CN113204063A - Anti-static antireflection optical film, anti-static coating liquid, antireflection coating liquid, preparation method and application - Google Patents
Anti-static antireflection optical film, anti-static coating liquid, antireflection coating liquid, preparation method and application Download PDFInfo
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Abstract
The invention relates to an anti-static antireflection optical film, an anti-static masking liquid, an antireflection masking liquid, a preparation method and application. Wherein, prevent static antireflection optical film includes: the flexible substrate and the anti-static coating layers attached to the surfaces of the two sides of the flexible substrate, wherein an antireflection coating layer is also attached to the anti-static coating layer on at least one side; the optical film is obtained by firstly coating antistatic masking liquid on the surfaces of two sides of a flexible substrate, then coating antireflection masking liquid after pre-drying, and then pre-drying and ultraviolet curing again. The optical film has low reflectivity, high transmissivity and excellent antistatic performance.
Description
Technical Field
The invention relates to a flexible antistatic antireflection optical film for a display device and a preparation method and application thereof.
Background
The 21 st century is an information age, and the application of electronic products has penetrated into the aspects of social life and become an indispensable tool and a necessity of daily life. In recent years, various display devices are widely applied to various electronic products, the display devices are easily affected by external light to cause display quality reduction, because the refractive index of a display material is generally 1.5-1.6, display equipment can generate 4-5% reflection on ambient light, and the reflected light can affect the display quality and reduce the user experience. In order to improve the display quality, it is necessary to reduce the reflection of ambient light, and an antireflection film is directly attached to the surface of the display device, so that the reflection of the display device can be reduced at a lower cost, better image quality is provided, and better user experience is brought.
In addition, during the production and use of the antireflection optical film, static electricity is generated on the film due to environmental factors and the insulation of materials, and the adverse effect caused by charge accumulation is one of the most frequent and difficult harm to eliminate. Therefore, it is necessary to impart antistatic function to the antireflection optical film, and an antistatic film with low surface resistance not only has antistatic function but also can impart antifouling and dust-proof effects to the film. In order to impart antistatic properties to the antireflection film layer, it is generally necessary to interpose a hardening coating layer or an antistatic layer having antistatic properties between the transparent base film and the low refractive index layer. Meanwhile, since the anti-static antireflection film is attached to the surface of the display device and is in close contact with the external environment, in order to maintain good image display quality, the anti-static antireflection film needs to have not only good transmittance and anti-static performance, but also high hardness and adhesion, and thus it is necessary to design and manufacture an optical film having sufficient surface hardness, good adhesion, excellent antireflection effect, and excellent anti-static capability.
Disclosure of Invention
At present, a flexible anti-static anti-reflection film with excellent anti-reflection function and anti-static performance is not reported.
Therefore, the invention provides a flexible anti-static antireflection optical function film for a display device and a preparation method thereof. The functional film provided by the invention comprises two layers, and an antistatic layer is coated on a polyethylene terephthalate (PET) flexible substrate by adopting a roll-to-roll coating technology, and then a nano coating with a periodic pore structure is coated after thermocuring, so that an antireflection effect is realized.
The technical scheme of the invention is as follows:
as a first aspect of the present invention, there is provided an antistatic antireflection optical film including: the flexible substrate and adhere to the antistatic coating layer on at least one side surface of flexible substrate, still adhere to on the antistatic coating layer and subtract reflection coating layer.
According to the anti-static antireflection optical film, the anti-static coating layers are respectively attached to the surfaces of the two sides of the flexible substrate, and the antireflection coating layer is attached to the anti-static coating layer on at least one side.
According to any one of the above anti-static antireflection optical films, the anti-static coating layers on the surfaces of the two sides of the flexible substrate are respectively attached with the antireflection coating layers, that is, the anti-static coating layers and the antireflection coating layers are respectively sequentially attached on the surfaces of the two sides of the flexible substrate.
The anti-static antireflection optical film according to any one of the above, wherein the flexible substrate is a polyethylene terephthalate (PET) film.
According to any of the above anti-static antireflection optical films, the thickness of the anti-static coating layer is 100-2000nm, and more preferably 100-1500 nm.
According to any of the above anti-static antireflection optical films, the thickness of the antireflection coating layer is 80-400nm, and more preferably 100-160 nm.
As a second aspect of the present invention, there is provided a method for manufacturing an antistatic antireflection optical film, comprising: and coating the antistatic coating liquid on at least one side surface of the flexible substrate, pre-drying, coating the antireflection coating liquid, and pre-drying again and performing ultraviolet curing to obtain the antistatic antireflection optical film.
According to the preparation method of the anti-static antireflection optical film, the anti-static coating liquid or the antireflection coating liquid is coated in a roll-to-roll coating mode, and a gravure roll coating head or a slit coating head is recommended to be used for coating.
According to any one of the preparation methods of the anti-static antireflection optical film, the linear speed of the anti-static masking liquid coating is 15-35m/min, the pre-drying temperature is 50-80 ℃, and the drying time is 0.5-1 min.
According to the preparation method of the antistatic antireflection optical film, the linear speed of the antireflection coating liquid coating is 15-30m/min, the pre-drying temperature is 50-70 ℃, the pre-drying time is 0.5-1min, and the energy density of ultraviolet curing is 800 mJ/cm-2The power density is 40-80mW/cm2。
According to the preparation method of the anti-static antireflection optical film, the anti-static masking liquid comprises a nano oxide, a solvent and a film-forming assistant, and the anti-static masking liquid comprises the following components in percentage by mass: 2-10 parts of nano oxide, 90-98 parts of solvent and 0.01-0.025 part of film-forming assistant.
According to the preparation method of the antistatic antireflection optical film, the nano oxide is selected from antimony-doped tin dioxide (ATO), aluminum-doped zinc oxide (AZO) and titanium oxide (TiO)2) At least one of; more preferably aluminum-doped zinc oxide (AZO); most preferably, the nano-oxide is an inorganic nano-particle selected from one of antimony-doped tin dioxide nano-powder, aluminum-doped zinc oxide nano-powder and titanium oxide nano-powder.
According to the above method for manufacturing an antistatic antireflection optical film, the solvent is at least one selected from water and ethanol.
According to the preparation method of the antistatic antireflection optical film, the film-forming assistant is at least one selected from polyvinyl alcohol, polyvinylpyrrolidone, modified comb acrylic ester copolymer surface assistant, hydroxyl polyether type organic silicon slipping agent, macromolecular polyether modified acrylic ester surface assistant, polyether modified dimethyl polysiloxane organic silicon surface assistant, polyacrylate type leveling assistant and epoxy phenyl vinyl silane oligomer.
According to the preparation method of the antistatic antireflection optical film, the antireflection coating liquid comprises resin, hollow organic silicon nano particles, a solvent, a wetting and leveling agent and a photoinitiator, and the mass ratio of each component is as follows: 0.5 to 1.5 percent of resin, 1.0 to 3.5 percent of hollow organic silicon particles, 92 to 98 percent of solvent, 0.05 to 0.15 percent of wetting and leveling agent and 0.05 to 0.15 percent of photoinitiator.
According to the preparation method of the antistatic antireflection optical film, the resin comprises urethane acrylate or epoxy acrylate.
According to the above method for producing an antistatic antireflection optical film, the resin is at least one selected from the group consisting of aliphatic urethane acrylate, epoxy acrylate, aromatic urethane acrylate, tris (2-hydroxyethyl) isocyanurate triacrylate, (2) ethoxylated bisphenol a dimethacrylate, urethane acrylate, high-functionality urethane acrylate, and 1, 4-butanediol dimethacrylate.
According to the above method for preparing the antistatic antireflection optical film, the resin may be a high-functionality resin, a medium-functionality resin or a low-functionality resin, and the specific functionality and the type of the resin may be set as required; wherein, the high-functionality resin is a resin with the functionality of more than or equal to 8, the medium-functionality resin is a resin with the functionality of 4-7, and the low-functionality resin is a resin with the functionality of 1-3.
According to the preparation method of the antistatic antireflection optical film, the particle size of the hollow organosilicon nanoparticles is 20-120nm, and the wall thickness is 5-10 nm; more preferably, the particle size is 40 to 80nm and the wall thickness is 5 to 8 nm.
According to the above method for manufacturing an antistatic antireflection optical film, the solvent is at least two selected from ethyl acetate, butyl acetate, methyl isobutyl ketone, isophorone, propylene glycol monomethyl ether, propylene glycol methyl ether acetate, isopropanol and isobutanol.
According to the preparation method of the antistatic antireflection optical film, the wetting and leveling agent is at least one selected from a hydroxy polyether type organic silicon slipping agent, a macromolecular polyether modified acrylate surface auxiliary agent, a polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent, a polyacrylate type leveling auxiliary agent, an epoxy phenyl vinyl silane oligomer, a short-chain perfluorinated fluorine-containing surfactant and a solvent type fluorinated polymer.
According to the above method for manufacturing an antistatic antireflection optical film, the photoinitiator is at least one selected from the group consisting of 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- (4-methylthiophenyl) -2-morpholin-1-one, bifunctional α -hydroxy ketone, 2-hydroxy-methylphenyl propane-1-one, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide.
According to a third aspect of the present invention, there is provided a method for preparing an antistatic masking liquid, comprising the steps of:
(1) preparing a dispersion liquid A: dispersing inorganic nano particles into a solvent, and stirring and uniformly mixing at room temperature;
(2) preparing an antistatic masking liquid: and mixing the dispersion liquid A, the solvent and the film-forming assistant, and uniformly stirring to obtain the antistatic masking liquid.
The invention provides an antistatic masking liquid as a fourth aspect, which comprises a nano oxide, a solvent and a film-forming assistant, wherein the mass ratio of each component is as follows: 2-10 parts of nano oxide, 90-98 parts of solvent and 0.01-0.025 part of film-forming assistant.
According to the antistatic coating liquid, the nano oxide is selected from antimony-doped tin dioxide (ATO), aluminum-doped zinc oxide (AZO) and titanium oxide (TiO)2) At least one of; more preferably aluminum-doped zinc oxide (AZO); most preferably, the nano-oxide is an inorganic nano-particle selected from one of antimony-doped tin dioxide nano-powder, aluminum-doped zinc oxide nano-powder and titanium oxide nano-powder.
The antistatic masking liquid as described in any one of the above claims, wherein said solvent is at least one selected from the group consisting of water and ethanol.
According to any one of the antistatic masking liquids, the film-forming assistant is at least one selected from polyvinyl alcohol, polyvinylpyrrolidone, modified comb acrylic ester copolymer surface assistant, hydroxy polyether type organosilicon slipping agent, macromolecular polyether modified acrylic ester surface assistant, polyether modified dimethyl polysiloxane organosilicon surface assistant, polyacrylate type leveling assistant and epoxy phenyl vinyl silane oligomer.
The antistatic masking liquid according to any one of the above, which is obtained by the above preparation method.
As a fifth aspect of the present invention, there is provided a method for producing an antireflection coating liquid, comprising the steps of:
(1) preparing a solvent A: mixing at least two solvents uniformly, stirring and mixing uniformly for 30min at room temperature.
(2) Preparation of resin dispersion B: mixing at least two resins, adding solvent A, stirring at room temperature for 30min, and mixing well.
(3) Preparing an antireflection coating solution: stirring the resin dispersion liquid B, the solvent A and the hollow organic silicon nano particles at room temperature for 60min, uniformly mixing, adding the wetting and leveling agent, and continuously stirring for 30 min; and finally, adding a photoinitiator, stirring for 30min, and filtering to obtain the antireflection coating liquid.
As a fifth aspect of the present invention, an antireflection coating solution is provided, which includes resin, hollow organosilicon nanoparticles, a solvent, a wetting and leveling agent, and a photoinitiator, and the antireflection coating solution includes the following components in parts by mass: 0.5 to 1.5 percent of resin, 1.0 to 3.5 percent of hollow organic silicon particles, 92 to 98 percent of solvent, 0.05 to 0.15 percent of wetting and leveling agent and 0.05 to 0.15 percent of photoinitiator.
According to the antireflection coating liquid described above, the resin includes urethane acrylate or epoxy acrylate.
The antireflection coating liquid according to any one of the above, wherein the resin is at least one selected from the group consisting of aliphatic urethane acrylate, epoxy acrylate, aromatic urethane acrylate, tris (2-hydroxyethyl) isocyanurate triacrylate, (2) ethoxylated bisphenol a dimethacrylate, urethane acrylate, high-functionality urethane acrylate, and 1, 4-butanediol dimethacrylate.
According to the antireflection coating liquid, the resin can be a high-functionality resin, a medium-functionality resin or a low-functionality resin, and the specific functionality and the type of the resin can be set as required; wherein, the high-functionality resin is a resin with the functionality of more than or equal to 8, the medium-functionality resin is a resin with the functionality of 4-7, and the low-functionality resin is a resin with the functionality of 1-3.
Most preferably, the resin is selected from one or more combinations of aliphatic urethane acrylate (functionality 7), aliphatic urethane acrylate (functionality 9), epoxy acrylate (functionality 2), aromatic urethane acrylate (functionality 10), tris (2-hydroxyethyl) isocyanurate triacrylate (functionality 3), (2) ethoxylated bisphenol a dimethacrylate (functionality 2), urethane acrylate (functionality 9), high functionality urethane acrylate (functionality 15), 1,4 butanediol dimethacrylate (functionality 2).
According to any one of the antireflection coating solutions, the particle size of the hollow organosilicon nanoparticles is 20-120nm, and the wall thickness is 5-10 nm; more preferably, the particle size is 40 to 80nm and the wall thickness is 5 to 8 nm.
The antireflection coating solution according to any one of the above, wherein the solvent is at least two selected from the group consisting of ethyl acetate, butyl acetate, methyl isobutyl ketone, isophorone, propylene glycol monomethyl ether, propylene glycol methyl ether acetate, isopropyl alcohol, and isobutyl alcohol;
according to any one of the antireflection coating solutions, the wetting and leveling agent is at least one selected from a hydroxy polyether type organic silicon slipping agent, a macromolecular polyether modified acrylate surface auxiliary agent, a polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent, a polyacrylate type leveling auxiliary agent, an epoxy phenyl vinyl silane oligomer, a short-chain perfluorinated fluorine-containing surfactant and a solvent type fluorinated polymer.
The anti-reflective coating according to any one of the preceding claims, said photoinitiator being selected from at least one of 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- (4-methylthiophenyl) -2-morpholin-1-one, difunctional alpha-hydroxy ketone, 2-hydroxy-methylphenyl propane-1-one, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide.
The antireflection coating solution according to any one of the above methods, wherein the antireflection coating solution is obtained by the above preparation method.
According to a sixth aspect of the invention, the invention provides an application of the antistatic antireflection optical film in protection of a display device.
The invention also provides application of the antistatic masking liquid or the antireflection masking liquid, namely, the masking liquid is applied to a substrate.
Therefore, the anti-static antireflection optical coating is provided, a transparent flexible substrate is used as a base material of the coating, an anti-static coating liquid is coated on the substrate in a roll-to-roll coating mode, the anti-static coating liquid is coated on the anti-static layer after thermocuring, a layer of antireflection film is prepared on the reverse side of the substrate by the same process after pre-drying and ultraviolet curing, and the anti-static antireflection flexible optical functional film is obtained.
The transparent film substrate used in the present invention is not particularly limited, and the transparent substrate is preferably a material excellent in light transmittance of visible light (light transmittance of more than 90%) and transparency (haze value of less than 1%), such as a polyethylene terephthalate (PET) film, a Polycarbonate (PC) film, a Triacetate (TAC) film, a polymethyl methacrylate (PMMA) film, or the like. Polyethylene terephthalate (PET) film is preferred. The thickness of the transparent substrate is not particularly limited and may be appropriately selected depending on the case, and is usually in the range of 10 to 500. mu.m, preferably 50 to 250. mu.m.
Compared with the existing antireflection film, the antistatic coating liquid and the antistatic antireflection optical coating coated by the antireflection coating liquid can reduce the reflectivity of a base material from 4.8% to 0.28%, improve the transmissivity from 90.8% to 99.58%, and increase the resistivity to 109Omega cm. In a word, the invention solves the balance problem of the anti-static performance and the anti-reflection function of the flexible anti-static anti-reflection film, is a comprehensive promotion technology and has originality.
Drawings
FIG. 1: examples 1-5 schematic diagrams of antistatic antireflective coatings for optical film samples;
FIG. 2: examples 6-10 schematic diagrams of antistatic antireflective coatings for optical film samples;
FIG. 3: transmittance profiles of flexible antistatic antireflective optical functional films for display devices of the present invention (examples 1-5 optical film samples);
FIG. 4: transmittance profiles of flexible antistatic antireflective optical functional films for display devices of the present invention (examples 6-10 optical film samples);
FIG. 5: reflectance profiles of flexible antistatic antireflective optical functional films for display devices of the present invention (examples 1-5 optical film samples);
FIG. 6: reflectance profiles of flexible antistatic antireflective optical functional films for display devices of the present invention (examples 6-10 optical film samples).
Detailed Description
In order that those skilled in the art will better understand the invention and thus more clearly define the scope of the invention as claimed, it is described in detail below with respect to certain specific embodiments thereof. It should be noted that the following are only some specific embodiments of the inventive concept, and are only a part of the examples of the present invention, wherein the specific direct description of the related structures is only for the convenience of understanding the present invention, and the specific features do not, of course, directly limit the scope of the implementation of the present invention. Such alterations and modifications as are made obvious by those skilled in the art and guided by the teachings herein are intended to be within the scope of the invention as claimed.
Example one
1. Preparing antireflection coating liquid AR-1
1.1 materials
Aliphatic urethane acrylate (molecular weight 1000, functionality 7), aliphatic urethane acrylate (molecular weight 2000, functionality 9), epoxy acrylate (molecular weight 2000, functionality 2), hollow silicone nanoparticles (d50 ═ 60nm, wall thickness 5nm), ethyl acetate, butyl acetate, isophorone, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- (4-methylthiophenyl) -2-morpholin-1-one.
1.2 methods
(1) Preparing a solvent A: and uniformly mixing ethyl acetate, butyl acetate and isophorone according to the mass ratio of 2:2:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: mixing 0.3g of aliphatic urethane acrylate (molecular weight 1000, functionality 7), aliphatic urethane acrylate (molecular weight 2000, functionality 9) and epoxy acrylate (molecular weight 2000, functionality 2) according to the mass ratio of 6:3:1, adding 2g of solvent A, stirring for 30min at room temperature, and uniformly mixing.
(3) Preparing an antireflection coating solution: stirring 2.3g of resin dispersion liquid B, 18g of solvent A and 0.4g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.01g of assistant hydroxy polyether type organic silicon slip agent and 0.01g of macromolecule polyether modified acrylate surface assistant, continuously stirring for 30min, finally adding 0.02g of photoinitiator 1-hydroxy cyclohexyl phenyl ketone and 0.02g of 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-acetone, stirring for 30min, and filtering to obtain the antireflection coating AR-1.
2. Preparing antistatic masking liquid AS-1
2.1 materials
Modified AZO inorganic nano-particles, water, ethanol, polyvinyl alcohol and a modified cosmetic acrylate copolymer surface auxiliary agent.
2.2 methods
(1) Preparing a solution A: and dispersing the modified AZO inorganic nano-particles 3:50 into water, and stirring for 30min at room temperature to obtain 10g of solution A.
(2) And sequentially adding the solution A, water, ethanol, polyvinyl alcohol and the modified cosmetic acrylate copolymer surface auxiliary agent according to the proportion of 1:1:0.5:0.005:0.005, and stirring for 2 hours to obtain the antistatic masking liquid AS-1.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-1 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an anti-reflection layer: coating AR-1 on the antistatic layer on one side by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The coated product was an antistatic antireflection optical film, which was named the optical film sample of example 1.
Example two
1. Preparing antireflection coating liquid AR-2
1.1 materials
Aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), epoxy acrylate (molecular weight 2000, functionality 2), hollow silicone nanoparticles (d50 ═ 70nm, wall thickness 8nm), ethyl acetate, methyl isobutyl ketone, propylene glycol monomethyl ether acetate, bifunctional α -hydroxyketone, 2-hydroxy-methylphenylpropane-1-one, polyether-modified dimethylpolysiloxane silicone surface auxiliaries, polyacrylate-type leveling auxiliaries.
1.2 methods
(1) Preparing a solvent A: and uniformly mixing ethyl acetate, methyl isobutyl ketone and propylene glycol methyl ether acetate according to the mass ratio of 2:3:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: mixing aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9) and epoxy acrylate (molecular weight 2000, functionality 2) according to the mass ratio of 5:3:2, adding 0.3g of solvent A in total, stirring at room temperature for 30min, and mixing uniformly.
(3) Preparing an antireflection coating solution: stirring 2.3g of resin dispersion liquid B, 18g of solvent A and 0.2g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.01g of assistant polyether modified dimethyl polysiloxane organic silicon surface assistant and 0.01g of polyacrylate type leveling assistant, continuously stirring for 30min, finally adding 0.02g of photoinitiator bifunctional alpha-hydroxyketone and 0.02g of 2-hydroxy-methyl phenyl propane-1-ketone, stirring for 30min, and filtering to obtain the antireflection coating liquid AR-2.
2. Preparing antistatic masking liquid AS-2
2.1 materials
Modified AZO inorganic nano-particles, water, ethanol, polyvinylpyrrolidone, modified cosmetic acrylate copolymer surface auxiliary agent and hydroxyl polyether type organic silicon slip agent.
2.2 methods
(1) Preparing a solution A: and dispersing the modified AZO inorganic nano-particles 2:25 into water, and stirring for 30min at room temperature to obtain 10g of solution A.
(2) Adding the solution A, water, ethanol, polyvinylpyrrolidone, the modified comb acrylic ester copolymer surface auxiliary agent and the hydroxyl polyether type organic silicon slip agent in sequence according to the proportion of 1:1:0.5:0.005:0.005:0.005, and stirring for 2 hours to obtain the antistatic masking liquid AS-2.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-2 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: coating AR-2 on the antistatic layer on one side by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The product after coating is the antistatic antireflection optical film which is named as the optical film sample in the embodiment 2.
EXAMPLE III
1. Preparing antireflection coating liquid AR-3
1.1 materials
High functionality urethane acrylate (functionality 15), urethane acrylate (functionality 9), 1, 4-butanediol dimethacrylate (functionality 2), (2) ethoxylated bisphenol a dimethacrylate (functionality 2), hollow silicone nanoparticles (d50 ═ 50nm, wall thickness 5nm), ethyl acetate, methyl isobutyl ketone, propylene glycol monomethyl ether, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide, polyether-modified dimethylpolysiloxane silicone surface auxiliaries, polyacrylate-type levelling auxiliaries.
1.2 methods
(1) Preparing a solvent A: and uniformly mixing ethyl acetate, methyl isobutyl ketone and propylene glycol monomethyl ether according to the mass ratio of 1:2:2, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: high functionality urethane acrylate (functionality 15), urethane acrylate (functionality 9), 1, 4-butanediol dimethacrylate (functionality 2), and (2) ethoxylated bisphenol A dimethacrylate (functionality 2) were mixed in a mass ratio of 4:4:0.5:0.5, and 0.3g in total, 2g of solvent A was added, and stirred at room temperature for 30min and mixed uniformly.
(3) Preparing an antireflection coating solution: stirring 2.3g of resin dispersion liquid B, 18g of solvent A and 0.5g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, then adding 0.02g of polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent and 0.01g of polyacrylate type leveling auxiliary agent, continuously stirring for 30min, finally adding 0.02g of photoinitiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide and 0.02g of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, stirring for 30min, and filtering to obtain the antireflection coating liquid AR-3.
2. Preparing antistatic masking liquid AS-3
2.1 materials: modified AZO inorganic nano-particles, water, isopropanol, polyvinyl alcohol and a hydroxyl polyether type organic silicon slip agent.
2.2 method:
(1) preparing a solution A: and dispersing the modified AZO inorganic nano-particles 1:10 into water, and stirring for 30min at room temperature to obtain 10g of solution A.
(2) Adding the solution A, water, isopropanol, polyvinyl alcohol and hydroxyl polyether type organic silicon slip agent in sequence according to the proportion of 1:1:0.5:0.005:0.005, and stirring for 2 hours to obtain the antistatic masking liquid AS-3.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-3 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: coating AR-3 on the antistatic layer on one side by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The product after coating is the antistatic antireflection optical film which is named as the optical film sample in the embodiment 3.
Example four
1. Preparing antireflection coating liquid AR-4
1.1 materials:
aromatic urethane acrylate (molecular weight 1200, functionality 10), urethane acrylate (functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), (2) ethoxylated bisphenol a dimethacrylate (functionality 2), hollow silicone nanoparticles (d50 ═ 50nm, wall thickness 5nm), isopropanol, butyl acetate, isophorone, 2-methyl-1- (4-methylthiophenyl) -2-morpholin-1-propanone, difunctional alpha-hydroxy ketones, polyacrylate-type leveling aids, epoxyphenylvinylsilane oligomers, short chain perfluorinated fluorinated surfactants.
1.2 method:
(1) preparing a solvent A: uniformly mixing isopropanol, butyl acetate and isophorone according to the mass ratio of 1:2:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: aromatic urethane acrylate (molecular weight 1200, functionality 10), urethane acrylate (functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), and (2) ethoxylated bisphenol a dimethacrylate (functionality 2) were mixed in a mass ratio of 5:2:2.5:0.5, 0.2g in total, and 2g of solvent a was added, stirred at room temperature for 30min, and mixed uniformly.
(3) Preparing an antireflection coating solution: stirring 2.2g of resin dispersion liquid B, 18g of solvent A and 0.2g of hollow organosilicon nano particles for 60min at room temperature, uniformly mixing, adding 0.02g of assistant polyacrylate type leveling assistant, 0.01g of epoxy phenyl vinyl silane oligomer and 0.01g of short-chain perfluorinated fluorine-containing surfactant, continuously stirring for 30min, finally adding 0.02g of photoinitiator 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-acetone and 0.02g of bifunctional alpha-hydroxyketone, stirring for 30min, and filtering to obtain the antireflection coating liquid AR-4.
2. Preparing antistatic masking liquid AS-4
2.1 materials
Modified AZO inorganic nano particles, water, isopropanol, polyacrylate type leveling auxiliary agent and epoxy phenyl vinyl silane oligomer.
2.2 methods
(1) Preparing a solution A: and dispersing the modified AZO inorganic nano particles 1:20 into water, and stirring at room temperature for 30min to obtain 20g of solution A.
(2) And sequentially adding the solution A, water, isopropanol, a polyacrylate type leveling auxiliary agent and an epoxy phenyl vinyl silane oligomer according to the proportion of 1:0.5:0.5:0.005:0.015, and stirring for 2 hours to obtain the antistatic masking liquid AS-4.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-4 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: coating AR-4 on the antistatic layer on one side by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The product after coating is the antistatic antireflection optical film which is named as the optical film sample in the embodiment 4.
EXAMPLE five
1. Preparing antireflection coating liquid AR-5
1.1 materials
Aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), epoxy acrylate (molecular weight 2000, functionality 2), hollow silicone nanoparticles (d50 ═ 40nm, wall thickness 5nm), isopropanol, methyl isobutyl ketone, propylene glycol methyl ether acetate, 1-hydroxycyclohexyl phenyl ketone, bifunctional α -hydroxy ketone, polyether-modified dimethylpolysiloxane silicone surface adjuvant, polyacrylate-type leveling adjuvant.
1.2 methods
(1) Preparing a solvent A: uniformly mixing isopropanol, methyl isobutyl ketone and propylene glycol methyl ether acetate according to the mass ratio of 1:3:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: mixing aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), epoxy acrylate (molecular weight 2000, functionality 2) in a mass ratio of 5:3: 1.5: 0.5g of the above components were mixed, and a total of 0.3g of the above components was added to 2g of solvent A, followed by stirring at room temperature for 30min and then uniformly mixing.
(3) Preparing an antireflection coating solution: stirring 2.3g of resin dispersion liquid B, 18g of solvent A and 0.3g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.02g of auxiliary agent polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent and 0.05g of polyacrylate type leveling auxiliary agent, continuously stirring for 30min, finally adding 0.02g of photoinitiator 1-hydroxycyclohexyl phenyl ketone and 0.02g of bifunctional group alpha-hydroxyketone, stirring for 30min, and filtering to obtain the antireflection coating AR-5.
2. Preparing antistatic masking liquid AS-5
2.1 materials
Modified AZO inorganic nano-particles, water, ethanol, polyvinyl alcohol and hydroxy polyether type organic silicon slipping agent.
2.2 methods
(1) Preparing a solution A: modified AZO inorganic nanoparticles 3:50 was dispersed in water and stirred at room temperature for 30min to obtain 10g of solution A.
(2) Adding the solution A, water, ethanol, polyvinyl alcohol and hydroxyl polyether type organic silicon slip agent in sequence according to the proportion of 1:1:0.5:0.015:0.015, and stirring for 2 hours to obtain the antistatic masking liquid AS-5.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-5 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: coating AR-5 on the antistatic layer on one side by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The product after coating is the antistatic antireflection optical film which is named as the optical film sample in the embodiment 5.
EXAMPLE six
1. Preparing AR-6 antireflection coating liquid
1.1 materials
Aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), high functionality urethane acrylate (functionality 15), 1, 4-butanediol dimethacrylate (functionality 2), hollow silicone nanoparticles (d50 ═ 70nm, wall thickness 5nm), isopropanol, propylene glycol methyl ether, propylene glycol butyl ether, 1-hydroxycyclohexyl phenyl ketone, bifunctional α -hydroxyketone, polyether-modified dimethylpolysiloxane silicone surface adjuvant, polyacrylate-type leveling adjuvant.
1.2 methods
(1) Preparing a solvent A: uniformly mixing isopropanol, propylene glycol methyl ether and propylene glycol butyl ether according to the mass ratio of 1:2:2, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: mixing aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), high functionality urethane acrylate (functionality 15), and 1, 4-butanediol dimethacrylate (functionality 2) according to the mass ratio of 5:3:1:1, and adding 2g of solvent A, stirring at room temperature for 30min, and mixing uniformly.
(3) Preparing an antireflection coating solution: stirring 2.1g of resin dispersion liquid B, 18g of solvent A and 0.5g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.05g of assistant polyether modified dimethyl polysiloxane organic silicon surface assistant and 0.02g of polyacrylate type leveling assistant, continuously stirring for 30min, finally adding 0.02g of photoinitiator 1-hydroxycyclohexyl phenyl ketone and 0.02g of bifunctional group alpha-hydroxyketone, stirring for 30min, and filtering to obtain the antireflection coating AR-6.
2. Preparing antistatic masking liquid AS-6
2.1 materials
Modified AZO inorganic nano-particles, water, ethanol, polyvinyl alcohol and hydroxy polyether type organic silicon slipping agent.
2.2 methods
(1) Preparing a solution A: and (3) dispersing the modified AZO inorganic nano-particles 3:20 into water, and stirring at room temperature for 30min to obtain 10g of solution A.
(2) And adding the solution A, water, ethanol, polyvinyl alcohol and epoxy phenyl vinyl silane oligomer in sequence according to the proportion of 1:2:2:0.015:0.01, and stirring for 2 hours to obtain the antistatic coating liquid AS-6.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-6 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: respectively coating AR-6 on the antistatic layers on the two side surfaces by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and then enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The product after coating is the antistatic antireflection optical film which is named as the optical film sample in the embodiment 6.
EXAMPLE seven
1. Preparing antireflection coating liquid AR-7
1.1 materials
Aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), high functionality urethane acrylate (functionality 15), 1, 4-butanediol dimethacrylate (functionality 2), hollow silicone nanoparticles (d50 ═ 50nm, wall thickness 5nm), isopropanol, ethyl acetate, butyl acetate, 1-hydroxycyclohexyl phenyl ketone, bifunctional α -hydroxyketone, polyether-modified dimethylpolysiloxane silicone surface auxiliaries, polyacrylate-type leveling auxiliaries.
1.2 methods
(1) Preparing a solvent A: uniformly mixing isopropanol, ethyl acetate and butyl acetate according to the mass ratio of 1:3:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: mixing 0.2g of aromatic urethane acrylate (molecular weight 1200, functionality 10), aliphatic urethane acrylate (molecular weight 2000, functionality 9), high-functionality urethane acrylate (functionality 15) and 1, 4-butanediol dimethacrylate (functionality 2) according to the mass ratio of 5:4:0.5:0.5, adding 2g of solvent A, stirring at room temperature for 30min, and uniformly mixing.
(3) Preparing an antireflection coating solution: stirring 2.2g of resin dispersion liquid B, 18g of solvent A and 0.5g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.02g of auxiliary agent polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent and 0.05g of polyacrylate type leveling auxiliary agent, continuously stirring for 30min, finally adding 0.02g of photoinitiator 1-hydroxycyclohexyl phenyl ketone and 0.02g of bifunctional group alpha-hydroxyketone, stirring for 30min, and filtering to obtain the antireflection coating AR-7.
2. Preparing antistatic masking liquid AS-7
2.1 materials
Modified AZO inorganic nanoparticles, water, ethanol, polyvinyl alcohol and polyvinylpyrrolidone.
2.2 methods
(1) Preparing a solution A: and dispersing the modified AZO inorganic nano-particles 1:10 into water, and stirring for 30min at room temperature to obtain 10g of solution A.
(2) And adding the solution A, water, ethanol, polyvinyl alcohol and polyvinylpyrrolidone in sequence according to the proportion of 1:1:0.5:0.015:0.01, and stirring for 2 hours to obtain the antistatic masking liquid AS-7.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-7 is coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: respectively coating AR-7 on the antistatic layers on the two side surfaces by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The coated product was an antistatic antireflection optical film, which was named the optical film sample of example 7.
Example eight
1. Preparing antireflection coating liquid AR-8
1.1 materials
Aliphatic urethane acrylate (molecular weight 1000, functionality 7), aliphatic urethane acrylate (molecular weight 2000, functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), epoxy acrylate (molecular weight 2000, functionality 2), hollow silicone nanoparticles (d50 ═ 60nm, wall thickness 5nm), isopropanol, methyl isobutyl ketone, isophorone, 1-hydroxycyclohexyl phenyl ketone, bifunctional α -hydroxy ketones, polyacrylate-type leveling aids, epoxy phenyl vinyl silane oligomers.
1.2 methods
(1) Preparing a solvent A: uniformly mixing isopropanol, methyl isobutyl ketone and isophorone according to the mass ratio of 1:3:1, and stirring at room temperature for 30min to obtain 20g of solvent A.
(2) Preparation of resin dispersion B: an aliphatic urethane acrylate (molecular weight 1000, functionality 7), an aliphatic urethane acrylate (molecular weight 2000, functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), and an epoxy acrylate (molecular weight 2000, functionality 2) were mixed in a mass ratio of 4:4:1:1, 0.1g in total, 2g of solvent A was added, and the mixture was stirred at room temperature for 30min and mixed uniformly.
(3) Preparing an antireflection coating solution: stirring 2.1g of resin dispersion liquid B, 18g of solvent A and 0.7g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.05g of assistant polyacrylate type leveling assistant and 0.05g of epoxy phenyl vinyl silane oligomer, continuously stirring for 30min, finally adding 0.02g of photoinitiator 1-hydroxycyclohexyl phenyl ketone and 0.02g of bifunctional group alpha-hydroxy ketone, stirring for 30min, and filtering to obtain the antireflection coating liquid AR-8.
2. Preparing antistatic masking liquid AS-8
2.1 materials
Modified AZO inorganic nano-particles, water, ethanol, modified cosmetic acrylate copolymer surface auxiliary agent and hydroxyl polyether type organic silicon slipping agent.
2.2 methods
(1) Preparing a solution A: the modified AZO inorganic nano-particles 1:25 are dispersed in water and stirred for 30min at room temperature to obtain 10g of solution A.
(2) Adding the solution A, water, ethanol, the modified toilet acrylic ester copolymer surface auxiliary agent and the hydroxyl polyether type organic silicon slip agent in sequence according to the proportion of 1:0.5:0.5:0.015:0.01, and stirring for 2 hours to obtain the antistatic masking liquid AS-8.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-8 is respectively coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: respectively coating AR-8 on the antistatic layers on the two side surfaces by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and then enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The product after coating is the antistatic antireflection optical film which is named as the optical film sample of the embodiment 8.
Example nine
1. Preparing antireflection coating liquid AR-9
1.1 materials
Aromatic urethane acrylate (molecular weight 1200, functionality 10), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), epoxy acrylate (molecular weight 2000, functionality 2), hollow silicone nanoparticles (d50 ═ 70nm, wall thickness 5nm), isopropanol, methyl isobutyl ketone, propylene glycol methyl ether acetate, 2-hydroxy-methylphenylpropane-1-one, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, polyether-modified dimethylpolysiloxane silicone surface auxiliaries, polyacrylate-type levelling auxiliaries.
1.2 methods
(1) Preparing a solvent A: uniformly mixing isopropanol, methyl isobutyl ketone and propylene glycol methyl ether acetate according to the mass ratio of 2:2:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: mixing aromatic urethane acrylate (molecular weight 1200, functionality 10), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), and epoxy acrylate (molecular weight 2000, functionality 2) in a mass ratio of 2:2:1, totaling 0.1g, adding 2g of solvent A, stirring at room temperature for 30min, and mixing uniformly.
(3) Preparing an antireflection coating solution: stirring 2.1g of resin dispersion liquid B, 18g of solvent A and 0.6g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.05g of assistant polyether modified dimethyl polysiloxane organic silicon surface assistant and 0.05g of polyacrylate type leveling assistant, continuously stirring for 30min, finally adding 0.02g of photoinitiator 2-hydroxy-methyl phenyl propane-1-ketone and 0.02g of 2,4, 6-trimethyl benzoyl-diphenyl phosphine oxide, stirring for 30min, and filtering to obtain the antireflection coating AR-9.
2. Preparing antistatic masking liquid AS-9
2.1 materials
Modified AZO inorganic nano-particles, water, ethanol, a hydroxyl polyether type organic silicon slipping agent and a macromolecular polyether modified acrylate surface auxiliary agent.
2.2 methods
(1) Preparing a solution A: and dispersing the modified AZO inorganic nano-particles 1:10 into water, and stirring for 30min at room temperature to obtain 10g of solution A.
(2) Adding the solution A, water, ethanol, a hydroxyl polyether type organic silicon slipping agent and a macromolecular polyether modified acrylate surface auxiliary agent in sequence according to the proportion of 1:1:1:0.015:0.015, and stirring for 2 hours to obtain the antistatic masking liquid AS-9.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-9 is respectively coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: respectively coating AR-9 on the antistatic layers on the surfaces of the two side surfaces by a gravure roller coating head, wherein the linear speed of the film running is 15m/min, the film passes through the roller coating head and then enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp in an ultraviolet mode, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The coated product was an antistatic antireflection optical film, which was named the optical film sample of example 9.
Example ten
1. Preparing antireflection coating liquid AR-10
1.1 materials
Aliphatic urethane acrylate (molecular weight 2000, functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), epoxy acrylate (molecular weight 2000, functionality 2), hollow silicone nanoparticles (d50 ═ 60nm, wall thickness 5nm), isopropanol, methyl isobutyl ketone, isophorone, propylene glycol methyl ether, 1-hydroxycyclohexyl phenyl ketone, difunctional alpha-hydroxy ketones, polyacrylate-type leveling aids, epoxyphenyl vinyl silane oligomers.
1.2 methods
(1) Preparing a solvent A: uniformly mixing isopropanol, methyl isobutyl ketone, isophorone and propylene glycol methyl ether according to the mass ratio of 1:3:1:1, and stirring at room temperature for 30min to obtain 20g of a solvent A.
(2) Preparation of resin dispersion B: an aliphatic urethane acrylate (molecular weight 2000, functionality 9), tris (2-hydroxyethyl) isocyanurate triacrylate (molecular weight 1200, functionality 3), and an epoxy acrylate (molecular weight 2000, functionality 2) were mixed in a mass ratio of 5:3:2, and 0.2g in total, and 2g of solvent a was added, stirred at room temperature for 30min, and mixed uniformly.
(3) Preparing an antireflection coating solution: stirring 2.2g of resin dispersion liquid B, 18g of solvent A and 0.7g of hollow organic silicon nano particles for 60min at room temperature, uniformly mixing, adding 0.05g of assistant polyacrylate type leveling assistant and 0.05g of epoxy phenyl vinyl silane oligomer, continuously stirring for 30min, finally adding 0.02g of photoinitiator 1-hydroxycyclohexyl phenyl ketone and 0.02g of bifunctional group alpha-hydroxy ketone, stirring for 30min, and filtering to obtain the antireflection coating AR-10.
2. Preparing antistatic masking liquid AS-10
2.1 materials
Modified AZO inorganic nano particles, water, ethanol, polyvinylpyrrolidone and modified cosmetic acrylate copolymer surface auxiliary agent.
2.2 methods
(1) Preparing a solution A: and dispersing the modified AZO inorganic nano particles 1:5 into water, and stirring for 30min at room temperature to obtain 10g of solution A.
(2) And sequentially adding the solution A, water, ethanol, polyvinylpyrrolidone and the modified cosmetic acrylate copolymer surface auxiliary agent according to the proportion of 1:1:1:0.015:0.015, and stirring for 2 hours to obtain the antistatic masking liquid AS-10.
3. Coating antistatic antireflection optical film
(1) Coating an antistatic layer: AS-10 is respectively coated on the two side surfaces of PET by a gravure roller coating head, the linear speed of the film is 25m/min, and the film passes through the coating head and then enters an oven for drying at the temperature of 65 ℃.
(2) Coating an antireflection layer: respectively coating AR-10 on the antistatic layers on the two side surfaces by a gravure roller coating head, wherein the linear speed of the film is 15m/min, the film passes through the coating head and enters an oven with the temperature of 55 ℃ for pre-drying, and then the film is cured by a mercury lamp through ultraviolet, wherein the curing energy density is 625mJ/cm2The power density is 74mW/cm2。
The coated product was an antistatic antireflective optical film, which was named example 10 optical film sample.
The optical films obtained in examples 1 to 5 and 6 to 10 were tested, and the test results of the respective samples are shown in tables 1 and 2.
Table 1 examples 1-5 optical film sample test data table
Table 2 examples 6-10 optical film sample test data table
The method for testing the parameters comprises the following steps:
1. optical Performance testing
A detection instrument: ultraviolet-visible spectrometer model U-4100 Hitachi
The detection method comprises the following steps: experiments were conducted with anti-static anti-reflective optical coatings coated on polyethylene terephthalate (PET) film substrates (coatings prepared in examples 1-10) in the range of 300-1000 nm.
By coating the surface of the PET substrate with a film (the coatings prepared in examples 1-5), we obtained that the maximum transmittance of the PET substrate increased from 91.76% to 95.67% after coating, the minimum reflectance decreased from 4.58% to 0.28% after coating, the transmittance test results are shown in FIG. 3, and the reflectance results are shown in FIG. 5. By coating the surface of the PET substrate with a film (the coatings prepared in examples 6-10), we obtained that the maximum transmittance of the PET substrate increased from 91.76% to 99.58% after coating, the minimum reflectance decreased from 4.58% to 0.5% after coating, the transmittance test results are shown in FIG. 4, and the reflectance results are shown in FIG. 6.
2. Antistatic Property test
A detection instrument: surface resistance meter model ST-4, SIMCO
The detection method comprises the following steps: the antistatic antireflective optical coating was coated on a PET substrate (the coatings prepared in examples 1-10) for testing, and the surface resistance was measured using a surface resistance meter.
By coating a film on the surface of a PET substrate, the surface resistance of the PET substrate can be increased from 1013Omega cm is reduced to 109-10Ω · cm, see tables 1 and 2.
3. Haze Property test
A detection instrument: haze tester model WGW photoelectric haze tester, instrument electron light
The detection method comprises the following steps: an experiment was performed in which an antistatic antireflective optical coating was coated on a PET film substrate (the coatings prepared in examples 1-10), and the haze of the sample was measured using a haze tester.
By coating the film on the surface of the PET substrate, the haze can be controlled below 1 percent, and the haze can be controlled to be shown in tables 1 and 2.
4. Hardness test
A detection instrument: 500 g pencil hardness tester
The detection method comprises the following steps: the pencil hardness of the film was measured using a Mitsubishi pencil according to ASTM D3363, and each sample (film prepared in examples 1 to 10) was tested in parallel three times and averaged.
The pencil hardness of the film layers of the optical film samples coated on the PET substrate is all H, and the test results are shown in tables 1 and 2.
Claims (10)
1. An antistatic antireflection optical film includes a flexible substrate; the flexible substrate is characterized by further comprising an anti-static coating film layer attached to at least one side surface of the flexible substrate, and an antireflection coating film layer is further attached to the anti-static coating film layer.
2. The antistatic antireflection optical film according to claim 1, wherein antistatic coating layers are respectively attached to the surfaces of both sides of the flexible substrate, and an antireflection coating layer is attached to the antistatic coating layer on at least one side;
preferably, the anti-static coating layers on the surfaces of the two sides of the flexible substrate are respectively attached with an anti-reflection coating layer;
preferably, the flexible substrate is a polyethylene terephthalate (PET) film;
preferably, the thickness of the anti-static coating layer is 100-2000nm, and more preferably 100-1500 nm;
preferably, the thickness of the antireflection coating layer is 80-400nm, and more preferably 100-160 nm.
3. The preparation method of the anti-static antireflection optical film is characterized by comprising the following steps of:
firstly coating antistatic coating liquid on at least one side surface of a flexible substrate, pre-drying, then coating antireflection coating liquid, and pre-drying again and performing ultraviolet curing to obtain an antistatic antireflection optical film;
preferably, the antistatic coating liquid or the antireflection coating liquid is coated in a roll-to-roll coating mode, and a gravure roll coating head or a slit coating head is recommended to be used for coating;
preferably, the linear speed of the coating of the antistatic masking liquid is 15-35m/min, the pre-drying temperature is 50-80 ℃, and the drying time is 0.5-1 min;
preferably, the linear speed of the antireflection coating liquid coating is 15-30m/min, the pre-drying temperature is 50-70 ℃, the pre-drying time is 0.5-1min, and the energy density of ultraviolet curing is 800 mJ/cm-2Work ofThe specific density is 40-80mW/cm2。
4. The preparation method of the antistatic antireflection optical film as claimed in claim 3, wherein the antistatic masking liquid comprises a nano oxide, a solvent and a film-forming aid, and the mass ratio of each component is as follows: 2-10 parts of nano oxide, 90-98 parts of solvent and 0.01-0.025 part of film-forming assistant;
preferably, the nano oxide is selected from at least one of antimony-doped tin dioxide, aluminum-doped zinc oxide and titanium oxide; more preferably aluminum-doped zinc oxide; most preferably, the nano-oxide is an inorganic nano-particle selected from one of antimony-doped tin dioxide nano-powder, aluminum-doped zinc oxide nano-powder and titanium oxide nano-powder;
preferably, the solvent is selected from at least one of water and ethanol;
preferably, the film-forming assistant is at least one selected from polyvinyl alcohol, polyvinylpyrrolidone, modified comb acrylic ester copolymer surface assistant, hydroxyl polyether type organic silicon slipping agent, macromolecular polyether modified acrylic ester surface assistant, polyether modified dimethyl polysiloxane organic silicon surface assistant, polyacrylate type leveling assistant and epoxy phenyl vinyl silane oligomer;
preferably, the antireflection coating liquid comprises resin, hollow organosilicon nanoparticles, a solvent, a wetting and leveling agent and a photoinitiator, and the mass ratio of each component is as follows: 0.5 to 1.5 percent of resin, 1.0 to 3.5 percent of hollow organic silicon particles, 92 to 98 percent of solvent, 0.05 to 0.15 percent of wetting and leveling agent and 0.05 to 0.15 percent of photoinitiator;
preferably, the resin comprises urethane acrylate or epoxy acrylate;
preferably, the resin is at least one selected from the group consisting of aliphatic urethane acrylate, epoxy acrylate, aromatic urethane acrylate, tris (2-hydroxyethyl) isocyanurate triacrylate, (2) ethoxylated bisphenol a dimethacrylate, urethane acrylate, high functionality urethane acrylate, and 1,4 butanediol dimethacrylate;
preferably, the particle diameter of the hollow organosilicon nano particle is 20-120nm, and the wall thickness is 5-10 nm; preferably, the particle size is 40-80nm, and the wall thickness is 5-8 nm;
preferably, the solvent is selected from at least two of ethyl acetate, butyl acetate, methyl isobutyl ketone, isophorone, propylene glycol monomethyl ether, propylene glycol methyl ether acetate, isopropanol, and isobutanol;
preferably, the wetting and leveling agent is at least one selected from a hydroxy polyether type organic silicon slipping agent, a macromolecular polyether modified acrylate surface auxiliary agent, a polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent, a polyacrylate type leveling auxiliary agent, an epoxy phenyl vinyl silane oligomer, a short-chain perfluorinated fluorine-containing surfactant and a solvent type fluorinated polymer;
preferably, the photoinitiator is at least one selected from the group consisting of 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- (4-methylthiophenyl) -2-morpholin-1-one, difunctional alpha-hydroxy ketone, 2-hydroxy-methylphenyl propane-1-one, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide.
5. The preparation method of the antistatic masking liquid is characterized by comprising the following steps:
(1) preparing a dispersion liquid A: dispersing inorganic nano particles into a solvent, and stirring and uniformly mixing at room temperature;
(2) preparing an antistatic masking liquid: and mixing the dispersion liquid A, the solvent and the film-forming assistant, and uniformly stirring to obtain the antistatic masking liquid.
6. An antistatic masking liquid is characterized by comprising a nano oxide, a solvent and a film forming auxiliary agent; the mass ratio of each component is as follows:
nano-oxide: 2-10,
solvent: 90-98,
film-forming auxiliary agent: 0.01-0.025;
preferably, the nano oxide is selected from at least one of antimony-doped tin dioxide, aluminum-doped zinc oxide and titanium oxide; more preferably aluminum-doped zinc oxide; most preferably, the nano-oxide is an inorganic nano-particle selected from one of antimony-doped tin dioxide nano-powder, aluminum-doped zinc oxide nano-powder and titanium oxide nano-powder;
preferably, the solvent is selected from at least one of water and ethanol;
preferably, the film-forming assistant is at least one selected from polyvinyl alcohol, polyvinylpyrrolidone, modified comb acrylic ester copolymer surface assistant, hydroxyl polyether type organic silicon slipping agent, macromolecular polyether modified acrylic ester surface assistant, polyether modified dimethyl polysiloxane organic silicon surface assistant, polyacrylate type leveling assistant and epoxy phenyl vinyl silane oligomer;
preferably, the antistatic coating liquid is obtained by the production method according to claim 5.
7. The preparation method of the antireflection coating liquid is characterized by comprising the following steps of:
(1) preparing a solvent A: uniformly mixing at least two solvents, and uniformly stirring at room temperature;
(2) preparation of resin dispersion B: mixing at least two resins, adding a solvent A, stirring for 30min at room temperature, and uniformly mixing;
(3) preparing an antireflection coating solution: stirring and mixing the resin dispersion liquid B, the solvent A and the hollow organic silicon nano particles uniformly at room temperature; and adding the wetting and leveling agent, continuing stirring, finally adding the photoinitiator, stirring, and filtering to obtain the antireflection coating liquid.
8. The antireflection coating liquid is characterized by comprising resin, hollow organic silicon nano particles, a solvent, a wetting and leveling agent and a photoinitiator, wherein the mass ratio of each component is as follows:
resin: 0.5-1.5,
hollow silicone particles: 1.0-3.5,
solvent: 92-98,
wetting and leveling agent: 0.05-0.15,
photoinitiator (2): 0.05-0.15.
9. The anti-reflection coating according to claim 8, characterized in that said resin comprises urethane acrylate or epoxy acrylate;
preferably, the resin is at least one selected from the group consisting of aliphatic urethane acrylate, epoxy acrylate, aromatic urethane acrylate, tris (2-hydroxyethyl) isocyanurate triacrylate, (2) ethoxylated bisphenol a dimethacrylate, urethane acrylate, high functionality urethane acrylate, and 1,4 butanediol dimethacrylate;
preferably, the particle diameter of the hollow organosilicon nano particle is 20-120nm, and the wall thickness is 5-10 nm; preferably, the particle size is 40-80nm, and the wall thickness is 5-8 nm;
preferably, the solvent is selected from at least two of ethyl acetate, butyl acetate, methyl isobutyl ketone, isophorone, propylene glycol monomethyl ether, propylene glycol methyl ether acetate, isopropanol, and isobutanol;
preferably, the wetting and leveling agent is at least one selected from a hydroxy polyether type organic silicon slipping agent, a macromolecular polyether modified acrylate surface auxiliary agent, a polyether modified dimethyl polysiloxane organic silicon surface auxiliary agent, a polyacrylate type leveling auxiliary agent, an epoxy phenyl vinyl silane oligomer, a short-chain perfluorinated fluorine-containing surfactant and a solvent type fluorinated polymer;
preferably, the photoinitiator is selected from at least one of 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-one, bifunctional α -hydroxy ketone, 2-hydroxy-methylphenyl propane-1-one, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide;
preferably, the antireflection coating liquid is obtained by the production method according to claim 7.
10. Use of the antistatic antireflection optical film according to claim 1 or 2 for protection of display devices.
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| CN114920983A (en) * | 2022-05-23 | 2022-08-19 | 晋江市亿兴橡塑有限公司 | Wear-resistant antistatic PVC artificial floor leather and preparation method thereof |
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