CN107254207A - A kind of ultraviolet light solidification super-hydrophobic transparent wear-resistant coating and preparation method thereof - Google Patents
A kind of ultraviolet light solidification super-hydrophobic transparent wear-resistant coating and preparation method thereof Download PDFInfo
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- CN107254207A CN107254207A CN201710464078.2A CN201710464078A CN107254207A CN 107254207 A CN107254207 A CN 107254207A CN 201710464078 A CN201710464078 A CN 201710464078A CN 107254207 A CN107254207 A CN 107254207A
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- resistant coating
- ultraviolet light
- hydrophobic
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- 239000011248 coating agent Substances 0.000 title claims abstract description 86
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000008023 solidification Effects 0.000 title abstract description 15
- 238000007711 solidification Methods 0.000 title abstract description 15
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Classifications
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- C—CHEMISTRY; METALLURGY
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- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
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- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
- B05D3/065—After-treatment
- B05D3/067—Curing or cross-linking the coating
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/12—Esters of monohydric alcohols or phenols
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
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- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
The invention discloses a kind of ultraviolet light solidification super-hydrophobic transparent wear-resistant coating and preparation method thereof, belong to photocureable coating technical field.The preparation method includes transparent base activating pretreatment, the dispersion liquid containing reactive nanoparticles and prepared；Active fluorine monomer, reactive diluent and light trigger are added in the dispersion liquid containing reactive nanoparticles, then homogenous application is on the transparent base after first step activating pretreatment, and in the case where obtaining UV energy effect, solidification obtains super-hydrophobic transparent wear-resistant coating.The features such as preparation method has efficient, wide adaptability, economy, energy-conservation and is environment-friendly, the features such as ultraviolet light solidification super-hydrophobic transparent wear-resistant coating prepare simultaneously obtained by has self-cleaning surface, surface anticorrosion, hydrophobic, anti-fog properties, freezing, with there is good adhesive force to base material.
Description
Technical field
The invention belongs to photocureable coating technical field, and in particular to it is a kind of be adapted to use on glass have it is high durable
Property, water droplet wash away, super-hydrophobic automatic cleaning nanometer transparent coating and preparation method thereof.
Background technology
The coating material solidified first part of patent of ultraviolet light (UV) was born in nineteen forty-seven, by the development of over half a century, ultraviolet light
(UV) it is coating material solidified to have become more ripe technology, in particular with the raising of people's environmental consciousness, production and research people
Member is important to note that the coating material solidified development and application of UV.The end of the sixties in last century, Beyer Co., Ltd is based on unsaturated-resin and rested in peace
Fragrant system development works out a kind of ultraviolet-curing paint of environment-friendly energy-saving.In recent years, with people to using energy source with
And in terms of environmental protection problem continuous attention, countries in the world are all serious to traditional volatile organic compound VOC emission
Solvent based coating limited and improved, more pay attention to based on environmental protection theory coating technology exploitation.At present, China
Develop into after the U.S., Japan, the global the third-largest radiation-curable products place of production, among these and with photocureable coating yield most
Greatly.In the past few years, ultraviolet light (UV) is coating material solidified in fibre coating, laser disc (CD) coating, digitized video light
Suffered from disk (DVD) adhesive, credit card, timber, beverage can, packaging for foodstuff, journal surface, medicine equipment and automobile industry
Very rapidly development.
Because the unique surface characteristic of hydrophobic and super hydrophobic surface makes it in self-cleaning surface, microfluid system and biofacies
Potential application is there is in terms of capacitive, there are extensive market prospects in national defence, daily life and numerous industrial circles, it is existing
Turn into the study hotspot of major industry companies.Disclosed in publication number CN103587185A patent document with nano particle with
Super-hydrophobic coat prepared by mixed with resin, although the super-hydrophobic coat possesses certain Scratch Resistance energy, but can not realize coating
Translucency.A kind of optical clear of suitable glass baseplate is disclosed in the A of publication number CN 104987520 patent document super thin
Water coating, but effective hardness of the coating on glass can not be ensured, limit the commercialized application of its coating.Current material
Surface hydrophobicity technology still fails to realize large-scale application, traces it to its cause and is there is substantial amounts of low-surface-energy in super-hydrophobic coat
Nano particle can not cause strength of coating while super-hydrophobic effect is ensured not high enough with Bulk coat chemically reactive, logical
The coating material often applied in glass baseplate has also been proposed higher requirement to translucency.How super-hydrophobic coat is being ensured
On the premise of energy, the high light transmittance of coating is realized, higher requirement is proposed to research staff.
The content of the invention
For problems of the prior art, the present invention provide a kind of ultraviolet light solidification super-hydrophobic transparent wear-resistant coating and
Its preparation method, the features such as preparation method has efficient, wide adaptability, economy, energy-conservation and be environment-friendly, while preparing institute
Obtained ultraviolet light solidification super-hydrophobic transparent wear-resistant coating has self-cleaning surface, surface anticorrosion, hydrophobic, anti-fog properties, freezing
The features such as, with there is good adhesive force to base material.
The ultraviolet light that the present invention is provided solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, comprises the following steps that：
The first step, transparent base activating pretreatment：After transparent substrate surface has been pre-processed, by the silicon of 1~5% mass concentration
Alkane coupling agent is added in the first organic solvent, is then wherein activated transparent base immersion, in transparent substrate surface
The active group of reaction is may participate in grafting；Described active group is the acryloyl-oxy based structures containing unsaturated functional group.
Second step, according to percentage by weight, second is added to by 0.5~10% nano particle and 2~6% silane couplers
Plant in organic solvent, reaction is hydrolyzed in the environment of pH 3~9, generate the dispersion liquid containing reactive nanoparticles.
3rd step, adds active fluorine monomer, reactive diluent and light-initiated in the dispersion liquid containing reactive nanoparticles
Agent, then homogenous application is solid in the case where obtaining UV energy effect on the transparent base after first step activating pretreatment
Change obtains super-hydrophobic transparent wear-resistant coating.
Compared with prior art, the advantage of the invention is that：
(1) reactive diluent in the present invention, reactive nanoparticles, formed altogether by the reaction that crosses one another between siloxanes
Valence link, effectively improves the wearability and hardness of super-hydrophobic coat, overcome traditional super-hydrophobic coat method be sprayed directly into it is transparent
After base material, because nano particle is after by external impacts, come off from coating surface, cause the problem of super-hydrophobic effect fails.
(2) micro-nano structure that the present invention is constructed is due to being free of macromolecular resin composition in coating system, and obtained film layer is thick
Degree can be controlled effectively, it is ensured that the optical transparence of coating.
(3) present invention research and the UV solidification super-hydrophobic transparent wear-resistant coatings prepared promote super-hydrophobic coat in application road
Paces, wide market are strided forward on road.
Brief description of the drawings
The super-hydrophobic transparent wear-resistant coating structural representation that Fig. 1 is prepared for the present invention, reactive grafting is passed through in glass surface
Siloxanes chemical group and nano particle.
Fig. 2 is spherical to observe that water droplet (3 μ L) shows on super-hydrophobic transparent wear-resistant coating under an optical microscope.
Fig. 3 is the super-hydrophobic transparent wear-resistant coating of the preparation of the embodiment of the present invention 1 at visible region (390nm~780nm)
Light transmittance curve.
Fig. 4 A and Fig. 4 B be respectively embodiment 1 and comparative example 1 obtained by coating measured respectively by contact angle measurement
Contact angle.
Embodiment
For the ease of the understanding of those skilled in the art, present invention work is further retouched with reference to the accompanying drawings and examples
State.
The present invention provides the preparation method that a kind of ultraviolet light solidifies super-hydrophobic transparent wear-resistant coating, comprises the following steps that：
The first step, transparent base activating pretreatment.
To the transparent base that uses, there is no particular limitation in the present invention, can (light transmittance is big from existing optical transparent properties
Select to use in material 80%).The transparent base used in the present invention can (indium tin be aoxidized for glass, crystalline ceramics, ITO
Thing transparent conductive semiconductor film), PET, polybutylene terephthalate and poly (ethylene naphthalate),
Polyethylene, polypropylene, glassine paper, diacetyl cellulose, tri acetyl cellulose, butyric acid acetylcellulose, polyvinyl chloride,
Vingon, polyvinyl alcohol, ethylene-vinyl acetate copolymer, polystyrene, makrolon, polymethylpentene, polysulfones,
Any one in polyether-ether-ketone, PEI, polyimides, fluororesin or polyamide, preferably uses glass baseplate.
The transparent base used in the present invention, can be pre-processed when needing to use to the surface of transparent base, so as to
The reaction bonded power of intensified response group and transparent substrate surface.For example using Corona discharge Treatment, plasma (plasma)
Processing, it is sharp using the processing for heating air, or in the presence of ozone using the processing of flame using the processing (wet method) of chromic acid
Handled with ultraviolet irradiation, using Piranha solution, (piranha solution, 98% concentrated sulfuric acid and 30% hydrogen peroxide are with volume
Than for 7:3 mixed liquor) cleaning.Surface preparation carries out appropriate selection according to the species of transparent base, generally from effect and
Operability considers.
Preferably, described pretreatment can be plasma (plasma) processing, secondary to elect Piranha solution as
(piranha solution) is cleaned.
After having pre-processed, by the silane coupler of 1~5% mass concentration be added to the first organic solvent (herein for
One kind in the absolute methanol of 99% concentration, ethanol, normal propyl alcohol, isopropanol) in, then transparent base immersion is wherein lived
Change, the active group of reaction is may participate in transparent substrate surface grafting.Described active group is to contain unsaturated functional group
Acryloyl-oxy based structures.
Second step, according to percentage by weight, second is added to by 0.5~10% nano particle and 2~6% silane couplers
Plant in organic solvent, reaction is hydrolyzed in the environment of pH 3~9, generate the dispersion liquid containing reactive nanoparticles.
Nano particle of the present invention includes sapphire, silicon nitride, white carbon, carborundum, silica, aluminum oxide, oxygen
Change zirconium, titanium oxide, frit, silica glass, receive lime glass, single element or multielement oxide, such as Al2O3、ITO、
SnO2、SiO2、TiO2、ZrO2、ZnO、Bi2O3、V2O5, ZnS, CoO, CoFeO, MnFeO or BaFeO.Any one is more kinds of
The composition of nano particle all alterables, and do not require that all nano particles are constituted including identical.Nano particle, which can have, appoints
Shape of anticipating and surface texture.The structure and aggregation pattern alterable of nano particle, and the geometrical morphology and/or structure of the present invention,
Pattern can be spherical, oval, polyhedron, sheet, it is many it is empty, crystal class formation is presented, nano grain surface can be smooth
, it is coarse, orderly, unordered or patterning.Nano particle can be of different sizes or be distributed, or for one kind
Size or distribution, the average diameter of nano particle is 5 nanometers~10000 nanometers, preferably 10~100nm.
The addition of described nano particle is preferably 1~8%.
Silane R of the present invention1nSi(OR2)4-n, wherein n=0~2；R1Can be CnH2n-1The alkane of (n=1~18)
Base, preferably be selected from tetraethoxysilane, MTMS, propyl trimethoxy silicane, octadecyl trimethoxysilane,
3- methyl allyl acyloxypropyl trimethoxysilanes, 3- methacryloxypropyls triethoxysilane, 3- methacryloxypropyls
Hydroxypropyl methyl dimethoxysilane, 3- methacryloxypropyls methyldiethoxysilane, VTES, second
Alkenyl trimethoxy silane, vinyl three-(2- methoxyethoxies)-silane, 3- aminopropyl triethoxysilanes, 3- aminopropyls three
Methoxy silane, N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes, N- (2- aminoethyls) -3- aminopropyl-triethoxy silicon
Alkane, 3- aminopropyltriethoxies dimethoxysilane, N- normal-butyl -3- aminopropyl trimethoxysilanes, N- normal-butyl -3- aminopropyls three
Ethoxysilane, 3- ureas propyl trimethoxy silicane, 3- diethylin propyl trimethoxy silicane, 3- (oxygen of 2,3- epoxies third) third
Base trimethoxy silane, 3- (oxygen of 2,3- epoxies third) propyl-triethoxysilicane, 3- (oxygen of 2,3- epoxies third) hydroxypropyl methyl diformazan
One or more in TMOS, 3- (oxygen of 2,3- epoxies third) hydroxypropyl methyl diethoxy silane.
Described silane is a kind of silane containing acryloxy, preferably γ-(methacryloxypropyl) propyl trimethoxy
Silane (the entitled KH570 of business) or 3- methacryloxypropyls methyl dimethoxysilane (the entitled KH572 of business) conduct
The coupling agent of photocuring, effect of the silane coupler in this reaction system is extremely important, nano particle and transparent base,
Connecting bridge beam action is played between reactive diluent, active fluorine monomer.
Second of organic solvent of the present invention, including benzene,toluene,xylene, styrene, butyl toluene, vinyl
Toluene, carbon disulfide, tricresyl phosphate orthoresol, pentane, hexane, octane, normal hexane, hexamethylene, gasoline, kerosene, positive hexanone, hexamethylene
Ketone, toluene cyclohexanone, chlorobenzene, chloroform, dichloro-benzenes, dichloromethane, chloroform, perchloromethane, dichloroethylene, trichloro ethylene,
Perchloroethylene, methanol, ethanol, normal propyl alcohol, isopropanol, N, N- DMAAs, ether, expoxy propane, methyl formate, first
Acetoacetic ester, propyl formate, butyl formate, amyl formate, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, acetic acid penta
Ester, acetone, butanone, espeleton, methylisobutylketone, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethene
Glycol ether, furans, acetonitrile, pyridine, phenol etc..
3rd step, adds active fluorine monomer, reactive diluent and light-initiated in the dispersion liquid containing reactive nanoparticles
Agent, then homogenous application is solid in the case where obtaining UV energy effect on the transparent base after first step activating pretreatment
Change obtains super-hydrophobic transparent wear-resistant coating.
By more than three step schemes transparent substrate surface obtain transparent hydrophobic structure as shown in figure 1, the superiors be containing
Fluorine low-surface-energy layer, centre is nanoparticle structure layer, and orlop is that siloxanes base material is grafted layer.
The manner of application that the present invention is used includes：Dip-coating, spin coating, blade coating, spraying, physical vapour deposition (PVD), chemical vapor deposition
Product, vacuum filter, evaporation, flame-spraying, electron spray, sprayed deposit, growth in situ, Microwave Irradiation Assisted Chemical vapour deposition process.
Described UV energy can be obtained from high-pressure sodium lamp, be generally used for the uv agent amount of irradiation 200~
400mj/cm2In the range of.
Described active fluorine monomer is high activity, fluorinated volume is high and has in relatively low surface-active fluorine monomer, film forming procedure
It can be enriched with coating surface, form fine and close, stable hydrophobic protection film layer.
Specifically, described active fluorine monomer, including perfluoroalkyl ethanol APEO, perfluoroalkyl ethanol polyoxy second
Alkene ether, hexafluorobutyl acrylate, trifluoroethyl methacrylate, dodecafluoroheptyl methacrylate, hexafluoropropylene trimer, six
Fluoropropene dimer, 4,4 '-(hexafluoroisopropylidenyl) diphenol, 4,4- (hexafluoro isopropyl alkene) two anhydride phthalic acids, ten difluoro enanthol, perfluor
N-hexane, full-fluorine octyl sulfuryl fluoride, perfluoro-cyclicether, 2- (trifluoromethyl) acrylic acid, perfluorooctanol acrylate, perfluoro butyl second
Base iodine, perfluor (2- methyl -3- oxa-s hexyl) fluoride, perfluorooctylethyl group acrylate, 1- iodine perfluoro decane, 2,5- are double
The fluoro nonanoyl fluorine of (trifluoromethyl) -3,6- dioxas 11,2- (the iodo- tetrafluoro ethyoxyls of 2-) four fluoro ethyl vikanes, 2- perfluors
Octyl group ethyl alcohol, perfluoro hexyl ethyl alcohol, PERFLUBRON, perfluoro caprylic acid, perfluor caproic acid, PFHB, 2- perfluoroalkyls
Ethyl alcohol, 2- fluoroacrylic methyl esters, hexafluoroisopropanol, hexafluoro butanol, 3- perfluoro hexyls propyl alcohol, tetrafluoropropanol, 2,2,3,3,4,
4,5,5- octafluoro -1- amylalcohols, the fluoro- 1- propyl alcohol of 2,2,3,3,3- five, 2- (perfluoro capryl) ethylmethyl acrylate, 2- (perfluors
Hexyl) ethylmethyl acrylate, perfluoro butyl ethyl propylene acid esters, 1H, 1H, 2H- perfluor -1- decene, triethoxy -1H,
The fluoro- N- octyl groups silane of 1H, 2H, 2H- 13, perfluorobutylethyl alcohol, perfluorobutyl ethylene, Potassium Hexafluorophosphate, perfluor iodo fourth
Alkane, 2- perfluor alkyl ethyl acrylates, perfluoro-hexyl iodide alkane, perfluoromethylcyclohexane (PFMCH), perfluor iodo-octane, 2- (perfluoro butyl)
Ethylmethyl acrylate, perfluorooctylethyl group iodine, perfluorohexyl ethylene, perfluoro hexyl ethyl iodide.
Described active fluorine monomer preferably comprise functionality acryloxy perfluorinated monomers any one or it is a variety of.Especially
Explanation, the compound containing acryloxy functionality can cause radical crosslinking to react by ultraviolet lighting, the freedom of activation
Base reacts with the component for playing cross-linking reaction that can undergo free radical initiation.
It according to percentage by weight is 0.01~5% that the addition of described active fluorine monomer, which is, the amount of being preferably added to is 0.1~
3%.
Described reactive diluent is the monomer that a class contains acryloxy functionality, can contain acryloxy, first
Any one or a variety of functional groups of base acryloxy, vinyl and pi-allyl, participate in the coating UV film-forming later stages
Cross-linking reaction, improves the performance such as intensity, adhesive force, weatherability of film layer after solidification.On the other hand, the acryloyl-oxy of low molecule amount
The monomer of base functional group assigns UV solidifying film layers good translucency.
Reactive diluent of the present invention is neopentylglycol diacrylate, trimethylolpropane trimethacrylate, season
Penta tetrol triacrylate, methyl methacrylate, methyl acrylate, two contracting 3 the third two liquor-saturated diacrylate, dipentaerythritol
Six acrylate, hexanediyl ester, the propylene diluted acid ester of diethylene glycol phthalate two, neopentylglycol diacrylate,
Pentaerythritol triacrylate, trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, different ice
Piece acrylate, isobornyl methacrylate, DPG dipropyl acid esters, propoxylation trimethylolpropane tris acrylic acid
In ester, season amylalcohol tetraacrylate, 1,3 butyleneglycol diacrylate any one or it is a variety of.
The addition of described reactive diluent is weight percentage 0.001~5%.
Reactive diluent of the present invention is being light-cured into the active group that is played in membrane process on connection glass baseplate, living
Property nano grain surface is with perfluorinated monomers containing acryloxy into cross-linked network structure, and described reactive diluent content is preferably
0.05~5%, further preferred content is 0.1~3%.
Light trigger of the present invention is the key component in this reaction, and it plays decisive work to laser curing velocity
With, it can be excited after UV energy is absorbed and cause photochemical transformations, reactive intermediate of the generation with initiation polymerizing power.
Light trigger of the present invention be 2- hydroxy-2-methyl -1- phenylacetones, 1- hydroxycyclohexyl phenyl ketones,
2- methyl -2- (4- morpholinyls) -1- [4- (methyl mercapto) phenyl] -1- acetone, the oxidation of 2,4,6- trimethylbenzoy-diphenies
Phosphine, 2,4,6- trimethylbenzoyl phenyl phosphinic acid ethyl esters, 2- dimethylamino -2- benzyls -1- [4- (4- morpholinyls) phenyl] -1-
It is any one in butanone, 2- hydroxy-2-methyls -1- [4- (2- hydroxyl-oxethyls) phenyl] -1- acetone, methyl benzoylformate
Kind.
The percentage by weight of the addition of described light trigger is 0.001~2%, preferably 0.01~1%.
Embodiment 1
Glass baseplate is immersed in Piranha washing lotion and cleaned, the organic solvent of remained on surface is removed, drying is continued to employ.Take 10
Part silane coupler is added in 100 parts of methanol, and clean glass baseplate is soaked wherein and 10h, alkyl is kept at room temperature
Activate glass substrate surface structure.
5 parts of gas phase nano aluminum oxide are taken, size is distributed in 50~80nm, be added in 100 parts of methanol；Regulation in addition
Solution ph is stirring reaction 12h under 3~4,30~45 DEG C of water bath conditions, finally gives the dispersion liquid of reactive nanoparticles.
50 parts of dispersion liquids are taken, 0.5 part of 2- perfluorooctylethyl group methacrylate, 1.5 parts of trimethylolpropane tris is added
Acrylate, 0.25 part of 1- hydroxycyclohexyl phenyl ketone, is uniformly mixed, and coating fluid is made.
Made coating fluid is sprayed on the clear glass substrate surface activated in advance, to formation between 60~80 DEG C
After coating is dried 10 minutes, with 300mj/cm2Ultraviolet irradiating dose dry coating is solidified, formed ultraviolet light
Solidify super-hydrophobic transparent wear-resistant coating, coating transparent is as shown in Figure 3.
Embodiment 2
By glass baseplate alcohol solvent cleaning, drying, progress plasma in plasma washing machine is then placed in pre-
Handle glass-faced construction.Take 10 parts of silane couplers to be added in 100 parts of ethanol, pretreated sheet glass is soaked at room temperature
Steep 10h, alkyl activation glass sheet surface structure.
5 parts of nano-ZnO powder are taken, size is distributed in 20~40nm, be added in 100 parts of normal propyl alcohols, adjust in addition molten
Liquid pH value is stirring reaction 24h under 3~4,40~50 DEG C of water bath conditions, finally gives the dispersion liquid of reactive nanoparticles.
50 parts of dispersion liquids are taken, 0.5 part of perfluoro butyl ethyl propylene acid esters, 1.5 parts of methyl methacrylates, 0.25 part is added
2- hydroxy-2-methyl -1- phenylacetones, are uniformly mixed, and coating fluid is made.
Made coating fluid is sprayed on the clear glass of alkylation, 10 are dried to the coating of formation between 60~80 DEG C
After minute, with 300mj/cm2Ultraviolet irradiating dose dry coating is solidified, formed ultraviolet light solidification it is super-hydrophobic
Transparent wear-resistant coating.
Embodiment 3
By glass baseplate alcohol solvent cleaning, drying, progress plasma in plasma washing machine is then placed in pre-
Handle glass-faced construction.Take 10 parts of silane couplers to be added in 100 parts of methanol, clean sheet glass is soaked at room temperature
8h, alkyl activation glass sheet surface structure.
Take 5 parts of Nano-meter SiO_2s2Powder, size is distributed in 10~30nm, is added in 100 parts of ethyl acetates, adjusts in addition
Solution ph is stirring reaction 12h under 4~5,40~50 DEG C of water bath conditions, finally gives the dispersion liquid of reactive nanoparticles.
Take 50 parts of dispersion liquids, add 0.5 part of 2- fluoroacrylic methyl ester, 1 part of dipentaerythritol acrylate, 0.5 part 2,
4,6- trimethylbenzoy-dipheny phosphine oxides, are uniformly mixed, and coating fluid is made.
The clear glass activated in advance is impregnated into coating fluid and soaked 10 minutes, then presss from both sides out right between 60~80 DEG C
After the coating of formation is dried 5 minutes, with 300mj/cm2Ultraviolet irradiating dose dry coating is solidified, and shape
Solidify super-hydrophobic transparent wear-resistant coating into ultraviolet light.
Embodiment 4
Sheet glass is immersed in Piranha washing lotion and cleaned, the organic solvent of remained on surface is removed, drying is continued to employ.Take 10 parts
Silane coupler is added in 100 parts of methanol, and clean sheet glass is soaked into 10h, alkyl activation glass sheet surface knot at room temperature
Structure.
6 parts of nanometer tin indium oxide powders are taken, size is distributed in 80~100nm, be added in 100 parts of isopropanols, in addition
It is stirring reaction 18h under 8~9,40~50 DEG C of water bath conditions to adjust solution ph, finally gives the scattered of reactive nanoparticles
Liquid.
Take 50 parts of dispersion liquids, add 1 part of 2- (perfluoro capryl) ethylmethyl acrylate, the liquor-saturated dipropyl of 1 part of two contracting 3 the third two
Olefin(e) acid ester, 0.5 part of methyl benzoylformate, is uniformly mixed, and coating fluid is made.
The clear glass activated in advance is impregnated into coating fluid and soaked 10 minutes, then presss from both sides out right between 60~80 DEG C
After the coating of formation is dried 5 minutes, with 300mj/cm2Ultraviolet irradiating dose dry coating is solidified, and shape
Solidify super-hydrophobic transparent wear-resistant coating into ultraviolet light.
Embodiment 5
Sheet glass is immersed in Piranha washing lotion and cleaned, the organic solvent of remained on surface is removed, drying is continued to employ.Take 10 parts
Silane coupler is added in 100 parts of methanol solutions, and clean sheet glass is soaked into 10h, alkyl activation sheet glass table at room temperature
Face structure.
Take 6 parts of nanometer ZrO2Particle, size is distributed in 40~50nm, is added in 100 parts of ethanol, adjusts in addition molten
Liquid pH value is stirring reaction 20h under 8~9,40~50 DEG C of water bath conditions, finally gives the dispersion liquid of reactive nanoparticles.
Take 50 parts of dispersion liquids, add 1 part of dodecafluoroheptyl methacrylate, 1.5 parts of dipentaerythritol acrylates,
0.5 part of 2- hydroxy-2-methyl -1- phenylacetone, is uniformly mixed, and coating fluid is made.
The clear glass activated in advance is impregnated into coating fluid and soaked 10 minutes, then presss from both sides out right between 60~80 DEG C
After the coating of formation is dried 1 minute, with 300mj/cm2Ultraviolet irradiating dose dry coating is solidified, and shape
Solidify super-hydrophobic transparent wear-resistant coating into ultraviolet light.Super-hydrophobic transparent is solidified to the ultraviolet light provided in above-described embodiment 1~5
Wear-resistant coating carries out performance test, as a result see the table below 1, the requirement of following technical indicator can be reached after tested.
The ultraviolet light of table 1 solidifies the performance test results of super-hydrophobic transparent wear-resistant coating
| Project | Testing standard | Test result |
| Pencil hardness | GB/T6739-2006 | More than 1H |
| Adhesive force | GB9286-98 | 0 grade |
| Contact angle | GB/T 26490-2011 | >150° |
| Roll angle | GB/T 30447-2013 | <5° |
| Translucency | GB/T 2680-1994 | >90% |
Comparative example 1
The component selected by ultraviolet light solidification super-hydrophobic transparent wear-resistant coating described in this comparative example and institute in embodiment 1
The raw material components provided are identical, and it is differed only in is operated according to each step of scheme of embodiment 1, but in final step
Take and the content of monomer of 2- fluoroacrylic methyl esters is kept to 0 part, other conditions keep constant.By this comparative example equally carry out 60~
80 DEG C of heat drying, then carry out ultraviolet light curing reaction.As optical photograph it is easily observed that obtained by sample, as a result such as Fig. 4 institutes
Show, the coating does not have ultra-hydrophobicity after ultraviolet light solidification process.
Comparative example 2
The component selected by ultraviolet light solidification super-hydrophobic transparent wear-resistant coating described in this comparative example and institute in embodiment 1
The raw material components provided are identical, and it is differed only in is carried out after equally operating according to the scheme of embodiment 1, to the activity in system
It (is that a class is post-processed by hydrophilic aerosil through HMDS that nano particle, which changes Degussa R812s products into,
Hydrophobic type fumed silica) after, same comparative example carries out carrying out ultraviolet light solidification after 60~80 DEG C of heat drying anti-
Should.
Hardness of paint film is tested with pencil method to embodiment 1 and comparative example 2 according to national standard GB/T6739-2006.The test side
Method is the assay method that hardness of film is represented using known hardness label.After tested, coating prepared in comparative example 2 test knot
Fruit can not show a candle to the 1H hardness of prepared coating in embodiment 1 for 5B.This test result illustrates that reactive nanoparticles are applied overall
Being chemically reacted in material with reactive diluent has obvious effect to lifting strength of coating, and R812s nanometers of gas outer silicon bags
Coating hardness can not be effectively improved by wrapping up in the accumulation of one layer of methyl group in the coating of dry solidification only physically.
Obviously, above-described embodiment is only intended to clearly illustrate illustrates with making, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (8)
1. a kind of ultraviolet light solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, it is characterised in that：Specific steps such as,
The first step, transparent base activating pretreatment：Transparent base is activated with silane-containing solution, can in transparent substrate surface grafting
Participate in the active group of reaction；
Second step, according to percentage by weight, 0.5~10% nano particle and 2~6% silane couplers are added into second has
In machine solvent, reaction is hydrolyzed in the environment of pH 3~9, the dispersion liquid containing reactive nanoparticles is generated；
3rd step, adds active fluorine monomer, reactive diluent and light trigger, so in the dispersion liquid containing reactive nanoparticles
Homogenous application solidifies in the case where obtaining UV energy effect and obtained on the transparent base after first step activating pretreatment afterwards
Super-hydrophobic transparent wear-resistant coating.
2. a kind of ultraviolet light according to claim 1 solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, its feature exists
In：Described activating pretreatment specifically,
Using plasma processing or Piranha solution cleaning transparent substrate surface；It is after having pre-processed, 1~5% mass is dense
The silane coupler of degree is added in the first organic solvent, is then wherein activated transparent base immersion, in transparent base
The active group of reaction is may participate on material surface grafting；Described active group is the acryloxy containing unsaturated functional group
Structure.
3. a kind of ultraviolet light according to claim 2 solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, its feature exists
In：The first described organic solvent is in absolute methanol, ethanol, normal propyl alcohol or the isopropanol of 99% weight percent concentration
It is a kind of.
4. a kind of ultraviolet light according to claim 1 solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, its feature exists
In：Nano particle described in second step includes sapphire, silicon nitride, white carbon, carborundum, silica, aluminum oxide, oxidation
Zirconium, titanium oxide, frit, silica glass, receive lime glass, single element or multielement oxide, the average diameter of nano particle
It it is 5 nanometers~10000 nanometers, the addition of described nano particle is 1~8%.
5. a kind of ultraviolet light according to claim 1 solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, its feature exists
In：Described UV energy is obtained from high-pressure sodium lamp, and uv agent amount is in 200~400mj/cm2In the range of.
6. a kind of ultraviolet light according to claim 1 solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, its feature exists
In：It according to percentage by weight is 0.01~5% that the addition of described active fluorine monomer, which is,；The addition of described reactive diluent
Measure as weight percentage 0.001~5%；The percentage by weight of the addition of described light trigger is 0.001~2%.
7. a kind of ultraviolet light according to claim 1 or 6 solidifies the preparation method of super-hydrophobic transparent wear-resistant coating, its feature
It is：It according to percentage by weight is 0.1~3% that the addition of described active fluorine monomer, which is,；The reactive diluent content is
0.05~5%；The percentage by weight of the addition of described light trigger is 0.01~1%.
8. a kind of ultraviolet light solidifies super-hydrophobic transparent wear-resistant coating, it is characterised in that：The superiors of the coating are fluorine-containing low table
Face ergosphere, centre is nanoparticle structure layer, and orlop is that siloxanes base material is grafted layer.
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