box, 3h is dried at 80 DEG C, obtain double thinization processing modifying titanium dioxides, take 2g to change
Property donaxine, double thinization of 2g handle modifying titanium dioxides, 20g styrene, 1.0g divinylbenzenes, 0.2g azo-bis-isobutyl cyanides,
0.2g hexadecanes are fitted into flask, stir 30min with 400r/min, are again heated to 50 DEG C, insulation reaction 2h, obtain reaction solution, to
Addition 0.10g dodecyl sodium sulfates in reaction solution, 0.4g polyvinyl alcohol, 2g emulsifier op-10s, 80mL deionized waters, with
800r/min stirs 50min, then is heated to 90 DEG C under nitrogen protection, continues stirring reaction 6h, filters, obtain after being cooled to room temperature
Filter residue, compounded mix is obtained, take 20g VTESs, 22g tetraethyl orthosilicates, 90g absolute ethyl alcohols, 8mL deionized waters
It is fitted into reactor, under 40 DEG C of waters bath with thermostatic control, with 400r/min stirring reaction 2h, it is molten for 20% silicon adds 50g mass fractions
Glue, 4g sodium sulfosuccinate dioctyl esters, 3g compounded mixs, under 50 DEG C of waters bath with thermostatic control, with 500r/min stirring reaction 2h, it must apply
Film liquid, coating liquid is uniformly smeared on the glass substrate, it is 0.5mm to control smearing thickness, and is dried up with nitrogen, then by film
Glass substrate afterwards is placed in drying box, and 40min is dried at 110 DEG C, naturally cools to room temperature, obtains glass with antifouling antifog
Film.
To glass made from example 1~3 antifouling antifog film and commercially available nano combined antifog film（Comparative example）Carry out performance
Detection, its testing result such as table 1 below：
Table 1
In summary, antifog antifog film produced by the present invention has good antifog, anti-reflection effect, while antifog film anti-pollution characteristic
Preferably, it is connected firmly with base material, close structure, there is the anti-fog performance of lasting stability, can effectively extend base material service life.
Claims (6)
1. a kind of glass preparation method of antifouling antifog film, it is characterised in that specifically preparation process is：
（1）Take reed catkins alkali and Silane coupling reagent KH-570 to add and 15~20h stirred in absolute ethyl alcohol, be centrifuged rear alcohol wash it is dry
It is dry, obtain modified donaxine；
（2）Hexamethylene, leukotrienes and titanium tetraisopropylate are taken, it is to be well mixed in the 10% tert-butylamine aqueous solution to add mass fraction, and
3~5h of insulation reaction at 180~200 DEG C, upper oil phase is collected after standing 1~2h, is dried after upper oil phase alcohol precipitation is centrifuged,
Obtain hydrophobic nano titanium dioxide；
（3）Hydrophobic nano titanium dioxide is scattered in chloroform, adds tridecafluoro-n-octyltriethoxysilane, 40~50
10~12h is stirred at DEG C, filtration washing is dried after standing 1~2h, obtains double thinization processing modifying titanium dioxides；
（4）Will modified donaxine, double thinization processing modifying titanium dioxide, styrene, divinylbenzene, azo-bis-isobutyl cyanide and ten
40~50 DEG C are heated to after six alkane are well mixed, 1~2h of insulation reaction, adds dodecyl sodium sulfate, polyvinyl alcohol, emulsification
Agent OP-10 and deionized water, 80~90 DEG C are heated under nitrogen protection, is filtered after 5~6h of stirring reaction, obtains compounded mix；
（5）VTES, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are fitted into reactor, 30~
1~2h of stirring reaction under 40 DEG C of waters bath with thermostatic control, mass fraction is added as 20% Ludox, sodium sulfosuccinate dioctyl ester and is answered
Filler is closed, 1~2h of stirring reaction, obtains coating liquid under 40~50 DEG C of waters bath with thermostatic control；
（6）Coating liquid is smeared on the glass substrate, it is 0.1~0.5mm to control smearing thickness, and is dried up with nitrogen, then will be applied
Glass substrate after film is placed in drying box, and 30~40min is dried at 105~110 DEG C, room temperature is naturally cooled to, obtains glass
With antifouling antifog film.
A kind of 2. preparation method of the antifouling antifog film of glass as claimed in claim 1, it is characterised in that the step（1）
In reed catkins alkali and Silane coupling reagent KH-570 mass ratio be 1.5：1~3.0：1.
A kind of 3. preparation method of the antifouling antifog film of glass as claimed in claim 1, it is characterised in that the step（2）
In hexamethylene, leukotrienes, the parts by volume of titanium tetraisopropylate and the tert-butylamine aqueous solution be 200~300 parts of hexamethylenes, 60~80 parts
Leukotrienes, 30~50 parts of titanium tetraisopropylates, 300~400 parts of mass fractions are the 10% tert-butylamine aqueous solution.
A kind of 4. preparation method of the antifouling antifog film of glass as claimed in claim 1, it is characterised in that the step（3）
In tridecafluoro-n-octyltriethoxysilane be 0.5~2.5 times of hydrophobic nano titanium dioxide quality.
A kind of 5. preparation method of the antifouling antifog film of glass as claimed in claim 1, it is characterised in that the step（4）
In modification donaxine, double thinization processing modifying titanium dioxide, styrene, divinylbenzene, azo-bis-isobutyl cyanide, hexadecane,
Dodecyl sodium sulfate, polyvinyl alcohol, the parts by weight of emulsifier op-10 and deionized water are 1~2 part of modified donaxine, 1~2
The double thinization processing modifying titanium dioxides of part, 10~20 parts of styrene, 0.5~1.0 part of divinylbenzene, 0.1~0.2 part of azo two
Isobutyl cyanogen, 0.1~0.2 part of hexadecane, 0.05~0.10 part of dodecyl sodium sulfate, 0.2~0.4 part of polyvinyl alcohol, 1~2 part
Emulsifier op-10 and 40~80 parts of deionized waters.
A kind of 6. preparation method of the antifouling antifog film of glass as claimed in claim 1, it is characterised in that the step（5）
In VTES, tetraethyl orthosilicate, absolute ethyl alcohol, deionized water, Ludox, sodium sulfosuccinate dioctyl ester
Parts by weight with compounded mix are 10~20 parts of VTESs, 11~22 parts of tetraethyl orthosilicates, 45~90 parts of nothings
Water-ethanol, 4~8 parts of deionized waters, 30~50 parts of mass fractions are 20% Ludox, 3~4 parts of sodium sulfosuccinate dioctyl esters and 2
~3 parts of compounded mixs.
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Application publication date: 20171201 |