CN115850768B - Low-haze anti-dazzle hardening film and preparation method thereof - Google Patents
Low-haze anti-dazzle hardening film and preparation method thereof Download PDFInfo
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- CN115850768B CN115850768B CN202211481079.5A CN202211481079A CN115850768B CN 115850768 B CN115850768 B CN 115850768B CN 202211481079 A CN202211481079 A CN 202211481079A CN 115850768 B CN115850768 B CN 115850768B
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- 238000002360 preparation method Methods 0.000 title description 5
- 238000000576 coating method Methods 0.000 claims abstract description 82
- 239000011248 coating agent Substances 0.000 claims abstract description 81
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 31
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920001577 copolymer Polymers 0.000 claims abstract description 22
- 229920005992 thermoplastic resin Polymers 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000010410 layer Substances 0.000 claims description 26
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 21
- 239000011347 resin Substances 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 18
- 239000003292 glue Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- 238000003848 UV Light-Curing Methods 0.000 claims description 10
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical group COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001723 curing Methods 0.000 claims description 9
- 239000011247 coating layer Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- -1 acrylic ester Chemical class 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000002834 transmittance Methods 0.000 abstract description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 9
- 239000004926 polymethyl methacrylate Substances 0.000 description 9
- 230000004313 glare Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009125 cardiac resynchronization therapy Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
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- Laminated Bodies (AREA)
- Optical Elements Other Than Lenses (AREA)
Abstract
The invention discloses a low-haze anti-dazzle hardening film, which comprises a substrate layer, a hardening coating and an anti-dazzle coating, wherein the hardening coating is clamped between the substrate layer and the anti-dazzle coating; the thermoplastic resin is methyl methacrylate/styrene copolymer, and the relative molecular weight of the methyl methacrylate/styrene copolymer is 8000-160000; the molar content of the methyl methacrylate in the methyl methacrylate/styrene copolymer is 55% -70%. The low-haze anti-glare hardened film has adjustable haze and light transmittance by coating anti-glare coating liquid on the surface of the hardened coating; the anti-dazzle coating liquid contains methyl methacrylate/styrene copolymer, and the molar content of methyl methacrylate in the copolymer is 55% -70%, so that the formed concave-convex microstructure is uniform in distribution and the haze of the hardened film is low.
Description
Technical Field
The invention relates to the technical field of films, in particular to a low-haze anti-dazzle hardening film and a preparation method thereof.
Background
Image displays typified by liquid crystal displays, plasma displays, CRTs are used in the optical field. The display touch panel assembled by adopting the multi-layer structure such as the glass plate, the resin film, the conductive layer and the like is realized by forming the concave-convex structure on the surface of the transparent base film because the external light source is arranged in the use environment, and the light is reflected by the surface of the display to cause a glare effect, so that the quality of a display image is influenced. The prior art has the defects that: the particles are easy to settle and hard to protrude from the surface in the coating process; the substrate base film is likely to have a problem of adhesion failure when bonded to the resin in which the fine particles are dispersed.
Disclosure of Invention
One of the purposes of the present invention is to overcome the defects existing in the prior art and provide a low-haze anti-glare hardened film, which not only has high light transmittance and good anti-glare optical properties, but also has low haze.
In order to achieve the above technical effects, the technical scheme of the invention is as follows: the low-haze anti-glare hardened film comprises a substrate layer, a hardening coating and an anti-glare coating, wherein the hardening coating is arranged between the substrate layer and the anti-glare coating, and the anti-glare coating of the anti-glare coating mainly comprises UV (ultraviolet) curing resin, thermoplastic resin, photoinitiator and a first solvent;
the thermoplastic resin is methyl methacrylate/styrene copolymer, and the relative molecular weight of the methyl methacrylate/styrene copolymer is 8000-160000;
the molar content of methyl methacrylate in the methyl methacrylate/styrene copolymer is 55% -70%.
The preferable technical scheme is as follows: the UV curing resin is polyurethane acrylic ester, and the functionality of the polyurethane acrylic ester is 2-6. The urethane acrylate is selected from one or more of Change ETERCURE 6118, U640 and ETERCURE 6145-100.
The preferable technical scheme is as follows: the first solvent is propylene glycol monomethyl ether and ethyl acetate, and the mass ratio of the propylene glycol monomethyl ether to the ethyl acetate is 1: (0.1-1).
The preferable technical scheme is as follows: the ratio of the mass of the UV curable resin to the mass of the thermoplastic resin in terms of nonvolatile matter is 1: (0.5-5).
The preferable technical scheme is as follows: the anti-dazzle coating liquid mainly comprises, by mass, 10 parts of UV curing resin, 6-25 parts of thermoplastic resin, 0.4-1 part of photoinitiator and 90-300 parts of first solvent. Further, the anti-glare coating liquid mainly comprises, by mass, 10 parts of UV curing resin, 10-25 parts of thermoplastic resin, 0.4-0.8 part of photoinitiator and 90-300 parts of first solvent.
The preferable technical scheme is as follows: the anti-dazzle coating liquid also comprises first hardening glue, wherein the mass of the first hardening glue accounts for 10-50% of the mass of the UV curing resin, and the solid content of the first hardening glue is 50-70%.
The preferable technical scheme is as follows: the main composition of the hardening coating liquid of the hardening coating comprises second hardening glue and a second solvent, and the solid content of the hardening coating liquid is 25-35%.
The preferable technical scheme is as follows: the first hardening glue and/or the second hardening glue is LUXYDIR EQS-1292.
The second object of the present invention is to overcome the defects existing in the prior art, and to provide a method for preparing a low haze antiglare hardened film, comprising the steps of:
s1: preparing a hardening film blank with a hardening coating;
s2: coating anti-dazzle coating liquid on the surface of the hardening coating of the hardening film blank, drying and curing to form an anti-dazzle coating, and preparing the low-haze anti-dazzle hardening film;
the ratio of the layer thickness of the hardened coating layer to the layer thickness of the antiglare coating layer is 1: (0.04-2), wherein the layer thickness of the hardened coating is 2-5 μm.
The preferable technical scheme is as follows: s2, setting the continuous drying temperature to 65+/-5 ℃, 75+/-5 ℃, 80+/-5 ℃, 90+/-5 ℃ and 80+/-5 ℃ in sequence; the curing energy is 480-520 mJ/cm 2 。
The invention has the advantages and beneficial effects that:
according to the low-haze anti-glare hardened film, an anti-glare coating liquid is coated on the surface of a hardened coating to form an anti-glare coating, so that the haze and the light transmittance are adjustable and controllable; the anti-dazzle coating liquid contains thermoplastic resin of methyl methacrylate/styrene copolymer, and is compounded with UV curing resin to form an anti-dazzle coating with concave-convex microstructure, the hardened film has high light transmittance and good optical property of anti-dazzle property, and the molar content of methyl methacrylate in the methyl methacrylate/styrene copolymer is in the range of 55-70%, so that the formed concave-convex microstructure is uniformly distributed and the haze of the hardened film is low.
Detailed Description
The following describes the invention in further detail with reference to examples. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
Low haze antiglare cured film
The base material layer is PET, and the thickness of the base material layer is 50-250 mu m. The composite layer of the hardening coating and the anti-glare coating improves the wear resistance of the hardening film and adjusts the haze of the hardening film. Further, the layer thickness of the hardened coating is 2 to 4 μm, and the ratio of the layer thickness of the hardened coating to the layer thickness of the antiglare coating is 1: (0.04 to 1), and further, the layer thickness of the hardened coating is 2 to 4 μm, and the ratio of the layer thickness of the hardened coating to the layer thickness of the antiglare coating is 1: (0.04-0.25). The anti-dazzle coating has the advantages that the wear resistance and hardness are reduced when the layer thickness is too small, and the anti-dazzle performance is poor; the thickness of the anti-dazzle coating layer is increased, so that the haze of the hardened film is increased, and obvious flash points appear on the film surface, namely the flash points.
Photoinitiator
The photoinitiator is one or more of PI 184, PI BP and PI MBF. Further, the photoinitiator was PI 184.
Anti-glare coating liquid
The thermoplastic resin is nonpolar resin, the UV curing resin is polar resin generally, the thermoplastic resin and the UV curing resin are compounded to form coating liquid, the solvent in the coating liquid is subjected to thermal evaporation, and the surface of the cured film layer forms a concave-convex microstructure, so that the glare of the cured film is reduced. The methyl methacrylate/styrene copolymer has excellent optical performance, and the protrusion height and the distribution morphology of the concave-convex microstructure are regulated by regulating the molar content of the methyl methacrylate in the copolymer, so that a hardened film with low haze and good anti-dazzling performance is formed. The excessive addition of the UV curing resin is accompanied by volatilization of the solvent, the two phases of the UV curing resin and the thermoplastic resin are separated, and the two phases of the methyl methacrylate/styrene copolymer are separated, so that the formation of an initial concave-convex microstructure is blocked, and the anti-dazzling performance of the hardened film is negatively influenced; too small an addition amount of the UV curable resin may cause poor leveling property of the anti-glare coating liquid, resulting in uneven distribution of the formed uneven microstructure, and uneven protrusion heights of the uneven microstructure.
The first solvent is propylene glycol monomethyl ether (PM) and Ethyl Acetate (EAC), on one hand, the leveling property of the combined solvent compounded anti-dazzle coating liquid is good, the formed anti-dazzle coating film surface is flat, and the residual solvent is less; on the other hand, the compatibility of the combination solvent compound and the methyl methacrylate/styrene copolymer is good, the distribution of the dissolved phases of the methyl methacrylate and the styrene in the first solvent is regulated, and the protrusion height and the distribution morphology of the concave-convex microstructure are further regulated.
First hardening glue
The anti-dazzle coating liquid contains first hardening glue, so that on one hand, the haze of the anti-dazzle coating is improved, and on the other hand, the adhesive force between the anti-dazzle coating and the hardening coating is improved.
Hardening coating liquid
The hardening coating liquid mainly comprises second hardening glue and a second solvent, wherein the second solvent is propylene glycol monomethyl ether.
Preparation of methyl methacrylate/styrene copolymer
The polymer is prepared by adopting a free radical polymerization method, azodiisobutyronitrile is selected as an initiator, and polymethyl methacrylate (PMMA, average molecular weight is 9000) and styrene monomer (St, solid content is more than 99.5%) are selected as raw materials. Adding PMMA and St into a reactor to form a toluene solution with the concentration of PMMA and St of 30%, introducing protective gas into the reactor, heating to 64-66 ℃, dropwise adding azodiisobutyronitrile, wherein the adding amount of the azodiisobutyronitrile is 3% of the total mass of the PMMA and St, heating to 73-75 ℃ at the heating rate of 0.5-1 ℃/10min, and preserving heat for reaction for 5h. The obtained polymer is subjected to precipitation, dissolution and reprecipitation, and the process is repeated for 3 times, and the purified polymer is dried for more than 10 hours under the vacuum condition of 35-45 ℃ for standby. The relative molecular weight of the obtained polymer is 80000-160000 measured by gel permeation chromatography.
Sample one, starting materials PMMA and St in a molar mass ratio of 30:70, the actual molar content of methyl methacrylate in the methyl methacrylate/styrene copolymer is 56%;
sample two, molar mass ratio of raw materials PMMA and St was 35:65, the actual methyl methacrylate/styrene copolymer had a methyl methacrylate molar content of 61%;
sample three, molar mass ratio of raw materials PMMA and St 40:60, the actual molar content of methyl methacrylate in the methyl methacrylate/styrene copolymer is 66%;
sample four, molar mass ratio of raw materials PMMA and St 25:75, the molar content of methyl methacrylate in the actual methyl methacrylate/styrene copolymer was 51%.
Examples 1 to 9 and comparative example 1
The composition of the anti-glare coating liquid is as follows in table 1 in parts by mass:
wherein, the mass ratio of the propylene glycol monomethyl ether to the ethyl acetate serving as the first solvent is 1:0.4.
the composition of the hardened coating liquid is as follows in parts by mass:
| second hardening glue | Propylene glycol monomethyl ether | |
| Suppliers (suppliers) | De ai Sheng | Meiji chemistry |
| Model number | LUXYDIR EQS-1292 | — |
| Hardening coating liquid | 50 | 50 |
The preparation methods of the low haze antiglare hardened films of examples 1 to 9 and comparative examples include the following steps:
s1: preparing a PET substrate layer of 100 μm, preparing a hardening coating liquid according to the above Table 2, coating a surface of the substrate layer with the hardening coating liquid, drying and curing, sequentially setting the continuous drying temperature at 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 85 deg.C, drying in a circulating oven for about 3 minutes, and further passing through a heat treatment oven of 520mJ/cm 2 Forming a hardened film blank with a hardened coating;
s2: preparing anti-glare coating liquid according to the above table 1, coating anti-glare coating liquid on the surface of the hardening coating of the hardening film blank, drying and curing, sequentially setting the continuous drying temperature to 65 ℃,75 ℃,80 ℃,90 ℃,80 ℃ and drying in a circulating oven for about 2 minutes, and then passing through a drying oven of 510mJ/cm 2 And (3) forming an anti-dazzle coating to prepare the low-haze anti-dazzle hardening film.
In the low-haze antiglare cured film, the layer thickness of the cured coating layer was 3 μm.
Performance test:
1. transmittance: instrument: NDH2000N.
2. Haze: instrument: NDH2000N.
3. Hardness: motorized pencil durometer DDQ-Y3.
4. Abrasion resistance: abrasion resistance tester WV-339.
5. Anti-glare properties: the low-haze anti-glare hardened film was placed on a green screen background of a cell phone of 200ppi and 300ppi pixels to visually observe the glare degree, and was not perceived as 1 grade; the micro-perception is class 2; the glare was perceived as grade 3.
6. Definition: sharpness meter ICM-1T.
The hardness of the hardened films of the examples and the comparative examples satisfies 500g/3H; the wear resistance is 1000g/100 times.
Experiments prove that the hardened film with the definition of more than 75 percent has no flash spots; a hardened film with a definition of 70-75% and a small amount of flash spots.
The preferred cured film satisfies: the light transmittance is more than 93%, the haze is less than 2%, the antiglare performance is grade 1, and the antiglare performance is grade 1 and the definition is more than 80.
The next hardening film satisfies: the light transmittance is more than 92%, the haze is less than 8%, the antiglare property is 200ppi and is 1 grade, and the definition is more than 70.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the scope of the invention.
Claims (6)
1. The low-haze anti-glare hardened film comprises a substrate layer, a hardening coating and an anti-glare coating, and is characterized in that the hardening coating is clamped between the substrate layer and the anti-glare coating, and an anti-glare coating liquid of the anti-glare coating mainly comprises UV (ultraviolet) curing resin, thermoplastic resin, a photoinitiator and a first solvent;
the thermoplastic resin is methyl methacrylate/styrene copolymer, and the relative molecular weight of the methyl methacrylate/styrene copolymer is 8000-160000;
the molar content of methyl methacrylate in the methyl methacrylate/styrene copolymer is 55% -70%;
the ratio of the mass of the UV curable resin to the mass of the thermoplastic resin in terms of nonvolatile matter is 1: (0.5-5);
the anti-glare coating liquid comprises, by mass, 10 parts of UV (ultraviolet) curing resin, 6-25 parts of thermoplastic resin, 0.4-1 part of photoinitiator and 90-300 parts of first solvent;
the UV curing resin is polyurethane acrylic ester, and the functionality of the polyurethane acrylic ester is 2-6;
the first solvent is propylene glycol monomethyl ether and ethyl acetate, and the mass ratio of the propylene glycol monomethyl ether to the ethyl acetate is 1: (0.1-1);
the ratio of the layer thickness of the hardened coating layer to the layer thickness of the antiglare coating layer is 1: (0.04-1), wherein the layer thickness of the cured coating is 2-4 μm.
2. The low-haze antiglare hardened film according to claim 1, wherein the antiglare coating liquid further comprises a first hardening glue, the mass of the first hardening glue is 10 to 50% of the mass of the UV-curable resin, and the solid content of the first hardening glue is 50 to 70%.
3. The low-haze antiglare cured film according to claim 2, wherein the cured coating liquid of the cured coating mainly comprises a second cured glue and a second solvent, and the cured coating liquid has a solid content of 25% to 35%.
4. The low-haze antiglare hardened film according to claim 3, wherein the first hardening glue and/or the second hardening glue is luxydireqs-1292.
5. A method for producing the low-haze antiglare hardened film according to any one of claims 1 to 4, comprising the steps of:
s1: preparing a hardening film blank with a hardening coating;
s2: and (3) coating anti-dazzle coating liquid on the surface of the hardening coating of the hardening film blank, and drying and curing to form an anti-dazzle coating to prepare the low-haze anti-dazzle hardening film.
6. The method for producing a low-haze antiglare hardened film according to claim 5, wherein the continuous drying temperature in S2 is set to 65±5 ℃,75±5 ℃,80±5 ℃,90±5 ℃,80±5 ℃ in that order; the curing energy is 480-520 mJ/cm 2 。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014071395A (en) * | 2012-10-01 | 2014-04-21 | Nippon Paper Industries Co Ltd | Anti-glare hard coat film |
| KR20170090679A (en) * | 2016-01-29 | 2017-08-08 | 주식회사 효성 | Low-haze anti-reflection film having superior transmission clarity |
| CN109810555A (en) * | 2018-12-21 | 2019-05-28 | 宁波激智科技股份有限公司 | The hardened layer coating fluid and a kind of cured film of a kind of high rigidity, anti-dazzle |
| JP2021030475A (en) * | 2019-08-19 | 2021-03-01 | 三菱瓦斯化学株式会社 | Transparent resin laminate, transparent substrate material and transparent protective material using it |
| CN114213694A (en) * | 2021-12-24 | 2022-03-22 | 苏州诺菲纳米科技有限公司 | Anti-glare film with high haze and low flash point and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4217097B2 (en) * | 2003-04-03 | 2009-01-28 | ダイセル化学工業株式会社 | Anti-glare film |
| JP2010066469A (en) * | 2008-09-10 | 2010-03-25 | Daicel Chem Ind Ltd | Antiglare film and method for manufacturing the same |
| JP2010066470A (en) * | 2008-09-10 | 2010-03-25 | Daicel Chem Ind Ltd | Antiglare film and method for manufacturing the same |
| TWI693734B (en) * | 2019-05-16 | 2020-05-11 | 明基材料股份有限公司 | Anti-glare film and polarizer with the same |
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- 2022-11-24 CN CN202211481079.5A patent/CN115850768B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014071395A (en) * | 2012-10-01 | 2014-04-21 | Nippon Paper Industries Co Ltd | Anti-glare hard coat film |
| KR20170090679A (en) * | 2016-01-29 | 2017-08-08 | 주식회사 효성 | Low-haze anti-reflection film having superior transmission clarity |
| CN109810555A (en) * | 2018-12-21 | 2019-05-28 | 宁波激智科技股份有限公司 | The hardened layer coating fluid and a kind of cured film of a kind of high rigidity, anti-dazzle |
| JP2021030475A (en) * | 2019-08-19 | 2021-03-01 | 三菱瓦斯化学株式会社 | Transparent resin laminate, transparent substrate material and transparent protective material using it |
| CN114213694A (en) * | 2021-12-24 | 2022-03-22 | 苏州诺菲纳米科技有限公司 | Anti-glare film with high haze and low flash point and preparation method thereof |
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