CN105038575A - Water-based anti-dazzle UV coating, hard coated film and preparation method of hard coated film - Google Patents
Water-based anti-dazzle UV coating, hard coated film and preparation method of hard coated film Download PDFInfo
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Abstract
The invention provides water-based anti-dazzle UV coating. The water-based anti-dazzle UV coasting comprises, by weight, 30-90 parts of waterborne polyurethane urethane acrylate prepolymer, 10-60 parts of diluting monomers, 5-100 parts of anti-dazzle particles, 0.05-10 parts of waterborne wetting dispersant, 0.05-5 parts of waterborne flatting agents, 1-20 parts of water, 0.5-10 parts of waterborne photoinitiator and 1-30 parts of waterborne isocyanate curing agents. The water-based anti-dazzle UV coating is water-based coating and is environmentally friendly, waterborne isocyanate curing agents are matched with the waterborne polyurethane urethane acrylate prepolymer and the diluting monomers, and the overall abrasion resistance of a coating obtained after the water-based anti-dazzle UV coating is cured can be obviously improved. The invention further provides a hard coated film and a preparation method of the hard coated film. An experimental result indicates that the rigidity of the hard coated film formed by the coating is 3 H, and no scratch is generated even though the hard collated film is rubbed by 1,000 g of loads 20 times.
Description
Technical field
The invention belongs to technical field of aqueous paint, particularly relate to the anti-dazzle UV coating of a kind of water-based, cured film and preparation method thereof.
Background technology
On the display screen of liquid-crystal display or plasma panel, for protection screen is not scratched, need to paste a floor height light-transmission type cured film on the display screen.But general high light-transmission type cured film in use, usually there will be and causes " dazzling light " phenomenon because plate surface is reflective." dazzle light " and not only have impact on the visuality of screen, and certain injury can be caused to human eye.At present, by adding a certain amount of anti-dazzle particle in hardening coat, making the light reflected from film surface become soft, thus reaching antiglare effect.
Because ultraviolet-curing paint has efficiently, is suitable for wide, economic, energy-conservation, eco-friendly feature, existing anti-glare paint is mostly ultraviolet light polymerization anti-glare paint (anti-dazzle UV coating); Anti-dazzle UV dope viscosity is higher, needs to add solvent or reactive thinner dilutes.In prior art, publication number a kind of anti-glare paint composition that has been the Introduction To Cn Patent of CN102985500A and there is the anti-dazzle film of superior abrasion resistance and resistance to soiling.This anti-glare paint composition comprises: adhesive resin, containing the particle based on the compound of the UV curable functional group of fluorine, light trigger, surperficial curable light trigger, surface with uneven pattern.Wherein, this anti-glare paint mainly uses ethyl methyl ketone and toluene as organic solvent.Ethyl methyl ketone has irritating smell, and toluene is carinogenicity material, to human body and environmental injury larger.Publication number a kind of anti-dazzle coating that has been the Introduction To Cn Patent of CN103952073A and preparation method thereof, in this anti-dazzle coating, each component according to parts by weight is: hyperergy monomer or hyperergy oligopolymer 10 ~ 80 parts; Low reactivity monomer or low reactivity oligopolymer 10 ~ 6 parts; 5 ~ 10 parts, anti-dazzle particle; Light trigger 1 ~ 10 part; Leveling auxiliary agent 0.01 ~ 5 part; Wetting and dispersing auxiliary agent 0.1 ~ 1 part; Organic solvent 20 ~ 90 parts.This anti-glare paint system is solvent-based system, needs to use ester class or ketones solvent, and the content of solvent is higher, unfriendly to environment.
In order to be down to minimum by the quantity discharged of volatile organic matter (VOC), eliminate the harm to human body in production process, the anti-dazzle UV coating of water-based becomes a kind of and selects preferably simultaneously.Water-borne coatings is low due to its viscosity, greatly reduces the consumption of easy volatile thinner, or without the need to using easy volatile thinner, thus reach the unification of the feature of environmental protection and performance.But, relative to the anti-dazzle UV coating of traditional solvent-borne type, the performance of water-based anti-dazzle UV coating is lower than the anti-dazzle UV coating of solvent-borne type, this is mainly determined by the membrane formation mechanism of the anti-dazzle UV coating of water-based, after water-based anti-dazzle UV coating drying and forming-film, the tightness of film forming not as the anti-dazzle UV coating of solvent-borne type, thus makes the properties of the film after solidifying if hardness, wear resistance etc. are not as the anti-dazzle UV coating of solvent-borne type.
Summary of the invention
The object of the present invention is to provide the anti-dazzle UV coating of a kind of water-based, cured film and preparation method thereof, water-based provided by the invention anti-dazzle UV coating is environmentally friendly, and has higher hardness and good wear resistance.
The invention provides the anti-dazzle UV coating of a kind of water-based, comprise the component of following parts by weight:
Aqueous polyurethane acrylate prepolymer: 30 ~ 90 parts;
Diluting monomer: 10 ~ 60 parts;
Anti-dazzle particle: 5 ~ 100 parts;
Water-based wetting dispersing agent: 0.05 ~ 10 part;
Water-based flow agent: 0.05 ~ 5 part;
Water: 1 ~ 20 part;
Water-soluble photoinitiator: 0.5 ~ 10 part;
Water-based isocyanate solidifying agent: 1 ~ 30 part.
Preferably, described aqueous polyurethane acrylate prepolymer is two functionality and above aqueous polyurethane acrylate prepolymer;
The parts by weight of described aqueous polyurethane acrylate prepolymer are 40 ~ 80 parts.
Preferably, described diluting monomer comprises esters of acrylic acid diluting monomer;
The parts by weight of described diluting monomer are 15 ~ 50 parts.
Preferably, described anti-dazzle particle comprises one or more in silicon-dioxide, aluminum oxide, Magnesium Silicate q-agent, pure aluminium silicate, neusilin, calcium carbonate, magnesiumcarbonate, aluminium hydroxide, titanium dioxide, polypropylene, zirconium white, spherical shaped silicone particle and acrylic resin particle;
The parts by weight of the anti-dazzle particle of described water-based are 10 ~ 80 parts.
Preferably, described water-based wetting dispersing agent comprises the alkyl alcohol amine salt of high molecular weight acidic polymkeric substance, acrylic copolymer, the alkane hydroxyl amine salt of lower molecular weight polynary hydroxy acid polymkeric substance, the alkanolamine of the polymer copolymerization ester of band acidic-group, the polymeric alkylammonium salt of multiple functional radical and containing one or more in pigment affinity groups polymer copolymerization body;
The parts by weight of described water-based wetting dispersing agent are 0.1 ~ 5.
Preferably, described water-based flow agent comprises polyester resin change properties of organic silicon, esters of acrylic acid flow agent, fluorin modified crylic acid ester copolymer, sulfonate type fluorine flow agent, the metal carboxylate fluorocarbon surfactant of the polyether silicones of non-reactive, the organic silicon modified by polyether of response type or response type;
The parts by weight of described water-based flow agent are 0.1 ~ 2.5 part.
Preferably, described water-soluble photoinitiator comprises cracking type initiator and/or hydrogen-abstraction initiator;
Described cracking type initiator comprises 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone, 1,1'-(methylene radical two-4,1-phenylene) two [2-hydroxy-2-methyl-1-acetone], 2-methyl isophthalic acid-[-4-methylthio group) phenyl]-2-morpholinyl-1-acetone, 2, one or more in 4,6-trimethylbenzoy-dipheny phosphine oxide, benzoin dimethylether, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxy-cyclohexyl-phenyl ketone and benzoyl derivatives;
Described hydrogen-abstraction initiator comprise benzophenone, 4-benzoyl-4'-methyl-diphenyl sulfide, 2-benzoyl methyl benzoate, isopropyl thioxanthone uh one or more in ketone and 4-(N, N-dimethylamino) ethyl benzoate;
The parts by weight of described water-soluble photoinitiator are 2 ~ 8 parts.
Preferably, the anti-dazzle UV coating of described water-based also comprises aqueous solvent;
Described aqueous solvent comprises one or more in alcoholic solvent, alcohol ether solvent and solvent of ether ester type;
The parts by weight of described aqueous solvent are 5 ~ 80 parts.
The invention provides a kind of cured film, obtained by the anti-dazzle UV coating of above-mentioned water-based.
The invention provides a kind of preparation method of cured film, comprise the following steps:
A) with weight parts, by 30 ~ 90 parts of aqueous polyurethane acrylate prepolymers, 10 ~ 60 parts of diluting monomers, 5 ~ 100 parts of anti-dazzle particles, 0.05 ~ 10 part of water-based wetting dispersing agent, 0.05 ~ 5 part of water-based flow agent, 1 ~ 20 part of water, 0.5 ~ 10 part of water-soluble photoinitiator and 1 ~ 30 part of water-based isocyanate solidifying agent mixing, obtain the anti-dazzle UV coating of water-based;
B) by described steps A) the anti-dazzle UV paint of water-based that obtains at matrix surface, carry out UV-irradiation, obtain cured film work in-process;
C) by described step B) the cured film work in-process that obtain carry out thermofixation, obtain cured film.
The invention provides the anti-dazzle UV coating of a kind of water-based, comprise the component of following parts by weight: aqueous polyurethane acrylate prepolymer: 30 ~ 90 parts; Diluting monomer: 10 ~ 60 parts; Anti-dazzle particle: 5 ~ 100 parts; Water-based wetting dispersing agent: 0.05 ~ 10 part; Water-based flow agent: 0.05 ~ 5 part; Water: 1 ~ 20 part; Water-soluble photoinitiator: 0.5 ~ 10 part; Water-based isocyanate solidifying agent: 1 ~ 30 part.Anti-dazzle UV coating in the present invention is water-borne coatings, environmentally friendly, and the anti-dazzle UV coating of water-based in the present invention with the addition of water-soluble photoinitiator and water-based isocyanate solidifying agent simultaneously, water-based isocyanate solidifying agent collocation aqueous polyurethane acrylate prepolymer and diluting monomer, the overall wear resistance of coating after the anti-dazzle UV paint solidification of described water-based can be significantly improved, experimental result shows, the hardness of the cured film that coating provided by the invention is formed is 3H, and load 1000g rubs 20 no markings.
Embodiment
The invention provides the anti-dazzle UV coating of a kind of water-based, comprise the component of following parts by weight:
Aqueous polyurethane acrylate prepolymer: 30 ~ 90 parts;
Diluting monomer: 10 ~ 60 parts;
Anti-dazzle particle: 5 ~ 100 parts;
Water-based wetting dispersing agent: 0.05 ~ 10 part;
Water-based flow agent: 0.05 ~ 5 part;
Water: 1 ~ 20 part;
Water-soluble photoinitiator: 0.5 ~ 10 part;
Water-based isocyanate solidifying agent: 1 ~ 30 part.
Water-based provided by the invention anti-dazzle UV coating is environmentally friendly, and has higher hardness and good wear resistance.
The anti-dazzle UV coating of water-based provided by the invention comprises aqueous polyurethane acrylate prepolymer, and described aqueous polyurethane acrylate prepolymer preferably has two functionality and above aqueous polyurethane acrylate prepolymer.The source of the present invention to described aqueous polyurethane acrylate prepolymer does not have special restriction, can buy its commercial goods, can prepare voluntarily according to method well known to those skilled in the art yet.In the present invention, described aqueous polyurethane acrylate prepolymer as the matrix resin of this formula, for improve the hardness of resin, wear-resisting, transmittance, to the surface appearance after the moisture dispersibility of particle, coating film.In the present invention, the parts by weight of described aqueous polyurethane acrylate prepolymer are 30 ~ 90 parts, are preferably 40 ~ 80 parts, are more preferably 50 ~ 70 parts.
In the present invention, described diluting monomer preferably includes esters of acrylic acid diluting monomer, more preferably hydroxyethyl methylacrylate is comprised, Rocryl 410, Hydroxyethyl acrylate, Propylene glycol monoacrylate, double cyclopentenyl acrylate, tetrahydrofurfuryl acrylate, iso-bornyl acrylate, adjacent phenylphenoxy ethyl propylene acid esters, tristane omega-diol diacrylate, three (2-hydroxyl ethyl ester) isocyanurate triacrylate, Viscoat 295, pentaerythritol triacrylate, trimethylolpropane trimethacrylate, tetramethylol methane tetraacrylate, two-trimethylolpropane tetra-acrylate, double pentaerythritol C5 methacrylate, one or more in dipentaerythritol acrylate and caprolactone modification double pentaerythritol methacrylate, the parts by weight of described diluting monomer are 10 ~ 60 parts, are preferably 15 ~ 50 parts, are more preferably 20 ~ 40 parts.Concrete, in an embodiment of the present invention, EM235 monomer, EM264 monomer or EM235 monomer that Changxing, Taiwan company provides can be adopted, or the MiramerM500 monomer that the special Chemical Co., Ltd. in U.S. source provides.
In the present invention, the anti-dazzle particle of described water-based preferably includes one or more in silicon-dioxide, aluminum oxide, Magnesium Silicate q-agent, pure aluminium silicate, neusilin, calcium carbonate, magnesiumcarbonate, aluminium hydroxide, titanium dioxide, polypropylene, zirconium white, spherical shaped silicone particle and acrylic resin particle; The particle diameter of described anti-dazzle particle is preferably 10 ~ 5000nm, is more preferably 50 ~ 900nm, most preferably is 100 ~ 600nm; The present invention preferably adopts the anti-dazzle particle combination of several different-grain diameter to add in described UV coating, micron-sized particle mainly plays the effect of outer mist degree, make entirety reach mist degree demand, the effect of interior mist degree is mainly played in the effect of nano level particle, makes light exquisiteness soft.After mixture, a kind of equilibrium state can be reached between intrinsic fog and outer mist.As, the anti-dazzle particle of 10 ~ 15nm and the anti-dazzle particle of 500 ~ 600nm are combined; The anti-dazzle particle of 70 ~ 100nm and the anti-dazzle particle of 600nm are combined; The anti-dazzle particle of the anti-dazzle particle of 4 ~ 5 μm, the anti-dazzle particle of 10 ~ 15nm and 500 ~ 600nm is combined; The anti-dazzle particle of 500nm and the anti-dazzle particle of 900nm are combined.The parts by weight of the anti-dazzle particle of described water-based are 5 ~ 100 parts, are preferably 10 ~ 50 parts, are more preferably 15 ~ 30 parts.In the present invention, described anti-dazzle particle can add with powder, also can add in a form of slurry, or the form of slurry and powder combination.
In the present invention, described water-based wetting dispersing agent preferably include the alkyl alcohol amine salt of high molecular weight acidic polymkeric substance, acrylic copolymer, the alkane hydroxyl amine salt of lower molecular weight polynary hydroxy acid polymkeric substance, the alkanolamine of the polymer copolymerization ester of band acidic-group, the polymeric alkylammonium salt of multiple functional radical, containing one or more in pigment affinity groups polymer copolymerization body; The parts by weight of described water-based wetting dispersing agent are 0.05 ~ 10 part, are preferably 0.1 ~ 2.5 part, are more preferably 0.2 ~ 2.5 part.In the present invention, described water-based wetting dispersing agent has the effect well soaking and disperse for the anti-dazzle particle of water-based, has well stable and anti-congregation for the anti-dazzle particle of water-based.Concrete, in an embodiment of the present invention, the model that BYK (Bi Ke chemistry) can be adopted to provide is the water-based wetting dispersing agent of DISPERBYK-180, DISPERBYK-184, DISPERBYK-190 or DISPERBYK-198; Or adopt the dispersion agent that the TEGO Series Dispersant of Ying Chuan Degussa group, YCK (firm digest) and De Qian Chemical Co., Ltd. provide.
In the present invention, described water-based flow agent preferably includes polyester resin change properties of organic silicon, esters of acrylic acid flow agent, fluorin modified crylic acid ester copolymer, sulfonate type fluorine flow agent, the metal carboxylate fluorocarbon surfactant of the polyether silicones of non-reactive, the organic silicon modified by polyether of response type or response type; The parts by weight of described water-based flow agent are 0.05 ~ 5 part, are preferably 0.1 ~ 2.5 part, are more preferably 0.2 ~ 1.3 part.In the present invention, described water-based flow agent has good levelling to the anti-dazzle particle of described water-based, sprawls effect, coordinates with above-mentioned water-based wetting dispersing agent, can ensure anti-dazzle particle being uniformly distributed and stability in storage in waterborne UV coating.Concrete, in an embodiment of the present invention, described water-based flow agent can adopt BYK-333, BYK-3500, BYK346 or BYK-348 flow agent of Bi Ke chemistry, or the flow agent adopting the TEGO of Ying Chuan Degussa group series flow agent, YCK (firm digest) and De Qian Chemical Co., Ltd. to provide.
In the present invention, described water is preferably deionized water, and the parts by weight of described water are 1 ~ 20 part, is preferably 3 ~ 15 parts, is more preferably 2 ~ 8 parts, most preferably is 4 ~ 6 parts.
In the present invention, described water-soluble photoinitiator preferably includes cracking type initiator and/or hydrogen-abstraction initiator; Described cracking type initiator comprises 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone, 1,1'-(methylene radical two-4,1-phenylene) two [2-hydroxy-2-methyl-1-acetone], 2-methyl isophthalic acid-[-4-methylthio group) phenyl]-2-morpholinyl-1-acetone, 2, one or more in 4,6-trimethylbenzoy-dipheny phosphine oxide, benzoin dimethylether, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxy-cyclohexyl-phenyl ketone and benzoyl derivatives; Described hydrogen-abstraction initiator comprise benzophenone, 4-benzoyl-4'-methyl-diphenyl sulfide, 2-benzoyl methyl benzoate, isopropyl thioxanthone uh one or more in ketone and 4-(N, N-dimethylamino) ethyl benzoate.In the present invention, the parts by weight of described water-soluble photoinitiator are 0.5 ~ 10 part, are preferably 2 ~ 8 parts, are more preferably 4 ~ 6 parts.Concrete, in an embodiment of the present invention, vapour can be adopted to cling to (Ciba) refine in IRGACURE2959, IRGACURE184 and IRGACURE1173 that company limited provides one or more.
In the present invention, the parts by weight of described water-based isocyanate solidifying agent are 1 ~ 30 part, are preferably 3 ~ 20 parts, are more preferably 5 ~ 10 parts, in an embodiment of the present invention, specifically can adopt XD-803, Byer-3100, Byer-2478 solidifying agent.In the present invention, water-based isocyanate solidifying agent collocation aqueous polyurethane acrylate prepolymer and diluting monomer, can significantly improve the overall wear resistance of the anti-dazzle UV coating of described water-based.
In the present invention, the anti-dazzle UV coating of described water-based preferably also comprises aqueous solvent, described aqueous solvent preferably includes one or more in alcoholic solvent, alcohol ether solvent and solvent of ether ester type, more preferably comprises ethanol, Virahol, propyl carbinol, isopropylcarbinol, sec-butyl alcohol, butyl glycol ether, propandiol butyl ether, propylene glycol monomethyl ether, 2-Butoxyethyl acetate, 1-Methoxy-2-propyl acetate, ethylene glycol ether acetate; The parts by weight of described aqueous solvent are preferably 5 ~ 80 parts, are more preferably 10 ~ 60 parts, most preferably are 20 ~ 40 parts.The present invention is preferably first by described aqueous solvent and water mixing, obtain mixed solvent, again aqueous polyurethane acrylate prepolymer, diluting monomer are added in mixed solvent, stir with the speed of 800 ~ 1000r/min, then water-soluble photoinitiator, water-based wetting dispersing agent and anti-dazzle particle (or anti-dazzle particle slurry) is added, improve stirring velocity to 1000 ~ 1200r/min, stir 1 ~ 3 hour, then flow agent and water-based isocyanate solidifying agent is added, stir 5 ~ 10min, obtain the anti-dazzle UV coating of water-based.
Present invention also offers a kind of cured film, obtained by the anti-dazzle UV coating of above-mentioned water-based.In the present invention, the thickness of described cured film is preferably 3 ~ 5 μm, is more preferably 4 μm, and when described cured film thickness is lower than 3 μm, hardness is difficult to the high rigidity reaching more than 2H, and wear resistance can be affected; When thickness is more than 5 μm, the easy embrittlement of coating, easily fractures.
Present invention also offers a kind of preparation method of cured film, comprise the following steps:
A) with weight parts, by 30 ~ 90 parts of aqueous polyurethane acrylate prepolymers, 10 ~ 60 parts of diluting monomers, 5 ~ 100 parts of anti-dazzle particles, 0.05 ~ 10 part of water-based wetting dispersing agent, 0.05 ~ 5 part of water-based flow agent, 1 ~ 20 part of water, 0.5 ~ 10 part of water-soluble photoinitiator and 1 ~ 30 part of water-based isocyanate solidifying agent mixing, obtain the anti-dazzle UV coating of water-based;
B) by described steps A) the anti-dazzle UV paint of water-based that obtains at matrix surface, carry out UV-irradiation, obtain cured film work in-process;
C) by described step B) the cured film work in-process that obtain carry out thermofixation, obtain cured film.
The present invention is preferably according to described steps A) in each component consumption and be prepared according to the preparation method of the anti-dazzle UV coating of above-mentioned water-based, when described anti-dazzle particle is slurry form, can directly add, when described anti-dazzle particle is powder, the anti-dazzle particle of described powder is preferably made into the anti-dazzle particle of slurry form by the present invention, adds in a form of slurry.
The present invention is preferably by solvent, dispersion agent and anti-dazzle mix particles, obtain anti-dazzle particle slurry, more preferably existing by solvent and dispersant, stir with the speed of 800 ~ 1000r/min, make in the dispersed solvent of dispersion agent, then anti-dazzle particle powder is added by amount, stir with the speed of 1000 ~ 1200r/min, after described anti-dazzle particle powder adds, improve rotating speed to 1800 ~ 2000r/min, stir after 1 ~ 2 hour, obtain anti-dazzle particle slurry.In the present invention, described solvent preferably includes one or more in alcoholic solvent, alcohol ether solvent and solvent of ether ester type, more preferably comprises ethanol, Virahol, propyl carbinol, isopropylcarbinol, sec-butyl alcohol, butyl glycol ether, propandiol butyl ether, propylene glycol monomethyl ether, 2-Butoxyethyl acetate, 1-Methoxy-2-propyl acetate, ethylene glycol ether acetate; Described dispersion agent preferably include the alkyl alcohol amine salt of high molecular weight acidic polymkeric substance, acrylic copolymer, the alkane hydroxyl amine salt of lower molecular weight polynary hydroxy acid polymkeric substance, the alkanolamine of the polymer copolymerization ester of band acidic-group, the polymeric alkylammonium salt of multiple functional radical, containing one or more in pigment affinity groups polymer copolymerization body; The kind of described anti-dazzle particle is consistent with the kind of the anti-dazzle particle described in technique scheme, does not repeat them here.In described anti-dazzle particle slurry, the parts by weight of described solvent are preferably 80 ~ 100 parts, are more preferably 90 ~ 95 parts; The parts by weight of described dispersion agent are preferably 0.5 ~ 2 part, are more preferably 1 ~ 1.5 part.The parts by weight of described anti-dazzle particle are preferably 5 ~ 30 parts, are more preferably 10 ~ 20 parts.
Anti-dazzle for described water-based UV paint at matrix surface, is carried out UV-irradiation by the present invention, obtains cured film work in-process, and the coating of described coating is preferably carried out drying by the present invention, and then carries out UV-irradiation, obtains cured film work in-process.In the present invention, the temperature of described drying is preferably 60 ~ 100 DEG C, is more preferably 70 ~ 90 DEG C, most preferably is 80 ~ 85 DEG C; The time of described drying is preferably 1 ~ 10min, is more preferably 2 ~ 8min, most preferably is 3 ~ 7min.
The cured film smooth surface that the present invention obtains is even, does not have defect.
In the present invention, described UV-irradiation amount is preferably 200 ~ 1000mj/m
2, be more preferably 400 ~ 800mj/m
2, most preferably be 600 ~ 700mj/m
2.The present invention preferably adopts high voltage mercury lamp emitting ultraviolet light to irradiate.Described matrix is preferably PET; The method of the present invention to described coating does not have special restriction, adopts ordinary method, and e.g., rolling method, scraper plate coating method, slit extrusion coating methods or gravure coating process, be preferably rolling method or gravure coating process.
The cured film work in-process obtained are carried out thermofixation by the present invention, obtain cured film, and the temperature of described thermofixation is preferably 20 ~ 60 DEG C, is more preferably 30 ~ 50 DEG C, most preferably is 35 ~ 40 DEG C; The time of described thermofixation is preferably 36 ~ 60 hours, is more preferably 40 ~ 55 hours, most preferably is 45 ~ 48 hours.The present invention preferably carries out described thermofixation under constant temperature.
The model that the present invention adopts Marl, Germany company to provide is that the pin of MillimarC1216 is stepped on film thickness instrument and tested the cured film thickness obtained, and result shows, the thickness of cured film of the present invention is between 3 ~ 4 μm.
The present invention adopts haze meter (upper Nereid's tech device Manufacturing Co., Ltd, model: WGT-S) to test total light transmittance (T) and the mist degree (H) of cured film of the present invention.Result shows, the total light transmittance of cured film provided by the invention is about 90 ~ 91, and mist degree is between 4.0 ~ 4.2.
The present invention carries out wiping repeatedly at cured film surface #0000 Steel Wool, load 1000g, and frictional distance is 5 ~ 6cm, when grinding vestige according to cured film, evaluates the number of times of friction.Result shows, the cured film in the present invention rubs 20 no markings.
In order to further illustrate the present invention, below in conjunction with embodiment, the anti-dazzle UV coating of a kind of water-based provided by the invention, cured film and preparation method thereof being described in detail, but can not limiting the scope of the present invention being understood as.
Embodiment 1
The raw material that the present embodiment uses and consumption (parts by weight) are in table 1.
The raw material of table 1 embodiment of the present invention 1 and consumption
| Aqueous polyurethane acrylate | UCECOAT 7200 | 40 parts |
| Aliphatic polyurethane dispersion | UCECOAT 7699 | 20 parts |
| Pentaerythritol triacrylate | EM 235 | 20 parts |
| Double pentaerythritol C5 methacrylate | Miramer M500 | 20 parts |
| Deionized water | Deionized water | 10 parts |
| 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone | IRGACURE 2959 | 2 parts |
| 1-hydroxy-cyclohexyl-phenyl ketone | IRGACURE 184 | 3 parts |
| Silicon-dioxide flatting silica | HP230 slurry | 10 parts |
| Organically-modified 500nm silicon-dioxide | NSI 500P | 10 parts |
| 10 ~ 15nm silicon-dioxide | IPA-ST | 20 parts |
| With the alkanolamine of acidic-group polymer copolymerization ester | DISPERBYK-180 | 0.4 part |
| Organic silicon modified by polyether | BYK-333 | 0.8 part |
| Water-based isocyanate solidifying agent | XD-803 | 10 parts |
| Propylene glycol monomethyl ether | Propylene glycol monomethyl ether | 15 parts |
| Virahol | Virahol | 5 parts |
Preparation method is as follows:
1) preparation of anti-dazzle particle slurry:
60 parts of propylene glycol monomethyl ethers, 30 parts of isopropanol solvents are added in the agitation vat with condenser, add 1 part of dispersant B YK-180, stir 10 minutes, stirring velocity 800r/min, makes wetting dispersing agent be dispersed in solvent.Then add 10 parts of HP230 (De Qian company, particle diameter 3 ~ 5 μm) by amount, stir, stirring velocity 1000r/min.After powder all adds, improve rotating speed to 2000r/min.After high-speed stirring disperses 1.0 hours, obtain HP230 dispersed paste.
Take 10 parts of scattered HP230 dispersed pastes respectively, 10 parts of NSI500P (Ya Ling tech materials company limited, particle diameter 500nm) and 20 parts of IPA-ST (Nissan Chemical Ind Ltd, particle diameter 10 ~ 15nm), place stand-by.
2) preparation of the anti-dazzle UV coating of water-based:
The mixed solvent of 15 parts of propylene glycol monomethyl ethers, 5 parts of Virahols, 10 parts of deionized waters is added in the agitation vat with condenser, then when at the uniform velocity stirring, by 40 parts of UCECOAT7200 water-based oligopolymer (profound new company), 20 parts of UCECOAT7699 water-based oligopolymer (profound new company), the EM235 monomer (Changxing, Taiwan company) of 20 parts, the MiramerM500 monomer (the special chemical company in U.S. source) of 20 parts adds in above-mentioned mixed solvent, it is made to be dissolved in mixed solvent, stirring velocity 800r/min.Then, add 2.0 parts of light trigger IRGACURE2959 (Ciba company), 3.0 parts of initiator IRGACURE184 (Ciba company), make it be dissolved in system.Then, add 0.4 part of DISPERBYK-180, make it be scattered in uniformly in this system.Then, add 10 parts of scattered HP230 slurry (De Qian companies gradually, particle diameter 3 ~ 5 μm), 10 parts of NSI500P (Ya Ling tech materials company limiteds, particle diameter 500nm) and 20 parts of IPA-ST (Nissan Chemical Ind Ltd, particle diameter 10 ~ 15nm), improve stirring velocity to 1000r/min, stir 1 hour.Then, add 0.8 part of BYK-333 (BYK company) in system, to stir.Before coating, add 10 parts of XD-803 solidifying agent in this water-based UV anti-glare paint, stir 5 minutes, obtain the anti-dazzle two solidification hard coating composition of water-based.
3) cured film preparation:
Use line rod spreader immediately, this cured coating fluid composition being coated on thickness is in the one side of optical grade pet film (PET film) of 125 μm, in 80 DEG C of dry 2min in an oven, be cured by the coating of UV-irradiation to drying, ultraviolet irradiation light quantity is 600mj/cm
2, the gauge control of cured coating layer is 3 ~ 4 μm, and obtained transparent hardened film work in-process, then put into 40 DEG C of thermostatic chambers, after fixing 48 hours, obtained transparent hardened film finished product.
Embodiment 2
The raw material that the present embodiment uses and consumption (parts by weight) are in table 2.
The raw material of table 2 embodiment of the present invention 2 and consumption
| Water-based aliphatic polyurethane dispersion | UCECOAT 7655 | 40 parts |
| Aqueous polyurethane acrylate | UCECOAT 7200 | 20 parts |
| Dipentaerythritol acrylate | EM 264 | 15 parts |
| Pentaerythritol triacrylate | EM 235 | 25 parts |
| Deionized water | Deionized water | 5 parts |
| 2-hydroxy-2-methyl-1-phenyl-1-acetone | IRGACURE 1173 | 3 parts |
| 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone | IRGACURE 2959 | 2 parts |
| Silicon-dioxide flatting silica | OK 520 | 10 parts |
| Organically-modified 600nm silicon-dioxide | NSI 650S | 8 parts |
| The silicon-dioxide of 70 ~ 100nm | IPA-ST-L | 15 parts |
| Containing pigment affinity groups polymer copolymerization body | DISPERBYK-184 | 0.3 part |
| Polyether-modified polydimethylsiloxane | BYK-3500 | 1.5 part |
| Water-based aliphatic isocyanates solidifying agent | Bayer-3100 | 8 parts |
| Butyl glycol ether | Butyl glycol ether | 17 parts |
| Virahol | Virahol | 3 parts |
Preparation method is as follows:
1) preparation of anti-dazzle particle slurry:
80 parts of butyl glycol ethers, 10 parts of isopropyl alcohol mixed solvents are added in the agitation vat with condenser, add 1.5 parts of dispersion agent DISPERBYK-184, stir 10 minutes, stirring velocity 800r/min, makes wetting dispersing agent be dispersed in solvent.Then add 10 parts of OK520 (Yingchuang Degussa Co., Ltd, particle diameter 3 μm) by amount, stir, stirring velocity 1000r/min.After powder all adds, improve rotating speed to 2000r/min.After high-speed stirring disperses 45 minutes, obtain OK520 dispersed paste.
Take 10 parts of scattered OK520 dispersed pastes respectively, 8 parts of NSI650S (Ya Ling tech materials company limited, particle diameter 600nm) and 15 parts of IPA-ST-L (Nissan Chemical Ind Ltd, particle diameter 70 ~ 100nm), place stand-by.
2) preparation of the anti-dazzle UV coating of water-based:
The mixed solvent of 17 parts of butyl glycol ethers, 3 parts of Virahols, 5 parts of deionized waters is added in the agitation vat with condenser, then when at the uniform velocity stirring, by 40 parts of UCECOAT7655 water-based oligopolymer (profound new company), 20 parts of UCECOAT7200 water-based oligopolymer (profound new company), 15 parts of EM264 monomers (Changxing, Taiwan company), the EM235 monomer (Changxing, Taiwan company) of 25 parts adds in above-mentioned mixed solvent, it is made to be dissolved in mixed solvent, stirring velocity 800r/min.Then, add 2.0 parts of light trigger IRGACURE2959 (Ciba company), 3.0 parts of initiator IRGACURE1173 (Ciba company), make it be dissolved in system.Then, add 0.3 part of DISPERBYK-184, make it be scattered in uniformly in this system.Then, add 10 parts of scattered OK520 (dispersed pastes gradually, 8 parts of NSI650S (Ya Ling tech materials company limiteds, particle diameter 600nm) and 15 parts of IPA-ST-L (Nissan Chemical Ind Ltd, particle diameter 70 ~ 100nm), improve stirring velocity to 1000r/min, stir 1 hour.Then, add 1.5 parts of BYK-3500 (BYK company) in system, to stir.Before coating, add 8 parts of Byer-3100 solidifying agent in this water-based UV anti-glare paint, stir 6 minutes, obtain the anti-dazzle two solidification hard coating composition of water-based.
3) cured film preparation:
Use line rod spreader immediately, this cured coating fluid composition being coated on thickness is in the one side of optical grade pet film (PET film) of 125 μm, in 80 DEG C of dry 2min in an oven, be cured by the coating of UV-irradiation to drying, ultraviolet irradiation light quantity is 600mj/cm2, the gauge control of cured coating layer is 3 ~ 4 μm, obtained transparent hardened film work in-process, then 40 DEG C of thermostatic chambers are put into, after fixing 48 hours, obtained transparent hardened film finished product.
Embodiment 3
The raw material that the present embodiment uses and consumption (parts by weight) are in table 3.
The raw material of table 3 embodiment of the present invention 3 and consumption
| Water-based aliphatic polyurethane dispersion | UCECOAT 7655 | 40 parts |
| Aliphatic polyurethane dispersion | UCECOAT 7699 | 20 parts |
| Double pentaerythritol C5 methacrylate | Miramer M500 | 40 parts |
| Deionized water | Deionized water | 6 parts |
| 1-hydroxy-cyclohexyl-phenyl ketone | IRGACURE 184 | 2 parts |
| 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone | IRGACURE 2959 | 3 parts |
| 4 ~ 5 microns of improved silicas | BED025E | 8 parts |
| The organically-modified silicon-dioxide of 500nm | NSI 500F | 10 parts |
| 10 ~ 15nm silicon-dioxide | PGM-ST | 10 parts |
| Containing pigment affinity groups polymer copolymerization body | DISPERBYK-190 | 1.0 part |
| Siloxane-Oxyalkylene Copolymers solution | BYK-346 | 1.4 part |
| Water-based isocyanate solidifying agent | Byer-2487 | 6 parts |
| Propylene glycol monomethyl ether | Propylene glycol monomethyl ether | 20 parts |
Preparation method is as follows:
1) anti-dazzle particle slurry:
Take 8 parts of BED025E (Ya Ling tech materials company limited respectively, 4 ~ 5 μm), 10 parts of NSI500F (Ya Ling tech materials company limited, 500nm) and 10 parts of PGM-ST (Misao Kusano, 10 ~ 15nm), prepare stand-by.
2) preparation of the anti-dazzle UV coating of water-based:
The mixed solvent of 20 parts of propylene glycol monomethyl ethers, 6 parts of deionized waters is added in the agitation vat with condenser, then when at the uniform velocity stirring, by 40 parts of UCECOAT7655 water-based oligopolymer (profound new company), 20 parts of UCECOAT7699 water-based oligopolymer (profound new company), 40 parts of MiramerM500 monomers (the special chemical company in U.S. source).Then, add 3.0 parts of light trigger IRGACURE2959 (Ciba company), 2.0 parts of initiator IRGACURE184 (Ciba company), make it be dissolved in system.Then, add 1 part of DISPERBYK-190, make it be scattered in uniformly in this system.Then, add 8 parts of BED025E (Hou Mao Science and Technology Ltd.s gradually, 4 ~ 5 μm), 10 parts of NSI500F (Ya Ling tech materials company limiteds, 500nm), 10 parts of PGM-ST (Misao Kusano, 10 ~ 15nm), improve stirring velocity to 1000r/min, stir 1 hour.Then, add 1.4 parts of BYK-346 (BYK company) in system, to stir.Before coating, add 6 parts of Byer-2487 solidifying agent in this water-based UV anti-glare paint, stir 5 minutes, obtain the anti-dazzle two solidification hard coating composition of water-based.
3) cured film preparation:
Use line rod spreader immediately, this cured coating fluid composition being coated on thickness is in the one side of optical grade pet film (PET film) of 125 μm, in 80 DEG C of dry 2min in an oven, be cured by the coating of UV-irradiation to drying, ultraviolet irradiation light quantity is 600mj/cm2, the gauge control of cured coating layer is 3 ~ 4 μm, obtained transparent hardened film work in-process, then 40 DEG C of thermostatic chambers are put into, after fixing 48 hours, obtained transparent hardened film finished product.
Embodiment 4
The raw material that the present embodiment uses and consumption (parts by weight) are in table 4.
The raw material of table 4 embodiment of the present invention 4 and consumption
| Aqueous polyurethane acrylate | WB-01 | 55 parts |
| Aliphatic polyurethane dispersion | UCECOAT 7733 | 15 parts |
| Pentaerythritol triacrylate | EM 235 | 10 parts |
| Double pentaerythritol C5 methacrylate | Miramer M500 | 20 parts |
| Deionized water | Deionized water | 5 parts |
| 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone | IRGACURE 2959 | 2.5 part |
| 2-hydroxy-2-methyl-1-phenyl-1-acetone | IRGACURE 1173 | 2.5 part |
| 500nm silicon-dioxide | TSD-L20D | 10 parts |
| 900nm silicon-dioxide | NSI 900 | 12 parts |
| Containing the copolymer solution of pigment affinity groups | DISPERBYK-198 | 1 part |
| Siloxane-Oxyalkylene Copolymers | BYK-348 | 1 part |
| Water-based isocyanate solidifying agent | XD-803 | 8 parts |
| Propylene glycol monomethyl ether | Propylene glycol monomethyl ether | 18 parts |
| Sec-butyl alcohol | Sec-butyl alcohol | 2 parts |
Preparation method is as follows:
1) anti-dazzle particle slurry:
Take 10 parts of TSD-L20D (Nanjing Tian Hang company limited, particle diameter 500nm) respectively, 12 parts of NSI900 (Ya Ling tech materials company limited, particle diameter 900nm), prepare stand-by.
2) preparation of the anti-dazzle UV coating of water-based:
The mixed solvent of 18 parts of propylene glycol monomethyl ethers, 2 parts of sec-butyl alcohols, 5 parts of deionized waters is added in the agitation vat with condenser, then when at the uniform velocity stirring, by 55 parts of WB-01 water-based oligopolymer (Changxing, Taiwan company), 15 parts of UCECOAT7733 water-based oligopolymer (profound new company), the EM235 monomer (Changxing, Taiwan company) of 10 parts, the MiramerM500 of 20 parts.Then, add 2.5 parts of light trigger IRGACURE2959 (Ciba company), 2.5 parts of initiator IRGACURE1173 (Ciba company), make it be dissolved in system.Then, add 1 part of DISPERBYK-198, make it be scattered in uniformly in this system.Then, add 10 parts of TSD-L20D (Nanjing Tian Hang company limited, particle diameter 500nm) gradually, 12 parts of NSI900 (Ya Ling tech materials company limited, particle diameter 900nm), improve stirring velocity to 1000r/min, stir 1 hour.Then, add 1 part of BYK-348 (BYK company) in system, to stir.Before coating, add 8 parts of XD-803 solidifying agent in this water-based UV anti-glare paint, stir 5 minutes, obtain the anti-dazzle two solidification hard coating composition of water-based.
3) cured film preparation:
Use line rod spreader immediately, this cured coating fluid composition being coated on thickness is in the one side of optical grade pet film (PET film) of 125 μm, in 80 DEG C of dry 2min in an oven, be cured by the coating of UV-irradiation to drying, ultraviolet irradiation light quantity is 600mj/cm2, the gauge control of cured coating layer is 3 ~ 4 μm, obtained transparent hardened film work in-process, then 40 DEG C of thermostatic chambers are put into, after fixing 48 hours, obtained transparent hardened film finished product.
The model that the cured film that embodiment 1 ~ 4 obtained adopts Marl, Germany company to provide is that the pin of MillimarC1216 is stepped on film thickness instrument and tested the cured film thickness obtained; Haze meter (upper Nereid's tech device Manufacturing Co., Ltd, model: WGT-S) is adopted to test total light transmittance (T) and the mist degree (H) of cured film of the present invention; On cured film surface, #0000 Steel Wool carries out wiping repeatedly, load 1000g, and frictional distance is 5 ~ 6cm, when grinding vestige according to cured film, evaluate the number of times of friction, result is as shown in table 5, and table 5 is the performance data of the cured film that the embodiment of the present invention 1 ~ 4 and comparative example 1 obtain.
The performance data of the cured film that table 5 embodiment of the present invention 1 ~ 4 obtains
As can be seen from Table 5, water-based anti-dazzle of the present invention is coated with and after product surface, can plays a protective role to product, eliminates " dazzle " simultaneously and pollutes.The coat inside particle distribution formed is even, not easily sedimentation and gathering occurs.Coating surface appearance is comparatively homogeneous, there will not be striped, grows dim, uneven problem, and, hardness and wear resistance higher.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the anti-dazzle UV coating of water-based, comprises the component of following parts by weight:
Aqueous polyurethane acrylate prepolymer: 30 ~ 90 parts;
Diluting monomer: 10 ~ 60 parts;
Anti-dazzle particle: 5 ~ 100 parts;
Water-based wetting dispersing agent: 0.05 ~ 10 part;
Water-based flow agent: 0.05 ~ 5 part;
Water: 1 ~ 20 part;
Water-soluble photoinitiator: 0.5 ~ 10 part;
Water-based isocyanate solidifying agent: 1 ~ 30 part.
2. the anti-dazzle UV coating of water-based according to claim 1, is characterized in that, described aqueous polyurethane acrylate prepolymer is two functionality and above aqueous polyurethane acrylate prepolymer;
The parts by weight of described aqueous polyurethane acrylate prepolymer are 40 ~ 80 parts.
3. the anti-dazzle UV coating of water-based according to claim 1, it is characterized in that, described diluting monomer comprises esters of acrylic acid diluting monomer;
The parts by weight of described diluting monomer are 15 ~ 50 parts.
4. the anti-dazzle UV coating of water-based according to claim 1, it is characterized in that, described anti-dazzle particle comprises one or more in silicon-dioxide, aluminum oxide, Magnesium Silicate q-agent, pure aluminium silicate, neusilin, calcium carbonate, magnesiumcarbonate, aluminium hydroxide, titanium dioxide, polypropylene, zirconium white, spherical shaped silicone particle and acrylic resin particle;
The parts by weight of the anti-dazzle particle of described water-based are 10 ~ 80 parts.
5. the anti-dazzle UV coating of water-based according to claim 1, it is characterized in that, described water-based wetting dispersing agent comprises the alkyl alcohol amine salt of high molecular weight acidic polymkeric substance, acrylic copolymer, the alkane hydroxyl amine salt of lower molecular weight polynary hydroxy acid polymkeric substance, the alkanolamine of the polymer copolymerization ester of band acidic-group, the polymeric alkylammonium salt of multiple functional radical and containing one or more in pigment affinity groups polymer copolymerization body;
The parts by weight of described water-based wetting dispersing agent are 0.1 ~ 5.
6. the anti-dazzle UV coating of water-based according to claim 1, it is characterized in that, described water-based flow agent comprises the polyether silicones of non-reactive, the organic silicon modified by polyether of response type or response type polyester resin change properties of organic silicon, esters of acrylic acid flow agent, fluorin modified crylic acid ester copolymer, sulfonate type fluorine flow agent, metal carboxylate fluorocarbon surfactant;
The parts by weight of described water-based flow agent are 0.1 ~ 2.5 part.
7. the anti-dazzle UV coating of water-based according to claim 1, is characterized in that, described water-soluble photoinitiator comprises cracking type initiator and/or hydrogen-abstraction initiator;
Described cracking type initiator comprises 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone, 1,1'-(methylene radical two-4,1-phenylene) two [2-hydroxy-2-methyl-1-acetone], 2-methyl isophthalic acid-[-4-methylthio group) phenyl]-2-morpholinyl-1-acetone, 2, one or more in 4,6-trimethylbenzoy-dipheny phosphine oxide, benzoin dimethylether, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxy-cyclohexyl-phenyl ketone and benzoyl derivatives;
Described hydrogen-abstraction initiator comprise benzophenone, 4-benzoyl-4'-methyl-diphenyl sulfide, 2-benzoyl methyl benzoate, isopropyl thioxanthone uh one or more in ketone and 4-(N, N-dimethylamino) ethyl benzoate;
The parts by weight of described water-soluble photoinitiator are 2 ~ 8 parts.
8. the anti-dazzle UV coating of the water-based according to claim 1 ~ 7 any one, is characterized in that, the anti-dazzle UV coating of described water-based also comprises aqueous solvent;
Described aqueous solvent comprises one or more in alcoholic solvent, alcohol ether solvent and solvent of ether ester type;
The parts by weight of described aqueous solvent are 5 ~ 80 parts.
9. a cured film, is obtained by the anti-dazzle UV coating of the water-based described in claim 1 ~ 8.
10. a preparation method for cured film, comprises the following steps:
A) with weight parts, by 30 ~ 90 parts of aqueous polyurethane acrylate prepolymers, 10 ~ 60 parts of diluting monomers, 5 ~ 100 parts of anti-dazzle particles, 0.05 ~ 10 part of water-based wetting dispersing agent, 0.05 ~ 5 part of water-based flow agent, 1 ~ 20 part of water, 0.5 ~ 10 part of water-soluble photoinitiator and 1 ~ 30 part of water-based isocyanate solidifying agent mixing, obtain the anti-dazzle UV coating of water-based;
B) by described steps A) the anti-dazzle UV paint of water-based that obtains at matrix surface, carry out UV-irradiation, obtain cured film work in-process;
C) by described step B) the cured film work in-process that obtain carry out thermofixation, obtain cured film.
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