CN115232347B - Optical film and preparation method thereof - Google Patents

Optical film and preparation method thereof Download PDF

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Publication number
CN115232347B
CN115232347B CN202211040041.4A CN202211040041A CN115232347B CN 115232347 B CN115232347 B CN 115232347B CN 202211040041 A CN202211040041 A CN 202211040041A CN 115232347 B CN115232347 B CN 115232347B
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hard coating
coating
coupling agent
silane coupling
hard
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CN115232347A (en
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张永汉
程军
刘永春
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Zhejiang Xuyuan Optoelectronic New Material Technology Co ltd
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Zhejiang Xuyuan Optoelectronics New Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C09D163/10—Epoxy resins modified by unsaturated compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/111—Anti-reflection coatings using layers comprising organic materials
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14—Protective coatings, e.g. hard coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2300/00—Characterised by the use of unspecified polymers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2400/00—Characterised by the use of unspecified polymers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/06—Unsaturated polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2475/04—Polyurethanes
    • C08J2475/14—Polyurethanes having carbon-to-carbon unsaturated bonds

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Abstract

The application relates to an optical film and a preparation method thereof, and belongs to the technical field of optical films. The preparation method comprises the following steps: preparing a hard coating: and coating the hard coating liquid on one surface of the transparent base film, and performing incomplete UV curing on the hard coating liquid after drying to form a hard coating, wherein the curing rate of the hard coating is less than 60%. Alkali treatment is carried out on the hard coating: soaking the hard coating in alkali liquor to convert part of unreacted acrylic double bonds in the hard coating into hydroxyl groups, and then taking out, washing and drying. Preparing an antireflection layer: coating the anti-reflection coating liquid on the surface of the hard coating after alkali treatment, and then drying and UV curing to form an anti-reflection layer; the anti-reflection coating liquid contains a hydrolyzed silane coupling agent, wherein one end of the hydrolyzed silane coupling agent is double bond, and the other end is-Si-OH. The preparation method can improve the binding force between the hard coating and the anti-reflection layer so as to improve the scratch resistance and durability of the optical film.

Description

Optical film and preparation method thereof
Technical Field
The application relates to the technical field of optical films, in particular to an optical film and a preparation method thereof.
Background
Portable display devices, such as mobile phones, tablet computers, electronic books, and notebook computers, have been developed with the development of artificial intelligence, and liquid crystal display panels have been developed in the directions of high definition, high brightness, large size, wide viewing angle, and the like. When these portable display devices are used outdoors, the color and definition of the display content are often reduced by the reflection of external light from the display screen due to the strong outdoor light. In order to improve the visibility and durability of the display screen, an anti-dazzle film is attached to the surface of the display screen, and the surface of the anti-dazzle film is provided with a concave-convex structure, so that when external reflected light is reflected, the reflected light is scattered to different angles due to the concave-convex structure, the influence of the reflected light on vision is reduced, the concave-convex structure on the surface of the coating is generally realized by adding particles or mechanically stamping in the coating, but the roughened anti-dazzle film also reduces the definition of a display image.
Under the environment that external light is strong, the visibility effect of the display screen is reduced, and two methods are generally available for improving the visibility, namely, the brightness of the screen is improved, the reflection of the screen is reduced, the power consumption is increased, the standby time of the intelligent terminal which is not long is further shortened, so that more and more display terminal manufacturers can adopt an antireflection film on the surface of the screen, the problem of visibility of the electronic product in the indoor and outdoor environment is solved, the power consumption is reduced, and the user experience is greatly improved.
The antireflection film is prepared by plating a layer of material with high and low refractive index stacked on the surface of a display screen, when light rays pass through different media, different optical path differences exist between different refractive indexes and film thicknesses, and the reflection optical path differences coming out of different media can form interference through the design of a film layer structure and the material, so that the antireflection effect is achieved. There are two common practices, one is wet coating of hard coatings, antireflection layers, etc.; the other is to coat a hard coating layer by a wet method, then coat an anti-fingerprint layer by a wet method after sputtering an anti-reflection layer by a dry method, and the wet method coating gradually replaces the sputtering method to form a main stream method due to high investment cost of dry sputtering equipment and low production efficiency.
The wet coating process is to coat a hard coating layer of 3-5 microns on the surface of transparent base film, and then coat an antireflection layer of 80-120 nm thickness on the hard coating layer.
Disclosure of Invention
The inventor researches have found that, since the anti-reflective layer of the anti-reflective film is thinner, the hardness and scratch resistance of the surface of the anti-reflective film are generally provided by the lower hard coating layer, and since portable 3C display devices including mobile phones, tablet computers, electronic books, vehicle-mounted displays and the like mostly adopt touch screens, the scratch resistance and durability of the surface of the film material are the other one except the requirement of the optical anti-reflective performance, so that the stronger the interlayer bonding force between the anti-reflective layer and the hard coating layer is, the longer the durability of the anti-reflective film is used.
Accordingly, an object of an embodiment of the present application includes providing an optical film and a method of manufacturing the same, which improves a coupling force between an anti-reflection layer and a hard coating layer to improve durability of the optical film in use.
In a first aspect, the present application provides a method for producing an optical film, comprising the steps of:
preparing a hard coating: coating a hard coating liquid on one surface of a transparent base film, and drying the hard coating liquid and then incompletely performing UV curing to form a hard coating, wherein the curing rate of the hard coating is less than 60%;
alkali treatment is carried out on the hard coating: soaking the hard coating in alkali liquor to convert part of unreacted acrylic double bonds in the hard coating into hydroxyl groups, and then taking out, washing and drying;
Preparing an antireflection layer: coating the anti-reflection coating liquid on the surface of the hard coating after alkali treatment, and then drying and UV curing to form an anti-reflection layer; the anti-reflection coating liquid contains a hydrolyzed silane coupling agent, wherein one end of the hydrolyzed silane coupling agent is double bond, and the other end is-Si-OH.
In the technical scheme, when the hard coating liquid is subjected to UV curing, the curing is incomplete, the curing rate is less than 60%, more unreacted acrylic double bonds are formed in the cured hard coating, after alkali washing, the unreacted acrylic double bonds can be converted into hydroxyl groups, and then when the antireflection layer is cured, as the hydrolyzed silane coupling agent is contained in the antireflection coating liquid, one end of the hydrolyzed silane coupling agent is a double bond, and the other end of the hydrolyzed silane coupling agent is-Si-OH, the antireflection coating liquid is bonded with the hydroxyl groups formed after alkali washing in the hard coating in the drying process, and the double bonds in the silane coupling agent react with the double bonds in the resin in the antireflection coating liquid during curing, so that firm chemical bond connection is formed between the hard coating and the antireflection layer, the bonding force between the hard coating and the antireflection layer is improved, and the scratch resistance and durability of the optical film are improved.
In some embodiments of the present application, the hard coat layer has a cure rate of 30% to 60%.
In the above technical scheme, the curing rate of the hard coating is within the range, so that the hard coating can be cured into a layer structure on one hand, and more unreacted acrylic double bonds can be remained in the hard coating on the other hand, so that the bonding force between the hard coating and the anti-reflection layer is increased through subsequent treatment.
In some embodiments of the present application, in preparing the hard coat layer, the components of the hard coat liquid include UV-curable oligomer, reactive monomer, and initiator, and the amount of initiator/(the amount of UV-curable oligomer+the amount of reactive monomer) ×100% =3 to 6%; the energy of UV curing is 200-350 mj/cm 2.
In the technical scheme, the addition amount of the initiator is 3-6%, and the curing rate of the hard coating can be 30-60% by matching with the UV curing energy of 200-350 mj/cm 2.
In some embodiments of the application, the conditions of the alkali treatment include: soaking the hard coating in alkali liquor with the mass concentration of 8-12% and the temperature of 40-60 ℃ for 1-3 min; wherein the alkali liquor is sodium hydroxide and/or potassium hydroxide solution.
In the above technical scheme, the alkali treatment can convert more unreacted acrylic double bonds into hydroxyl groups so as to realize the subsequent linkage with the hydrolyzed silane coupling agent.
In some embodiments of the present application, the components of the antireflection coating liquid include an antireflection coating and a hydrolyzed silane coupling agent, and (the amount of hydrolyzed silane coupling agent/the amount of active ingredient of the antireflection coating) ×100% =0.5 to 5%.
In the technical scheme, the hydrolyzed silane coupling agent is added into the anti-reflection coating liquid, so that on one hand, the-Si-OH in the hydrolyzed silane coupling agent can be bonded with the hydroxyl in the hard coating after alkaline washing in the curing process; on the other hand, the double bond on the silane coupling agent may react with the double bond on the resin in the anti-reflective coating material in order to improve the bonding force between the hard coating layer and the anti-reflective layer.
In some embodiments of the present application, the method for preparing the hydrolyzed silane coupling agent includes: and (3) reacting a silane coupling agent solution with a double bond at one end for 2 hours and more under the condition that the pH value is 4.0-5.0, so that the-Si-X is hydrolyzed into the-Si-OH, wherein the solvent in the solution comprises water and ethanol.
In the technical scheme, more-Si-X in the silane coupling agent can be hydrolyzed into-Si-OH.
In some examples of the present application, the mass ratio of the double bond-containing silane coupling agent to water and ethanol was 1 (0.8 to 1.2) to 15 to 25.
In the technical scheme, the addition amount of the ethanol is more, so that the silane coupling agent can be hydrolyzed better.
In some embodiments of the present application, the silane coupling agent is at least one of 3-methacryloxypropyl trimethoxysilane, 3-methacryloxypropyl methyl dimethoxy silane, 3-methacryloxypropyl methyl diethoxy silane, 3-methacryloxypropyl triethoxy silane, and 3-acrylic propyl trimethoxy silane.
In a second aspect, an embodiment of the present application provides an optical film prepared by the above-mentioned preparation method. The binding force between the hard coating and the antireflection of the optical film is high, and the scratch resistance and the durability of the optical film are improved.
In some embodiments of the present application, the hard coating layer has a thickness of 3 to 5 μm and the antireflection layer has a thickness of 0.09 to 0.11 μm. The thickness of each layer can lead to better comprehensive performance of the optical film.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a process flow chart of a preparation method of an optical film according to an embodiment of the present application.
Detailed Description
Fig. 1 is a process flow chart of a preparation method of an optical film according to an embodiment of the present application. Referring to fig. 1, the preparation method of the optical film provided by the application comprises the following steps:
s110, preparing a hard coating: and coating the hard coating liquid on one surface of the transparent base film, and performing incomplete UV curing on the hard coating liquid after drying to form a hard coating, wherein the curing rate of the hard coating is less than 60%.
Wherein, the hard coating liquid comprises the following components: 15 to 30 parts by weight of a UV curable oligomer, 4 to 8 parts by weight of a reactive monomer, 1 to 3 parts by weight of an initiator, 60 to 80 parts by weight of a solvent and 0.1 to 0.2 part by weight of a leveling agent, and the amount of the initiator/(the amount of UV curable oligomer+the amount of reactive monomer) ×100% =3 to 6%.
As an example, the UV-curable oligomer is added in the hard coat liquid in an amount of 15 parts by weight, 20 parts by weight, 25 parts by weight or 30 parts by weight; the addition amount of the reactive monomer is 4 parts by weight, 5 parts by weight, 6 parts by weight, 7 parts by weight or 8 parts by weight; the addition amount of the initiator is 1 part by weight, 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight or 3 parts by weight; the addition amount of the solvent is 60 parts by weight, 65 parts by weight, 70 parts by weight, 75 parts by weight or 80 parts by weight; the addition amount of the leveling agent is 0.1 weight part, 0.15 weight part or 0.2 weight part; and the amount of initiator/(amount of UV curable oligomer+amount of reactive monomer) ×100% is 3%, 3.5%, 4%, 4.5%, 5%, 5.5% or 6%.
Wherein the UV curable oligomer can be one or more of polyurethane acrylate, epoxy acrylate, polyester acrylate and pure acrylic acid.
The reactive monomer may be one or more of ortho-phenylphenoxyethyl acrylate, ethylene glycol dimethacrylate, propoxylated neopentyl glycol diacrylate, propoxylated glycerol triacrylate, 1, 4-butanediol diacrylate, 1, 6-hexanediol diacrylate, trimethylolethane triacrylate, ethoxylated pentaerythritol tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, and dipentaerythritol hexaacrylate.
The photoinitiator is 1-hydroxycyclohexyl phenyl ketone (184), 1' - (methylenebis-4, 1-phenylene) bis [ 2-hydroxy-2-methyl-1-propanone ] (127), 2-hydroxy-methylphenyl propane-1-one (1173), 2-methyl-1- (4-methylthiophenyl) -2-morpholino-1-propanone (907), benzoin dimethyl ether (651), 2,4,6 (trimethylbenzoyl) diphenyl phosphine oxide (TPO), and the like.
The solvent can be one or more of alcohols, ketones and esters; wherein the alcohols are one or more of methanol, ethanol, n-propanol, isopropanol, n-butanol and isobutanol; ketones such as one or more of acetone, butanone, methyl ethyl ketone, methyl isobutyl ketone, and cyclohexanone; esters such as one or more of methyl acetate, ethyl acetate, propyl acetate and butyl acetate.
The leveling agent may be one or more of a fluorine-based leveling agent, an organosiloxane leveling agent, and an organosilicon modified acrylic leveling agent. Optionally, the leveling agent can be BYK-UV 3500, BYK-UV 3505, BYK-UV 3530, BYK-UV 3535, BYK-UV 3560, BYK-UV 3565; di-high TEGO Flow 300, flow 375, flow 425, TEGO Glide 415, glide 450; FTERGENT 602A of Nieuses, japan; one or more of F-445, F-470, F-479, F-553, F-556 of Dakai ink chemistry.
After the hard coating liquid is coated, the hard coating liquid is dried in the following way: drying at 60-110 deg.c for 2-3 min. As an example, the hard coating solution is dried at a temperature of 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, or 110 ℃; the drying time of the hard coating liquid is 2min, 2.2min, 2.5min, 2.8min or 3min.
In the application, the UV curing oligomer and the active monomer in the hard coating liquid contain acrylic double bonds, and when the curing rate of the hard coating is less than 60%, more acrylic double bonds in the hard coating are uncured (do not participate in reaction).
Illustratively, the hard coat layer has a cure rate of 20%, 30%, 40%, 50% or 60%. Alternatively, the hard coat layer has a cure rate of 30% to 60%.
When the amount of the initiator added to the hard coat liquid is 1 to 3 parts by weight, the energy of UV curing is 200 to 350mj/cm 2, and the curing rate of the hard coat layer can be 30 to 60%. As an example, the UV curing energy is 200mj/cm 2、250mj/cm2、300mj/cm2 or 350mj/cm 2.
Optionally, the transparent base film has a thickness of 15 to 250 μm; alternatively, the transparent base film has a thickness of 25 to 80 μm, 80 to 150 μm, or 150 to 250 μm. As an example, the thickness of the transparent base film is 25 μm, 38 μm, 40 μm, 50 μm, 60 μm, 80 μm, 100 μm, 125 μm, 188 μm, or 250 μm.
The method of applying the hard coating liquid may be a slit coating method, a micro gravure coating method, a blade coating method, a Mayer bar coating method, a roll coating method, and a blade coating method to form a coating layer. If the coating mode is selected to be a micro gravure coating method and a slit coating method, the coating effect can be better.
In the application, the solid content of the hard coating liquid is 20-40%, and the coating amount of the hard coating liquid is 15-30 g/m 2. By the combination of the solid content and the coating amount, the thickness of the hard coat layer can be kept between 3 and 5 μm. As an example, the solids content of the hard coating liquid is 20%, 25%, 30%, 35% or 40%; the coating amount of the hard coating liquid is 20g/m 2、25g/m2、30g/m2、35g/m2 or 42g/m 2; the thickness of the hard coat layer was 3 μm, 3.5 μm, 4 μm, 4.5 μm or 5 μm.
S120, alkali treatment is carried out on the hard coating: soaking the hard coating in alkali liquor to convert part of unreacted acrylic double bonds in the hard coating into hydroxyl groups, and then taking out, washing and drying.
Because the curing rate is less than 60%, the hard coating after curing has more unreacted acrylic double bonds, and the hard coating can convert the unreacted acrylic double bonds into hydroxyl groups after alkali washing.
The specific mode of alkali washing is as follows: soaking the hard coating in alkali liquor with the mass concentration of 8-12% and the temperature of 40-60 ℃ for 1-3 min; wherein the alkali liquor is sodium hydroxide and/or potassium hydroxide solution.
Illustratively, the lye is 8%, 9%, 10%, 11% or 12% by mass; the temperature of the alkali liquor is 40 ℃, 45 ℃, 50 ℃, 55 ℃ or 60 ℃; the time of soaking in alkali liquor is 1min, 1.5min, 2min, 2.5min or 3min.
S130, preparing an antireflection layer: coating the anti-reflection coating liquid on the surface of the hard coating after alkali treatment, and then drying and UV curing to form an anti-reflection layer; the anti-reflection coating liquid contains a hydrolyzed silane coupling agent, wherein one end of the hydrolyzed silane coupling agent is double bond, and the other end is-Si-OH.
The anti-reflection coating liquid contains the hydrolyzed silane coupling agent, one end of the hydrolyzed silane coupling agent is double bond, and the other end is-Si-OH, so that the anti-reflection coating liquid is bonded with hydroxyl groups formed after alkaline washing in the hard coating in the drying process, and the double bond in the silane coupling agent reacts with the double bond in the resin in the anti-reflection coating liquid during curing, thereby forming firm chemical bond connection between the hard coating and the anti-reflection layer, improving the bonding force between the hard coating and the anti-reflection layer, and improving the scratch resistance and durability of the optical film.
The anti-reflection coating liquid comprises the following components: 15 to 25 parts by weight of an antireflective coating, 0.1 to 2 parts by weight of a hydrolyzed silane coupling agent, 70 to 90 parts by weight of a solvent, and 0.1 to 0.2 part by weight of a leveling agent, and (the amount of an active ingredient of the hydrolyzed silane coupling agent/the amount of an active ingredient of the antireflective coating) ×100% =0.5 to 5%.
As an example, the addition amount of the antireflection coating is 15 parts by weight, 20 parts by weight, or 25 parts by weight; the addition amount of the hydrolyzed silane coupling agent is 0.1 part by weight, 0.2 part by weight, 0.5 part by weight, 1 part by weight, 1.5 parts by weight or 2 parts by weight; the addition amount of the solvent is 70 parts by weight, 75 parts by weight, 80 parts by weight, 85 parts by weight or 90 parts by weight; the addition amount of the leveling agent is 0.1 weight part, 0.15 weight part or 0.2 weight part; and (amount of active ingredient of silane coupling agent after hydrolysis/amount of active ingredient of antireflection coating) ×100% is 0.5%, 1%, 2%, 3%, 4% or 5%.
Among them, the anti-reflection coating is commercially available anti-reflection coating, for example: SL-023 from chemical production of Sichuan of Japan, ELCOM P-5062 from chemical production of volatile catalyst, SL-044 from chemical production of Sichuan of Japan, etc. The amount of the active ingredient of the anti-reflection coating refers to the solid content of the anti-reflection coating, that is, the amount of the solvent removed after curing.
The solvent may be a solvent in the hard coating solution, and the leveling agent may be a leveling agent in the hard coating solution, which will not be described herein.
The silane coupling agent is at least one of 3-methacryloxypropyl trimethoxy silane, 3-methacryloxypropyl methyl dimethoxy silane, 3-methacryloxypropyl methyl diethoxy silane, 3-methacryloxypropyl triethoxy silane and 3-acrylic propyl trimethoxy silane.
The hydrolyzed silane coupling agent is added into the anti-reflection coating liquid, and the specific treatment mode can be as follows: and adding the silane coupling agent into a hydrolysis solvent, and reacting under the target condition to obtain the hydrolyzed silane coupling agent, wherein the added weight parts of the hydrolyzed silane coupling agent are the amount of the hydrolyzed silane coupling agent in the anti-reflection coating liquid, and the amount of the effective components of the hydrolyzed silane coupling agent is consistent with the amount of the silane coupling agent before hydrolysis, and the other parts are ignored.
For example: the anti-reflection coating liquid comprises the following components: 20 parts by weight of an anti-reflection coating, 1 part by weight of a hydrolyzed silane coupling agent, 80 parts by weight of a solvent and 0.15 part by weight of a leveling agent. The preparation method of the hydrolyzed silane coupling agent comprises the following steps: the silane coupling agent was added to the hydrolysis solvent (although an acid solution was required to be added to adjust the pH of the solution, the amount of the acid solution added was small and negligible), and the reaction was carried out under the target conditions to obtain 1 part by weight of the hydrolyzed silane coupling agent, and at this time, the solution in the hydrolyzed silane coupling agent was added together, which corresponds to the addition of 1 part by weight of the hydrolyzed silane coupling agent.
Optionally, the hydrolysis method of the silane coupling agent comprises: and (3) reacting a silane coupling agent solution with a double bond at one end for 2 hours and more under the condition that the pH value is 4.0-5.0, so that the-Si-X is hydrolyzed into the-Si-OH, wherein the solvent in the solution comprises water and ethanol. Further, the mass ratio of the silane coupling agent containing double bonds to water and ethanol is 1 (0.8-1.2) to 15-25.
Illustratively, the pH of the hydrolysis is 4.0, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, 4.9, or 5.0; the hydrolysis time is 2h, 2.5h, 3h, 3.5h or 4h; the mass ratio of the addition amount of the silane coupling agent, the water and the ethanol is 1:0.8:15, 1:1:15, 1:1.2:15, 1:0.8:20, 1:0.8:25, 1:1:20, 1:1:25, 1:1.2:20 or 1:1.2:25 in sequence.
For example: 1 part by weight of a silane coupling agent solution containing a double bond at one end is reacted for 2 hours or more under the condition that the pH value of the solution is 4.0-5.0 (the pH value of the solution is adjusted by adding an acid solution, but the addition amount of the acid solution is small and can be ignored), so that-Si-X is hydrolyzed into-Si-OH, wherein the solvent in the solution comprises 1 part by weight of water and 20 parts by weight of ethanol, 22 parts by weight of a hydrolyzed silane coupling agent is obtained, and the effective component of the hydrolyzed silane coupling agent is 1 part by weight.
After the anti-reflection coating liquid is coated, the coating liquid is firstly dried for 1 to 3 minutes at the temperature of between 70 and 100 ℃, and then is irradiated by ultraviolet under the conditions that the oxygen concentration is less than 500ppm and the light dosage is 300 to 500mj/cm 2, so that the low refractive index layer is obtained. The anti-reflection layer is very thin, and ultraviolet light curing reaction is carried out under the condition of low oxygen, so that oxygen polymerization inhibition is avoided, and the wear resistance of the optical film is better.
Alternatively, the method of applying the antireflection coating liquid may be a slit coating method, a micro gravure coating method, a blade coating method, a Mayer bar coating method, a roll coating method, and a blade coating method to form a coating layer. If the coating mode is selected to be a micro gravure coating method and a slit coating method, the coating effect can be better.
As an example, the drying conditions of the antireflection coating liquid are: drying at 70deg.C for 3min; or drying at 85deg.C for 2min; or drying at 100deg.C for 1min; the conditions of ultraviolet irradiation are as follows: ultraviolet irradiation under the conditions that the oxygen concentration is 100ppm and the light dose is 350mj/cm 2; or ultraviolet irradiation under the conditions of 200ppm of oxygen and 400mj/cm 2 of light dose; or ultraviolet irradiation under the conditions of 300ppm of oxygen and 450mj/cm 2 of light dose; or ultraviolet irradiation at an oxygen concentration of 400ppm and a light dose of 500mj/cm 2.
Optionally, the solid content of the anti-reflection coating liquid is 2-3%, and the coating amount of the anti-reflection coating liquid is 3-10 g/m 2. The thickness of the antireflection layer is also made to be 0.09 to 0.11 μm by the combination of the solid content and the coating amount. As an example, the solid content of the antireflective coating liquid is 2%, 2.2%, 2.4%, 2.6%, 2.8% or 3.0%; the coating amount of the anti-reflection coating liquid is 3g/m 2、5g/m2、8g/m2 or 10g/m 2; the thickness of the anti-reflection layer may be 0.09 μm, 0.10 μm or 0.11 μm.
The optical film can be prepared by the method, and comprises a transparent base film, a hard coating attached to the surface of the transparent base film and an antireflection layer attached to the surface of the hard coating. Wherein the thickness of the hard coating layer is 3-5 mu m, and the thickness of the antireflection layer is 0.09-0.11 mu m.
When the hard coating liquid is subjected to UV curing, the curing rate is less than 60%, more unreacted acrylic double bonds are formed in the cured hard coating, after alkali washing, the unreacted acrylic double bonds can be converted into hydroxyl groups, then when the anti-reflection coating layer is cured, as the anti-reflection coating liquid contains the hydrolyzed silane coupling agent, one end of the hydrolyzed silane coupling agent is double bonds, and the other end is-Si-OH, the anti-reflection coating liquid is bonded with the hydroxyl groups formed after alkali washing in the hard coating layer in the drying process, and the double bonds in the silane coupling agent react with the double bonds in the resin in the anti-reflection coating liquid in the curing process, so that firm chemical bond connection is formed between the hard coating layer and the anti-reflection layer, the bonding force between the hard coating layer and the anti-reflection layer is improved, and the scratch resistance and durability of the optical film are improved.
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Examples
The present embodiment provides an optical film including a transparent base film and a hard coat layer attached to the transparent base film, and an antireflection layer attached to the hard coat layer, which are laminated in this order from bottom to top. The preparation method of the optical film comprises the following steps:
(1) And coating the hard coating liquid on the transparent base film, drying for 2min at 100 ℃, and then irradiating with ultraviolet to obtain the hard coating.
(2) Soaking the hard coating in alkali liquor, taking out, washing with water and drying.
(3) And coating the anti-reflection coating liquid on the soaked hard coating, drying for 2min at 80 ℃, and irradiating with high-pressure mercury lamp ultraviolet rays with the oxygen concentration of 200ppm and the light dosage of 350mj/cm 2 to obtain the anti-reflection layer.
Wherein the hard coating liquid and the anti-reflection coating liquid are shown in the following table:
TABLE 1 hard coat liquid HC-1 composition
TABLE 2 hard coat liquid HC-2 composition
TABLE 3 hard coat liquid HC-3 composition
TABLE 4 composition of anti-reflective coating liquid LR-1
TABLE 5 composition of anti-reflective coating liquid LR-2
TABLE 6 composition of anti-reflective coating liquid LR-3
TABLE 7 composition of anti-reflective coating liquid LR-4
TABLE 8 composition of anti-reflective coating liquid LR-5
The preparation method of the hydrolytic silane coupling agent-1 comprises the following steps: KBM-503 of japan, deionized water and ethanol were mixed in a weight ratio of 1:1:18, and hydrolyzed at 60 ℃ for 4 hours by adjusting ph=4.0 with oxalic acid.
The preparation method of the hydrolytic silane coupling agent-2 comprises the following steps: the Japanese Xinyue KBM-5103, deionized water and ethanol are mixed according to the weight ratio of 1:1:18, oxalic acid is used for adjusting pH=4.0, and hydrolysis is carried out for 4 hours at the temperature of 60 ℃.
Test example 1
The preparation conditions of the optical films provided in examples 1 to 12 and comparative examples 1 to 4 are shown in Table 9, and the properties of the optical films are examined in Table 10. The respective parameter calculation methods or test methods in tables 9 and 10 are as follows:
TABLE 9 summary of conditions for producing optical films
Wherein, 1, coating thickness test:
The thickness of the hard coat layer and the thickness of the antireflection layer of the optical film were measured using the light diffraction principle using the germany NXT coating thickness gauge ETA-SST thickness test system.
2. Degree of crosslinking (%) of UV curing of the hard coating surface:
After the hard coating liquid on the transparent polymer-based film to be tested is dried, the absorption peak and the penetration intensity of the hard coating surface at each wave band before and after UV curing are measured by adopting an attenuated total reflection method (Attenuated Total Reflectance, ATR) under the condition of a scanning range of 650cm -1～4000cm-1 by using a Simer Fecolet iN10 Fourier transform infrared spectrometer, and the crosslinking degree (Conversion) after UV curing is calculated according to the following formula.
Wherein:
AFacryl absorption intensity at 809cm -1 after ultraviolet light curing;
AIacryl absorption intensity at 809cm -1 before ultraviolet light is cured;
Afc=o, absorption intensity at 1720cm -1 after uv curing;
AIc = o absorption intensity at 1720cm -1 before uv light curing.
Wherein the absorption intensity a= -log t;
wherein T refers to the penetrating strength of the coating at 809cm -1、1720cm-1 before and after ultraviolet curing.
3. Water contact angle before alkali wash and water contact angle after alkali wash:
Water contact angle before alkaline wash (°): after a JC2000D water contact angle measuring instrument of shanghai middle morning digital equipment limited was used, purified water was injected into a connecting tube at one end of a measuring needle and water drops from the other end of the measuring needle were flown out, a hard coating film to be measured was taken in a size of 1cm×3cm, the coating film was placed face up and horizontally on a measuring platform and fixed with an adhesive tape, a button was rotated to cause the needle to extrude a liquid drop (set to 2.0 mL), the platform with the hard coating film to be measured was lifted until it was brought into contact with the liquid drop, and the water contact angle was calculated by an angle measuring method through measuring software.
Water contact angle after basicity (°): the method is consistent with the method for testing the water contact angle before alkali washing, except that the object to be tested is a hard coating layer after alkali washing (the hard coating layer after the step (2)).
Antireflection layer water contact angle: consistent with the method of testing the water contact angle prior to alkaline washing, the object of the test was only the anti-reflective layer of the optical film.
4. Penetration (%), haze (%):
The transmittance and haze of the optical film were measured by the transmitted light method using a Japanese electrochromic NDH 2000N type haze meter according to JIS K-7105.
5. Adhesion of the hardcoat layer to the antireflective layer:
the optical film was put in boiling water at 100 ℃ for 1 hour, then dried, and according to standard ASTM D-3359, a hundred grids were drawn on the surface of the coating by a hundred grid knife, and after a 3m 600 type adhesive tape was stuck on the drawn hundred grids, the adhesive tape was rapidly torn off in a 180 degree direction, and the peeling state of the hundred grids was observed by a magnifying glass.
5B: the coating is not fallen off at all;
4B: the shedding area of the hundred grid coating is less than 5%;
3B: 5% -15% of the shedding area of the hundred grid coating;
2B: 15% -35% of the shedding area of the hundred grid coating;
1B: 35% -65% of the shedding area of the hundred grid coating;
0B: the shedding area of the hundred grid coating is more than 65 percent.
6. Pencil hardness:
The pencil hardness of the optical film was measured in accordance with JISK-5600 standard using an Elcometer 3086 pencil hardness tester. The measurement method comprises the following steps: using a mitsubishi pencil with a hardness of 3H to 5H, 5 lines were drawn under a load of 500g, and then the presence or absence of scratch of the optical film coating was observed, and judged according to the following criteria.
[ Criterion ]
Scratch 0-2 pieces of judgment "Pass"
3-5 Scratches are made to judge 'NG'
7. Steel wool friction resistance:
the surface of the antireflection film was rubbed back and forth at 60Hz by using a Shenzhen Zhen Jia machine ZJ-339-GSR steel wool tester under a load of 1000g and using Japanese Bonstar #0000 steel wool with a rubbing head of 2cm X2 cm, to confirm the occurrence of scratches on the surface of the coating.
[ Criterion ]
Scratch-free O is avoided within 300 times of friction;
No scratch is generated within 200 times of friction and a scratch delta is generated within 300 times;
scratch is found within 200 times of abrasion.
8. Average reflectance (%):
The optical film sample was cut into 8cm x 8cm pieces, a black tape was attached to the back of the coating, and the average reflectance at an angle of 6 degrees in the visible light region of 380 to 780nm was measured using a Shimadzu UV-2600i ultraviolet-visible spectrophotometer.
Table 10 properties of optical films
As can be seen from a combination of tables 9 and 10, the optical films provided in comparative examples 1 to 4 were poor in abrasion resistance. Wherein, in comparative example 1, the hard coat layer was not alkali-washed; comparative example 2, the cure rate of the hard coat layer reached 77.8%; comparative example 3, in which the silane coupling agent was not hydrolyzed; in comparative example 4, the hard coat layer was not alkali-washed, and the silane coupling agent was not added, and the abrasion resistance of the finally obtained optical film was not good.
In examples 1 to 12, and comparative examples 2 and 3 of the present application, the water contact angle before alkali washing of the hard coating layer was high, and the water contact angle after alkali washing was reduced, which can be shown that some unreacted acrylic double bonds were converted into hydroxyl groups, and the water contact angle of the hard coating layer was reduced.
In examples 1 to 12 of the present application, the hard coat layer was first incompletely cured, then the hard coat layer was alkali-washed, and the antireflection layer was prepared, and the antireflection coating liquid for forming the antireflection layer contained a silane coupling agent having a double bond at one end and-Si-OH at one end, so that the abrasion resistance of the optical film could be improved.
As can be seen from comparative examples 1 to 8 and example 9, the addition amount of the silane coupling agent after hydrolysis is 1.38 to 3.7%, and both scratch resistance and water boiling adhesion of the optical film can be improved.
As can be seen from comparative examples 1 to 8, and examples 10 to 12, when the hard coat layer is alkali-washed, the conditions of alkali washing are: the concentration is 8.5-10%, the temperature is 45-60 ℃ and the time is 70-120 s, so that the alkali washing effect of the hard coating is better.
The embodiments described above are some, but not all embodiments of the application. The detailed description of the embodiments of the application is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.

Claims (10)

1. A method for producing an optical film, comprising the steps of:
Preparing a hard coating: coating a hard coating liquid on one surface of a transparent base film, and performing incomplete UV curing on the hard coating liquid after drying to form a hard coating, wherein the curing rate of the hard coating is less than 60%;
Alkali treatment is carried out on the hard coating: soaking the hard coating in alkali liquor to convert part of unreacted acrylic double bonds in the hard coating into hydroxyl groups, and then taking out, washing and drying;
Preparing an antireflection layer: coating the anti-reflection coating liquid on the surface of the hard coating after alkali treatment, and then drying and UV curing to form an anti-reflection layer; the anti-reflection coating liquid contains a hydrolyzed silane coupling agent, wherein one end of the hydrolyzed silane coupling agent is a double bond, and the other end of the hydrolyzed silane coupling agent is-Si-OH.
2. The method of claim 1, wherein the hard coat layer has a cure rate of 30 to 60%.
3. The method according to claim 2, wherein in preparing the hard coat layer, the components of the hard coat liquid include UV-curable oligomer, reactive monomer, and initiator, and the amount of the initiator/(the amount of UV-curable oligomer+the amount of reactive monomer) ×100% = 3-6%;
The energy of the UV curing is 200-350 mj/cm 2.
4. A production method according to any one of claims 1 to 3, wherein the conditions of the alkali treatment include: soaking the hard coating in alkali liquor with the mass concentration of 8-12% and the temperature of 40-60 ℃ for 1-3 min; wherein the alkali liquor is sodium hydroxide and/or potassium hydroxide solution.
5. The method according to any one of claims 1 to 3, wherein the components of the antireflection coating liquid include an antireflection coating and the hydrolyzed silane coupling agent, and (the amount of the effective component of the hydrolyzed silane coupling agent/the amount of the effective component of the antireflection coating) ×100% = 0.5 to 5%.
6. The method according to claim 5, wherein the method for producing the hydrolyzed silane coupling agent comprises: and (3) reacting a silane coupling agent solution with a double bond at one end for 2 hours and more under the condition that the pH value is 4.0-5.0, so that the-Si-X is hydrolyzed into the-Si-OH, wherein the solvent in the solution comprises water and ethanol.
7. The preparation method according to claim 6, wherein the mass ratio of the double bond-containing silane coupling agent to water and ethanol is 1 (0.8-1.2): 15-25.
8. The method according to claim 6 or 7, wherein the silane coupling agent is at least one of 3-methacryloxypropyl trimethoxysilane, 3-methacryloxypropyl methyl dimethoxy silane, 3-methacryloxypropyl methyl diethoxy silane, 3-methacryloxypropyl triethoxy silane, and 3-acrylic propyl trimethoxysilane.
9. An optical film prepared by the preparation method of any one of claims 1 to 8.
10. The optical film according to claim 9, wherein the hard coat layer has a thickness of 3 to 5 μm and the antireflection layer has a thickness of 0.09 to 0.11 μm.
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