CN117665980A - Restorative antiglare film - Google Patents
Restorative antiglare film Download PDFInfo
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- CN117665980A CN117665980A CN202211048929.2A CN202211048929A CN117665980A CN 117665980 A CN117665980 A CN 117665980A CN 202211048929 A CN202211048929 A CN 202211048929A CN 117665980 A CN117665980 A CN 117665980A
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- meth
- restorative
- antiglare
- weight
- antiglare film
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- 239000002245 particle Substances 0.000 claims abstract description 63
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 46
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 34
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- 239000000758 substrate Substances 0.000 claims abstract description 25
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 claims abstract description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 37
- -1 siloxane structure Chemical group 0.000 claims description 27
- 230000003746 surface roughness Effects 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 7
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- 125000002723 alicyclic group Chemical group 0.000 description 2
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- 125000003118 aryl group Chemical group 0.000 description 2
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 2
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- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- KCZQSKKNAGZQSZ-UHFFFAOYSA-N 1,3,5-tris(6-isocyanatohexyl)-1,3,5-triazin-2,4,6-trione Chemical compound O=C=NCCCCCCN1C(=O)N(CCCCCCN=C=O)C(=O)N(CCCCCCN=C=O)C1=O KCZQSKKNAGZQSZ-UHFFFAOYSA-N 0.000 description 1
- 229940043375 1,5-pentanediol Drugs 0.000 description 1
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 description 1
- ZJWDJIVISLUQQZ-UHFFFAOYSA-N 2,4-dimethylpentane-1,5-diol Chemical compound OCC(C)CC(C)CO ZJWDJIVISLUQQZ-UHFFFAOYSA-N 0.000 description 1
- AOFFRVQVWKIQEV-UHFFFAOYSA-N 2-(2-hydroxy-4-prop-2-enoyloxybutoxy)carbonylbenzoic acid Chemical compound C=CC(=O)OCCC(O)COC(=O)C1=CC=CC=C1C(O)=O AOFFRVQVWKIQEV-UHFFFAOYSA-N 0.000 description 1
- AJKXDPSHWRTFOZ-UHFFFAOYSA-N 2-ethylhexane-1,6-diol Chemical compound CCC(CO)CCCCO AJKXDPSHWRTFOZ-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical class OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 description 1
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 description 1
- QWGRWMMWNDWRQN-UHFFFAOYSA-N 2-methylpropane-1,3-diol Chemical compound OCC(C)CO QWGRWMMWNDWRQN-UHFFFAOYSA-N 0.000 description 1
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000005058 Isophorone diisocyanate Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
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- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
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- 229910000831 Steel Inorganic materials 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
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- 239000002216 antistatic agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- KORSJDCBLAPZEQ-UHFFFAOYSA-N dicyclohexylmethane-4,4'-diisocyanate Chemical compound C1CC(N=C=O)CCC1CC1CCC(N=C=O)CC1 KORSJDCBLAPZEQ-UHFFFAOYSA-N 0.000 description 1
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- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical group OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
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- 229920001296 polysiloxane Polymers 0.000 description 1
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Abstract
The present invention provides a restorable antiglare film comprising a transparent substrate and a restorable antiglare layer formed on the transparent substrate, wherein the restorable antiglare layer comprises an amino (meth) acrylate copolymer containing a siloxane group and a plurality of (meth) acrylate resin particles, wherein the amino (meth) acrylate copolymer has a weight average molecular weight (Mw) of between 4,000 and 60,000, and the (meth) acrylate resin particles have a 30% compressive strength of 14.7MPa to 49MPa and a recovery ratio of 22% or more. The restorative antiglare film can provide scratch restorability and stable and reliable antiglare property.
Description
Technical Field
The present invention relates to an antiglare film usable for an image display apparatus, and more particularly, to a restorative antiglare film which can provide scratch restorability and stable and reliable antiglare properties.
Background
With the increasing development of display technology, image display devices such as Liquid Crystal Displays (LCDs), organic light emitting diode displays (OLEDs), etc., demands for display performance such as high contrast ratio, wide viewing angle, high luminance, thin, large, high definition, and additional function diversification have been widely put forward.
As hand-held products increase, the surface of the display needs to have abrasion resistance to maintain the definition and visibility of the display image. Therefore, a hard coating is generally used on a display surface, and scratches are suppressed by using the hardness and lubricity of the hard coating to protect the display surface.
Also disclosed in the art is a self-repairable paint protective coating which utilizes rubber-like elasticity and lubricity for inhibiting surface scratches. This scratch-inhibiting protective coating is not suggested for use on display surfaces because of its light reflectivity. Although silica particles may be added to the protective coating to increase the haze of the protective layer and reduce the light reflectivity of the protective layer, the addition of the particles may destroy the self-healing properties of the protective layer, such that a coating thickness of at least 15 μm is required to achieve the self-healing properties of the protective layer, and a greater thickness is required to achieve the desired healing properties.
The invention provides an antiglare film with self-repairing property, which provides stable and excellent antiglare property under scratch repairing property.
Disclosure of Invention
The purpose of the present invention is to provide a restorative antiglare film that has scratch-repairing properties and provides stable and satisfactory antiglare properties.
The restorable antiglare film of the present invention comprises a transparent substrate and a restorable antiglare layer on the transparent substrate, wherein the restorable antiglare layer comprises an amino (meth) acrylate copolymer containing a siloxane group and a plurality of (meth) acrylate resin particles, wherein the (meth) acrylate resin particles have a 30% compressive strength of 14.7 to 49MPa and a restoration rate of 22% or more.
In the restorative antiglare layer of the restorative antiglare film of the present invention, the particle diameter of the (meth) acrylic resin particles is between 1 μm and 15 μm, and preferably between 2 μm and 12 μm, and the amount of the (meth) acrylic resin particles used is between 1 part by weight and 20 parts by weight, and preferably between 1 part by weight and 18 parts by weight, per one hundred parts by weight of the amino (meth) acrylic copolymer.
In the restorative antiglare layer of the restorative antiglare film of the present invention, the hysteresis loss (hysteresis loss) of the (meth) acrylic resin particles is not more than 30%, and preferably not more than 25%.
In the restorative antiglare layer of the restorative antiglare film of the present invention, the product of the particle diameter of the (meth) acrylic resin particles and the amount of the (meth) acrylic resin particles used per one hundred parts by weight of the amino (meth) acrylic copolymer is between 10 and 55.
In the restorative antiglare film of the present invention, the thickness of the restorative antiglare layer is between 3 μm and 15 μm, preferably between 3 μm and 12 μm.
In the restorative antiglare film of the present invention, the surface roughness of the restorative antiglare film is such that the arithmetic average height Ra is between 0.14 and 0.75 μm, the maximum height Ry is between 1.00 and 6.50 μm, the ten-point average roughness Rz is between 0.70 and 3.50 μm, the single-peak average spacing S is between 0.050 and 0.300 μm, and the average peak spacing Sm is between 0.30 and 0.55 μm.
In the restorative antiglare layer of the restorative antiglare film of the present invention, the amino (meth) acrylate copolymer is represented by formula (I) and has a weight-average molecular weight (Mw) of from 4,000 to 60,000,
wherein M1 and M2 are respectively carbamate chain segments, and Q is a siloxane structure shown as formula (II)
Wherein Z1 and Z2 are each hydrogen or C1 to C4 alkyl, a is an integer of 2 to 70, and the siloxane structure accounts for 1 to 10 mass percent of the total mass of the amino (meth) acrylate copolymer.
In still another embodiment of the restorative antiglare film according to the present invention, the restorative antiglare film may further incorporate a leveling agent of a (meth) acryl-modified organosilicon compound having a perfluoropolyether functional group in the restorative antiglare layer.
According to a preferred embodiment of the restorative antiglare film of the present invention, the leveling agent is used in an amount of 0.3 to 1.0 parts by weight, preferably 0.4 to 0.8 parts by weight per one hundred parts by weight of the amino (meth) acrylate copolymer in the restorative antiglare layer.
Another object of the present invention is to provide a method for producing a restorable antiglare film, comprising uniformly mixing an amino (meth) acrylate copolymer and a plurality of (meth) acrylate resin particles to form a restorable antiglare solution, coating the restorable antiglare solution on a transparent substrate, drying the substrate coated with the restorable antiglare solution, and then curing by radiation or electron beam to form the restorable antiglare film.
The above summary is intended to provide a simplified illustration of the disclosure so that the reader will provide a basic understanding of the disclosure. This summary is not an extensive overview of the disclosure and is intended to neither identify key/critical elements of the embodiments of the invention nor delineate the scope of the invention. The basic spirit of the present invention and the technical means and embodiments adopted by the present invention will be readily apparent to those having ordinary skill in the art to which the present invention pertains from consideration of the following embodiments.
Detailed Description
In order that the manner in which the invention is described above in a complete and thorough description of the invention, an illustrative description of embodiments and specific examples of the invention is provided below; this is not the only form of practicing or implementing the invention as embodied. The embodiments disclosed below may be combined with or substituted for each other where advantageous, and other embodiments may be added to one embodiment without further description or illustration.
The advantages, features, and technical approaches to the present invention will be more readily understood by reference to the following detailed description of exemplary embodiments and may be embodied in various forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed to provide a thorough and complete understanding of the present invention by those skilled in the art, and will only be defined by the appended claims.
And unless otherwise defined, all terms (including technical and scientific terms) and terminology used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and terms such as commonly used dictionaries should be interpreted as having a meaning that is consistent with the context of the relevant art and will not be interpreted in an excessively idealized or overly formal sense unless expressly so defined herein.
In addition, herein, the term "(meth) acrylate" refers to methacrylate and acrylate; the "30% compressive strength" is the compressive stress to which the (meth) acrylic resin particles undergo a 30% deformation in particle diameter during compression; the "recovery rate" is a particle diameter recovery ratio of the (meth) acrylic resin particles when the stress is reduced to 1.96mN after the stress is applied to 9.81 mN; and "hysteresis loss" is the energy lost in the recovery period of the deformation of the (meth) acrylic resin particles after the stress is applied, and represents the deformation recovery rate of the particles after the stress is applied.
An object of the present invention is to provide a restorative antiglare film having both scratch-repairing property and good antiglare property.
The restorable antiglare film of the present invention comprises a transparent substrate and a restorable antiglare layer on the transparent substrate, wherein the restorable antiglare layer comprises an amino (meth) acrylate copolymer containing a siloxane group and a plurality of (meth) acrylate resin particles, wherein the (meth) acrylate resin particles have a 30% compressive strength of 14.7 to 49MPa and a restoration rate of 22% or more.
In one embodiment of the restorative antiglare film of the present invention, a film material having good mechanical strength and light transmittance may be selected as a suitable substrate, and it may be, but is not limited to, a resin film material of polymethyl methacrylate (PMMA), polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polycarbonate (PC), triacetyl cellulose (TAC), polyimide (PI), polyethylene (PE), polypropylene (PP), polyvinyl alcohol (PVA), polyvinyl chloride (PVC), or Cyclic Olefin Copolymer (COC), etc.
In a preferred embodiment of the restorative antiglare film of the present invention, the substrate is preferably selected to have a light transmittance of 80% or more, and more preferably 90% or more. The thickness of the substrate is between about 10 μm and 500. Mu.m, preferably between 15 μm and 250. Mu.m, particularly preferably between 20 μm and 100. Mu.m.
In the restorative antiglare film of the present invention, the thickness of the restorative antiglare layer may be between 3 μm and 15 μm, preferably between 3 μm and 12 μm. In a preferred embodiment of the restorative antiglare film of the present invention, if the thickness of the restorative antiglare layer is too thin, it is difficult to provide good scratch restorability; if the thickness of the restorative antiglare layer is too thick, the antiglare property is not expected.
In the restorative antiglare layer of the restorative antiglare film of the present invention, the amino (meth) acrylate copolymer is represented by formula (I) and has a weight-average molecular weight (Mw) of from 4,000 to 60,000
Wherein M1 and M2 are respectively carbamate chain segments, and Q is a siloxane structure shown as formula (II)
Wherein Z1 and Z2 are each hydrogen or C1 to C4 alkyl, a is an integer from 2 to 70, and the siloxane structure comprises 1 to 10 weight percent of the total weight of the amino (meth) acrylate copolymer.
In a preferred embodiment of the present invention, the amino (meth) acrylate copolymer contains a urethane segment M1 formed by reacting a polyfunctional isocyanate with a hydroxyl group. The polyfunctional isocyanate suitable for the present invention is a polyisocyanate having 3 to 6 isocyanate groups and is a polyisocyanate oligomer containing an isocyanurate ring polymerized from an aliphatic diisocyanate. Suitable aliphatic diisocyanates in the amine (meth) acrylate copolymers of the present invention may be, for example, one of Hexamethylene Diisocyanate (HDI) adduct, HDI isocyanurate polyisocyanate, HDI dimer, isophorone diisocyanate, or a combination thereof, but are not limited thereto.
In a preferred embodiment of the invention, the amino (meth) acrylate copolymer contains a urethane segment M2 formed by the reaction of a polycarbonate diol and a diisocyanate. Suitable diol compounds in the amino (meth) acrylate copolymer of the present invention may be, for example, one of 1, 4-butanediol, 1, 5-pentanediol, 1, 6-hexanediol, 1, 8-octanediol, 2-methyl-1, 3-propanediol, 2-ethyl-1, 6-hexanediol, 2, 4-dimethyl-1, 5-pentanediol, a diol compound containing an alicyclic or aromatic ring, or a combination thereof, but are not limited thereto. The diisocyanate suitable for the present invention may be, for example, one of Hexamethylene Diisocyanate (HDI), isophorone diisocyanate (IPDI), trimethylhexamethylene diisocyanate (TMDI), dicyclohexylmethane-4, 4' -diisocyanate (HMDI), or a combination thereof, but is not limited thereto.
As the amino (meth) acrylate copolymer used in the restorative antiglare film of the present invention, commercially available products such as "AUP-727", "AUP-828", "AUP-838C", "AUP-849" or "AUP-1410" manufactured by Tokushiki Co., ltd. In Japan can be preferably used.
In the restorative antiglare film of the present invention, the particle diameter of the (meth) acrylic resin particles used in the restorative antiglare layer is between 1 μm and 15 μm, and preferably between 2 μm and 12 μm, and the amount of the (meth) acrylic resin particles used may be between 1 part by weight and 20 parts by weight, and preferably between 1 part by weight and 18 parts by weight, per one hundred parts by weight of the amino (meth) acrylic acid ester copolymer.
In the restorative antiglare layer of the restorative antiglare film of the present invention, the product of the particle diameter of the (meth) acrylic resin particles and the amount of the (meth) acrylic resin particles used per one hundred parts by weight of the amino (meth) acrylate copolymer is between 10 and 55, and preferably between 10 and 40. In the restorative antiglare film of the present invention, the restorative antiglare film of the present invention can be obtained by adjusting the particle diameter of the (meth) acrylic resin particles and the amount of the amino (meth) acrylic copolymer used per one hundred parts by weight of the (meth) acrylic resin particles.
In the restorative antiglare film of the present invention, the hysteresis loss (hysteresis loss) of the (meth) acrylic resin particles of the restorative antiglare layer is not more than 30%, and preferably not more than 25%.
In the restorative antiglare film of the present invention, the (meth) acrylic resin particles of the restorative antiglare layer are derived by polymerizing 80 to 20 weight percent of a crosslinkable oligomer obtained by reacting a polyol, a polyisocyanate and a (meth) acrylic ester having a hydroxyl group, and 20 to 80 weight percent of a monofunctional (meth) acrylic monomer mixture, and the crosslinkable oligomer has an acrylic equivalent weight of 400 to 600 g/mol. When the crosslinkable oligomer has too low or too high acrylic equivalent weight, the (meth) acrylic resin particles cannot have proper flexibility. In addition, the crosslinkable oligomer, after curing alone, has a glass transition temperature (Tg) of between 0 and 30℃and preferably between 0 and 25 ℃. When Tg is less than 0 ℃, the (meth) acrylic resin particles may have tackiness; when Tg is more than 30 ℃, it is difficult to obtain (meth) acrylic resin particles having high reversion properties.
In one (meth) acrylic resin particle embodiment of the present invention, a polyol suitable for preparing the crosslinkable oligomer may be, for example, but not limited to, one of polycarbonate polyol, polyester polyol, polyether polyol, aliphatic hydrocarbon polyol, alicyclic hydrocarbon polyol, etc., or a combination thereof. And the polyol preferably has 2 to 4 hydroxyl groups and a number average molecular weight (Mn) of 200 to 3000.
In the (meth) acrylic resin particles of the present invention, the isocyanate suitable for preparing the crosslinkable oligomer may be used as those well known in the art, and is not particularly limited, for example, aromatic polyisocyanate, aromatic aliphatic polyisocyanate, aliphatic polyisocyanate or alicyclic polyisocyanate, and the like.
In one embodiment of the (meth) acrylic resin particles of the present invention, the (meth) acrylic ester having a hydroxyl group suitable for preparing the crosslinkable oligomer may be, for example, one of or a combination of 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl methacrylate, 2-hydroxypropyl acrylate, 4-hydroxybutyl acrylate, caprolactone-modified 2-hydroxyethyl acrylate, polyethylene glycol mono (meth) acrylate, polypropylene glycol monoacrylate, 2- (meth) acryloyloxyethyl-2-hydroxyethyl phthalate, pentaerythritol triacrylate, and the like, but is not limited thereto.
In one embodiment of the (meth) acrylic resin particles of the present invention, the monofunctional (meth) acrylic monomer is a (meth) acrylic ester obtained by esterifying an alcohol compound having 1 to 8 carbon atoms, and is not particularly limited, and may be, for example, one of methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, and pentyl (meth) acrylate, or a combination thereof.
In a preferred embodiment of the present invention, wherein the (meth) acrylic resin particles may further have a structure derived from other monomers such as 2-ethylhexyl (meth) acrylate, methyl methacrylate, styrene, acryloylmorpholine, phenoxyethyl (meth) acrylate, phenoxypropyl (meth) acrylate, benzyl (meth) acrylate, polyethoxyphenyl (meth) acrylate, phenylbenzyl (meth) acrylate, o-phenylphenol (meth) acrylate, cyclohexyl (meth) acrylate, dicyclopentenyl (meth) acrylate, dicyclopentanyl (meth) acrylate, ethylene glycol di (meth) acrylate, propylene glycol di (meth) acrylate, 1, 4-butanediol-di (meth) acrylate, 1, 6-hexanediol-di (meth) acrylate, 1, 9-nonanediol-di (meth) acrylate, and the like by containing the monomers upon polymerization. The other monomers may be used alone or in combination of two or more.
The (meth) acrylic resin particles used in the restorative antiglare film of the present invention are preferably commercially available, for example, TECHPOLYMER manufactured by Sekisui Kasei Co., ltd., japan TM MB series, MBP series, ACP series, ACX series, e.g., MB-8C, MBP-8, ACX-806C, ACX-1502C, XX-5214Z, XX3954Z, etc.
According to the restorative antiglare film of the present invention, the surface roughness of the antiglare layer is such that the arithmetic average height Ra is between 0.14 and 0.75 μm, the maximum height Ry is between 1.00 and 6.50 μm, the ten-point average roughness Rz is between 0.70 and 3.50 μm, the single peak average spacing S is between 0.050 and 0.300 μm, and the average peak spacing Sm is between 0.30 and 0.55 μm.
The restorative antiglare film of the present invention can repair and restore the surface immediately when the surface is slightly damaged or scratched, while providing stable and excellent antiglare properties.
In still another embodiment of the restorable antiglare film of the present invention, a leveling agent of a (meth) acryl-modified organosilicon compound having a perfluoropolyether functional group is added to the restorable antiglare layer to provide a coating surface with good coating or flatness, and also to provide the antiglare film with good antifouling property and abrasion resistance. The organosilicon compound has a number average molecular weight (Mn) of between 1,500 and 16,000. Suitable leveling agents for the (meth) acryl-modified organosilicon compounds of the perfluoropolyether function are, for example, but not limited to, as commercially available X-71-1203E, KY-1203, KY-1211 or KY-1207 (from the more chemical industry, japan).
In one embodiment of the present invention, the leveling agent is used in an amount of 0.3 to 1.0 parts by weight, preferably 0.4 to 0.8 parts by weight, per one hundred parts by weight of the amino (meth) acrylate copolymer.
Another object of the present invention is to provide a method for producing a restorable antiglare film, comprising uniformly mixing an amino (meth) acrylate copolymer and a plurality of (meth) acrylate resin particles to form a restorable antiglare solution, coating the restorable antiglare solution on a transparent substrate, drying the substrate coated with the restorable antiglare solution, and then curing by radiation or electron beam to form the restorable antiglare film.
The solvent used in the method for producing an antiglare film of the present invention may be an organic solvent widely used in this technical field, for example, ketones, aliphatic or alicyclic hydrocarbons, aromatic hydrocarbons, ethers, esters or alcohols, etc. One or more organic solvents may be used in both the acrylate composition and the antiglare solution, and suitable solvents include, but are not limited to, acetone, butanone, cyclohexanone, methyl isobutyl ketone, hexane, cyclohexane, methylene chloride, dichloroethane, toluene, xylene, propylene glycol methyl ether, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, isopropyl alcohol, n-butanol, isobutyl alcohol, cyclohexanol, diacetone alcohol, propylene glycol methyl ether acetate, tetrahydrofuran, and the like, or the like.
In other embodiments of the present invention, additives such as antistatic agents, colorants, flame retardants, ultraviolet absorbers, antioxidants, surface modifiers, leveling agents without polyether modification, and defoamers may also be added to the prepared restorative antiglare solution as desired to provide different functional properties.
The method for applying the restorative antiglare solution may be, for example, a roll coating method, a doctor blade coating method, a dip coating method, a roll coating method, a spin coating method, a spray coating method, a slit coating method, or other coating methods widely used in the art.
The following examples serve to further illustrate the invention, without restricting the scope of the invention.
Examples
Example 1: preparation of restorative antiglare film
9 parts by weight of an amino (meth) acrylate copolymer (AUP-828, available from Tokushiki Co., ltd., japan), 1 part by weight of (meth) acrylic resin particles (XX-5214Z, available from Sekisui Kasei Co., ltd., japan) having a particle diameter of 3 μm, and 20 parts by weight of methyl isobutyl ketone (MIBK) were mixed and stirred for 1 hour to uniformly disperse, thereby forming a restorative antiglare solution. The restorative antiglare solution was coated on a polyethylene terephthalate (PET) substrate having a thickness of 80 μm, and dried at 80 ℃ to form a restorative antiglare layer having a thickness of 9.3 μm on the PET substrate.
The obtained antiglare film was measured for transmittance, haze, antiglare property, recovery and surface roughness by the optical measurement method described later, and the results are shown in tables 1 and 2 below.
Example 2: preparation of restorative antiglare film
5.6 parts by weight of an amino (meth) acrylate copolymer (AUP-828, available from Tokushiki Co., ltd., japan), 0.99 parts by weight of (meth) acrylic resin particles (XX-5214Z, available from Sekisui Kasei Co., ltd., japan) having a particle diameter of 3 μm, and 13.32 parts by weight of methyl isobutyl ketone (MIBK) were mixed and stirred for 1 hour to uniformly disperse, thereby forming a restorative antiglare solution. The restorative antiglare solution was coated on a polyethylene terephthalate (PET) substrate having a thickness of 80 μm, and dried at 80 ℃ to form a restorative antiglare layer having a thickness of 7.3 μm on the PET substrate.
The obtained antiglare film was measured for transmittance, haze, antiglare property, recovery and surface roughness by the optical measurement method described later, and the results are shown in tables 1 and 2 below.
Example 3: preparation of restorative antiglare film
5.6 parts by weight of an amino (meth) acrylate copolymer (AUP-828, available from Tokushiki Co., ltd., japan), 0.06 parts by weight of (meth) acrylic resin particles (XX-3954Z, available from Sekisui Kasei Co., ltd., japan) having a particle diameter of 10 μm, and 11.4 parts by weight of methyl isobutyl ketone (MIBK) were mixed and stirred for 1 hour to uniformly disperse, thereby forming a restorative antiglare solution. The restorative antiglare solution was coated on a polyethylene terephthalate (PET) substrate having a thickness of 80 μm, and dried at 80 ℃ to form a restorative antiglare layer having a thickness of 9.4 μm on the PET substrate.
The obtained antiglare film was measured for transmittance, haze, antiglare property, recovery and surface roughness by the optical measurement method described later, and the results are shown in tables 1 and 2 below.
Example 4: preparation of restorative antiglare film
5.6 parts by weight of an amino (meth) acrylate copolymer (AUP-828, available from Tokushiki Co., ltd., japan), 0.18 parts by weight of (meth) acrylic resin particles (XX-3954Z, available from Sekisui Kasei Co., ltd., japan) having a particle diameter of 10 μm, and 11.65 parts by weight of methyl isobutyl ketone (MIBK) were mixed and stirred for 1 hour to uniformly disperse, thereby forming a restorative antiglare solution. The restorative antiglare solution was coated on a polyethylene terephthalate (PET) substrate having a thickness of 80 μm, and dried at 80 ℃ to form a restorative antiglare layer having a thickness of 8.0 μm on the PET substrate.
The obtained antiglare film was measured for transmittance, haze, antiglare property, recovery and surface roughness by the optical measurement method described later, and the results are shown in tables 1 and 2 below.
Example 5: preparation of restorative antiglare film
9 parts by weight of an amino (meth) acrylate copolymer (AUP-828, available from Tokushiki Co., ltd., japan), 1 part by weight of (meth) acrylic resin particles (XX-5214Z, available from Sekisui Kasei Co., ltd., japan), 0.013 part by weight of a (meth) acryl-modified silicone compound (KY-1203E, available from Shin-Etsu Chemical Co., ltd., japan) having a perfluoropolyether functional group, and 20 parts by weight of methyl isobutyl ketone (MIBK) were mixed and stirred for 1 hour to uniformly disperse them, thereby forming a restorative antiglare solution. The restorative antiglare solution was coated on a polyethylene terephthalate (PET) substrate having a thickness of 80 μm, and dried at 80 ℃ to form a restorative antiglare layer having a thickness of 7.5 μm on the PET substrate.
The obtained antiglare film was measured for transmittance, haze, antiglare property, recovery, surface abrasion resistance and roughness by the optical measurement method described later, and the results are shown in tables 1 and 2 below.
Optical measuring method
The restorative antiglare film produced in the foregoing example was optically measured according to the measurement method of Japanese Industrial Standard (JIS).
Light transmittance measurement: the measurement was performed by using an NDH-2000 haze meter (manufactured by Nippon Denshoku industries Co., ltd.) according to the measurement method of JIS K7361.
Measurement of haze: haze was evaluated according to the description of JIS K7136 using NDH-2000 (manufactured by Nippon electric color industry Co., ltd.).
Measurement of antiglare properties: the restorative antiglare film was glued to a black acrylic plate, the surface of the antiglare film was reflected by 2 solar lights, and the antiglare property of the antiglare film was evaluated on the following 2 scales by visually comparing the degree of blooming of the fluorescent lights.
X: the separated 2 fluorescent tubes can be clearly seen, and the outline of the fluorescent tube can be clearly distinguished to be linear;
o: the separated 2 fluorescent tubes cannot be clearly seen.
Surface roughness measurement
Measurement of surface roughness: surface roughness measurement the average spacing (Sm) of the irregularities on the surface of the restorative antiglare film, the arithmetic average roughness (Ra) and the maximum roughness (Ry) of the irregularities were measured by using a MITUTOYO Formtracer CS-5000 surface roughness and profile measuring instrument according to JIS B0601-1994 method.
Method for measuring recovery and abrasion resistance
Restorative measurement: brass brush was used on the surface of the restorative antiglare film at 100gf/cm 2 Is rubbed back and forth 10 times within 20 seconds under a rubbing load of 20 seconds, and after the scratch is formed on the surface of the antiglare layer for five minutes, it is confirmed whether the scratch is disappeared.
O: no scratch was found on the surface;
x: scratches were found on the surface.
Abrasion resistance measurement: on the surface of the restorative antiglare film, #0000 steel wool was used at 200gf/cm 2 Is rubbed back and forth at a speed of 60rpm for 10 times, and then, whether the surface of the restorative antiglare layer is scratched or not is observed with eyes.
O: no scratches were found on the surface;
x: scratches were found on the surface.
Table 1: optical measurement results of antiglare films of examples 1 to 5
Note 1: the amount used per hundred parts by weight of particles of the amino (meth) acrylate copolymer
Table 2: surface roughness measurement results of antiglare films of examples 1 to 5
As shown in tables 1 and 2, the restorative antiglare films prepared in examples 1 to 5 of the present invention have good light transmittance and provide excellent haze and antiglare properties, and have good restorability. Meanwhile, the restorative antiglare film has a fine surface with an arithmetic average height Ra of 0.151 to 0.688 μm, a maximum height Ry of 1.076 to 5.695 μm, a ten-point average roughness Rz of 0.716 to 3.325 μm, a single peak average spacing S of 0.062 to 0.256 μm, and an average peak spacing Sm of 0.411 to 0.532 μm. In addition, the restorative antiglare film produced in example 5 contains a leveling agent of a (meth) acryl-modified organosilicon compound having a perfluoropolyether functional group, and has excellent abrasion resistance while having excellent light transmittance, antiglare property and restorability.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited thereto, and that various changes and modifications may be made by any person skilled in the art without departing from the spirit and scope of the present invention, and therefore, the scope of the present invention should be defined as set forth in the appended claims.
Claims (10)
1. A restorative antiglare film, comprising:
a transparent substrate; and
a restorative antiglare layer on the transparent substrate, and the restorative antiglare layer comprises:
amino (meth) acrylate copolymers containing siloxane groups; and
a plurality of (meth) acrylic resin particles having a 30% compressive strength of 14.7 to 49MPa and a recovery ratio of 22% or more.
2. The restorative antiglare film according to claim 1, wherein the particle diameter of the (meth) acrylic resin particles of the restorative antiglare layer is between 1 μm and 15 μm, and the amount of the (meth) acrylic resin particles used is between 1 part by weight and 20 parts by weight per one hundred parts by weight of the amino (meth) acrylic copolymer.
3. The restorative antiglare film according to claim 2, the particle diameter of the (meth) acrylic resin particles of the restorative antiglare layer is between 2 μm and 12 μm, and the amount of the (meth) acrylic resin particles used is between 1 part by weight and 18 parts by weight per one hundred parts by weight of the amino (meth) acrylic copolymer.
4. The restorative antiglare film according to claim 1, wherein a product of a particle diameter of the (meth) acrylic resin particles in the restorative antiglare layer and a usage amount of the (meth) acrylic resin particles per one hundred parts by weight of the amino (meth) acrylate copolymer is between 10 and 55.
5. The restorative antiglare film of claim 1, the restorative antiglare layer having a thickness of between 3 μιη to 15 μιη.
6. The restorative antiglare film according to claim 1, having a surface roughness of: the arithmetic mean height Ra is between 0.14 and 0.75 μm, the maximum height Ry is between 1.00 and 6.50 μm, the ten-point mean roughness Rz is between 0.70 and 3.50 μm, the single peak mean spacing S is between 0.050 and 0.300 μm, and the mean peak spacing Sm is between 0.30 and 0.55 μm.
7. The restorative antiglare film according to claim 1, wherein the amino (meth) acrylate copolymer is represented by formula (I) and has a weight average molecular weight (Mw) of from 4,000 to 60,000,
wherein M1 and M2 are respectively carbamate chain segments, and Q is a siloxane structure shown as formula (II)
Wherein Z1 and Z2 are each hydrogen or C1 to C4 alkyl, a is an integer of 2 to 70, and the siloxane structure accounts for 1 to 10 mass percent of the total mass of the amino (meth) acrylate copolymer.
8. The restorative antiglare film according to claim 1, wherein the (meth) acrylate resin particles of the restorative antiglare layer have a hysteresis loss of not more than 30%.
9. The restorative antiglare film according to claim 1, wherein the restorative antiglare layer further comprises a leveling agent of a (meth) acryl-modified organosilicon compound having a perfluoropolyether functional group.
10. The restorative antiglare film according to claim 9, wherein the leveling agent of the (meth) acryl-modified organosilicon compound having a perfluoropolyether functional group is used in an amount of 0.3 to 1.0 parts by weight per one hundred parts by weight of the amino (meth) acrylate copolymer.
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