WO2011162191A1 - 粘着剤層、粘着フィルムおよび光学装置 - Google Patents
粘着剤層、粘着フィルムおよび光学装置 Download PDFInfo
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- WO2011162191A1 WO2011162191A1 PCT/JP2011/064001 JP2011064001W WO2011162191A1 WO 2011162191 A1 WO2011162191 A1 WO 2011162191A1 JP 2011064001 W JP2011064001 W JP 2011064001W WO 2011162191 A1 WO2011162191 A1 WO 2011162191A1
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- sensitive adhesive
- pressure
- adhesive layer
- film
- meth
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/50—Aqueous dispersion, e.g. containing polymers with a glass transition temperature (Tg) above 20°C
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2433/00—Presence of (meth)acrylic polymer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness
- Y10T428/24612—Composite web or sheet
Definitions
- the present invention relates to a pressure-sensitive adhesive layer, a pressure-sensitive adhesive film, and an optical device. Specifically, the present invention relates to an optical device and a pressure-sensitive adhesive layer and a pressure-sensitive adhesive film suitably used for the optical device.
- adhesive films have been widely used in various industrial fields, and are obtained by providing an adhesive layer on the surface of a substrate.
- a water-dispersed pressure-sensitive adhesive composition having a solid content of 47% by weight obtained by adding an acrylic thickener to an acrylic copolymer emulsion is applied onto a release film and then dried.
- a pressure-sensitive adhesive layer for example, see Patent Document 1 below.
- the pressure-sensitive adhesive layer may be required to have an excellent appearance, and the pressure-sensitive adhesive layer of Patent Document 1 may not be able to obtain such a good appearance.
- An object of the present invention is to provide a pressure-sensitive adhesive layer having an excellent appearance, a pressure-sensitive adhesive film including the pressure-sensitive adhesive layer, and an optical device.
- the pressure-sensitive adhesive layer of the present invention is a pressure-sensitive adhesive layer obtained by applying and drying a water-dispersed pressure-sensitive adhesive composition, and has a depth in the thickness direction of 0.2 to 20 ⁇ m on the surface of the pressure-sensitive adhesive layer.
- the number of recesses having a maximum length of 1 to 10 mm along the surface is 1 m 2 or 5 or less.
- the water-dispersed pressure-sensitive adhesive composition has a solid content concentration of 5 to 32% by weight and the pressure-sensitive adhesive layer has a thickness of 3 to 100 ⁇ m.
- the pressure-sensitive adhesive layer of the present invention contains a water-dispersed acrylic polymer and a thickener, and the viscosity of the water-dispersed pressure-sensitive adhesive composition at 30 ° C. and a shear rate of 1 sec ⁇ 1 is 0.1 to It is preferable that the pressure is 50 Pa ⁇ s.
- the thickener is prepared as a 1% by weight aqueous solution and further has a turbidity of 100 NTU or less when adjusted to pH 8.
- the pressure-sensitive adhesive layer of the present invention it is preferable that the pressure-sensitive adhesive layer having a thickness of 23 ⁇ m has a haze value of 1.0% or less.
- the pressure-sensitive adhesive film of the present invention comprises a base material and a pressure-sensitive adhesive layer laminated on the surface of the base material, and the adhesive layer is obtained by applying and drying a water-dispersed pressure-sensitive adhesive composition.
- the depth in the thickness direction is 0.2 to 20 ⁇ m, and the number of recesses having a maximum length of 1 to 10 mm along the surface is 5 or less per 1 m 2. It is characterized by that.
- the substrate is an optical film.
- the optical device of the present invention includes an optical film and a pressure-sensitive adhesive layer laminated on the surface of the optical film, and the adhesive layer is obtained by applying and drying a water-dispersed pressure-sensitive adhesive composition.
- the depth in the thickness direction is 0.2 to 20 ⁇ m, and the number of recesses having a maximum length of 1 to 10 mm along the surface is 5 or less per 1 m 2. It is characterized by that.
- the pressure-sensitive adhesive layer of the present invention has an excellent appearance, and the pressure-sensitive adhesive film of the present invention provided therewith is used for various industrial applications as a film having an excellent appearance.
- the optical device of the present invention including the above-described pressure-sensitive adhesive film of the present invention can ensure excellent optical characteristics.
- FIG. 1 is a process diagram for explaining a production method of an embodiment of the pressure-sensitive adhesive layer of the present invention, wherein (a) is a step of preparing a release film, and (b) is a water-dispersed pressure-sensitive adhesive composition. The step of forming a coating liquid layer made of a material on the surface of the release film, (c) shows a step of drying the coating liquid layer to form an adhesive layer.
- FIG. 2 is a process diagram for explaining the method for producing the pressure-sensitive adhesive layer of Example 1 when foreign matter is present between the back surface of the release film and the surface of the support member.
- (B) is a step of separating the release film from the support member, and (c) is a pressure-sensitive adhesive by drying the coating solution layer.
- FIG. 3 is a process diagram for explaining a method for producing a pressure-sensitive adhesive layer of Comparative Example 1 in the case where foreign matter is present between the back surface of the release film and the surface of the support member.
- (B) is a step of separating the release film from the support member, and (c) is a pressure-sensitive adhesive by drying the coating solution layer.
- FIG. 4 shows a cross-sectional view of an adhesive optical film which is an embodiment of the adhesive film of the present invention.
- FIG. 5 is a process diagram for explaining a method for producing the pressure-sensitive adhesive layer shown in FIG.
- the pressure-sensitive adhesive layer of the present invention can be obtained by applying a water-dispersed pressure-sensitive adhesive composition to the surface of a member to be coated and drying it.
- the water-dispersed pressure-sensitive adhesive composition contains, for example, a water-dispersed acrylic polymer and a thickener.
- the water-dispersed acrylic polymer contains, for example, (meth) acrylic acid alkyl ester having an alkyl group having 4 to 18 carbon atoms and a carboxyl group-containing vinyl monomer as essential components, and can be copolymerized with the above-described essential components. It can be obtained by polymerizing a monomer component optionally containing a copolymerizable vinyl monomer.
- the (meth) acrylic acid alkyl ester having an alkyl group having 4 to 18 carbon atoms is preferably a (meth) acrylic acid in which the alkyl portion is a linear or branched alkyl group having 4 to 18 carbon atoms.
- Alkyl esters that is, methacrylic acid alkyl esters and / or acrylic acid alkyl esters, for example, butyl (meth) acrylate, isobutyl (meth) acrylate, sec-butyl (meth) acrylate, (meth) acrylic acid t-butyl, pentyl (meth) acrylate, neopentyl (meth) acrylate, isopentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, (meth) 2-ethylhexyl acrylate, isooctyl (meth) acrylate, (meth) a Nonyl rillate, isononyl (meth) acrylate, decyl (meth) acrylate, isodecyl (meth) acrylate, undecyl (me
- the proportion of the (meth) acrylic acid alkyl ester is, for example, 60 to 99 parts by weight, preferably 70 to 99 parts by weight, more preferably 80 to 99 parts by weight, based on 100 parts by weight of the total amount of monomer components. is there.
- the carboxyl group-containing vinyl monomer is a vinyl monomer having a carboxyl group, for example, an unsaturated monocarboxylic acid such as (meth) acrylic acid, crotonic acid, cinnamic acid, for example, fumaric acid, maleic acid, itaconic acid, etc.
- unsaturated monocarboxylic acids such as fumaric anhydride, maleic anhydride, itaconic anhydride and the like, and unsaturated dicarboxylic anhydrides such as itaconic acid monomethyl, itaconic acid monobutyl, 2-acryloyloxyethylphthalic acid, etc.
- Acid monoesters for example, unsaturated tricarboxylic acid monoesters such as 2-methacryloyloxyethyl trimellitic acid, 2-methacryloyloxyethyl pyromellitic acid, for example, carboxyalkyl such as carboxyethyl acrylate, carboxypentyl acrylate, etc. Acrylate and the like.
- carboxyl group-containing vinyl monomers can be used alone or in combination.
- unsaturated monocarboxylic acid is mentioned.
- the mixing ratio of the carboxyl group-containing vinyl monomer is, for example, 0.5 to 15 parts by weight, preferably 0.5 to 10 parts by weight, and more preferably 1 to 10 parts by weight with respect to 100 parts by weight of the total amount of monomer components. Part.
- Examples of the copolymerizable vinyl monomer include functional group-containing vinyl monomers other than carboxyl group-containing vinyl monomers, and examples include mono [monoalkylene oxide (meth) acrylate] phosphate esters and mono [polyalkylene oxides].
- (Meth) acrylate] Phosphoric acid group-containing vinyl monomers such as phosphate esters, for example, vinyl esters such as vinyl acetate and vinyl propionate, for example, glycidyl (meth) acrylate, epoxy such as methyl glycidyl (meth) acrylate
- Group-containing monomers such as hydroxyl group-containing vinyl monomers such as 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxybutyl acrylate, such as (meth) acrylamide, N, N-dimethyl (meth) a Rilamide, N, N-diethyl (meth) acrylamide, N-isopropyl (meth) acrylamide, N-butyl (meth) acrylamide, N-methoxymethyl (meth) acrylamide, N-methylol (meth) acrylamide, N-methylolpropane
- Amide group-containing vinyl monomers such as (meth) acrylamide and
- examples of the copolymerizable vinyl monomer include alkoxysilyl group-containing vinyl monomers.
- alkoxysilyl group-containing vinyl monomer examples include silane (meth) acrylate monomers and silane vinyl monomers.
- silane (meth) acrylate monomer examples include (meth) acryloyloxymethyl-trimethoxysilane, (meth) acryloyloxymethyl-triethoxysilane, 2- (meth) acryloyloxyethyl-trimethoxysilane, 2- ( (Meth) acryloyloxyethyl-triethoxysilane, 3- (meth) acryloyloxypropyl-trimethoxysilane, 3- (meth) acryloyloxypropyl-triethoxysilane, 3- (meth) acryloyloxypropyl-tripropoxysilane, 3 -(Meth) acryloyloxyalkyl-trialkoxysilanes such as (meth) acryloyloxypropyl-triisopropoxysilane, 3- (meth) acryloyloxypropyl-tributoxysilane, eg (meth) Acryloyl
- silane-based vinyl monomer examples include vinyltrialkoxysilanes such as vinyltrimethoxysilane, vinyltriethoxysilane, vinyltripropoxysilane, vinyltriisopropoxysilane, and vinyltributoxysilane, as well as vinylalkyldisilanes corresponding to these.
- Alkoxysilanes and vinyldialkylalkoxysilanes such as vinylmethyltrimethoxysilane, vinylmethyltriethoxysilane, ⁇ -vinylethyltrimethoxysilane, ⁇ -vinylethyltriethoxysilane, ⁇ -vinylpropyltrimethoxysilane, ⁇ -vinyl Vinyl alkyl trials such as propyltriethoxysilane, ⁇ -vinylpropyltripropoxysilane, ⁇ -vinylpropyltriisopropoxysilane, ⁇ -vinylpropyltributoxysilane Other Kishishiran, these corresponding (vinyl) alkyl dialkoxy silane, or the like (vinyl alkyl) dialkyl (mono) alkoxysilanes.
- examples of copolymerizable vinyl monomers include olefinic monomers such as ethylene, propylene, isoprene, butadiene, and isobutylene, such as (meth) acrylic.
- (Meth) acrylic acid alkyl esters having a linear or branched alkyl group having 1 to 3 carbon atoms such as methyl acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, and isopropyl (meth) acrylate
- (meth) acrylic acid cycloaliphatic hydrocarbon esters such as (meth) acrylic acid cyclohexyl, (meth) acrylic acid bornyl, (meth) acrylic acid isobornyl, for example, (meth) acrylic acid phenyl (meth)
- Acrylic acid aryl esters such as styrene Contains nitrogen atoms such as styrene monomers such as (meth) acryloylmorpholine, aminoethyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, and t-butylaminoethyl (meth) acrylate Vinyl mono
- examples of the copolymerizable vinyl monomer include polyfunctional monomers.
- polyfunctional monomer examples include (mono or poly) ethylene glycol such as ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, and tetraethylene glycol di (meth) acrylate.
- alkylene glycol di (meth) acrylate such as di (meth) acrylate and propylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate and 1,6-hexanediol di (meth) Acrylate, pentaerythritol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tri (meth) acrylate, dipentaerythritol hexa (meth) acrylate
- Examples include relate and divinylbenzene.
- the polyfunctional monomer include epoxy acrylate, polyester acrylate, and urethane acrylate.
- copolymerizable vinyl monomers can be used alone or in combination of two or more.
- phosphoric acid group-containing vinyl monomers and alkoxysilyl group-containing vinyl monomers are preferable, and mono [polyalkylene oxide (meth) acrylate] phosphoric acid esters and silanes ( And (meth) acrylate monomers.
- the blending ratio of the copolymerizable vinyl monomer is, for example, 39 parts by weight or less, preferably 19 parts by weight or less, and more preferably 18 parts by weight or less with respect to 100 parts by weight of the total amount of monomer components.
- the blending ratio of the phosphate group-containing vinyl monomer is, for example, 0.5 to 20 parts by weight, preferably 0. 5 to 10 parts by weight, more preferably 1 to 5 parts by weight.
- the blending ratio is, for example, 0.001 to 1 part by weight, preferably 0.005 to 0.1 part by weight with respect to 100 parts by weight of the total amount of monomer components. Part.
- a monomer component is mix
- emulsion polymerization for example, a polymerization initiator, an emulsifier, and the like are blended and polymerized in water together with the above-described monomer components. More specifically, for example, known emulsion polymerization methods such as a batch charging method (batch polymerization method), a monomer dropping method, and a monomer emulsion dropping method can be employed. In the monomer dropping method, continuous dropping or divided dropping is selected. Reaction conditions and the like are selected as appropriate, but the polymerization temperature is, for example, 20 to 100 ° C.
- the dissolved oxygen concentration in the reaction solution containing the monomer component can be reduced by nitrogen substitution before, while or after the polymerization initiator is mixed with the monomer component.
- the polymerization initiator is not particularly limited, and a polymerization initiator usually used for emulsion polymerization is used.
- a polymerization initiator usually used for emulsion polymerization is used.
- 2,2′-azobisisobutyronitrile (AIBN) 2,2′-azobis (2-methylpropionamidine) disulfate
- 2,2′-azobis (2-methylpropionamidine) dihydrochloride 2,2′-azobis (2-amidinopropane) dihydrochloride
- 2,2′-azobis [N- (2-carboxyethyl) -2-methylpropionamidine] hydrate 2,2′-azobis ( N, N′-dimethyleneisobutylamidine)
- 2,2′-azobis [2- (2-imidazolin-2-yl) propane] dihydrochloride such as potassium persulfate (KPS), Persulfate initiators such as ammonium persulfate (APS), for example, peroxide
- Substituted ethane-based initiators such as phenyl-substituted ethanes, for example, carbonyl-based initiators such as aromatic carbonyl compounds, such as redox combinations of persulfates and sodium bisulfite, peroxides and sodium ascorbate, etc. And system initiators.
- polymerization initiators can be used alone or in combination of two or more. Of these polymerization initiators, preferably, a persulfate-based initiator is used.
- the blending ratio of the polymerization initiator is appropriately selected and is, for example, 0.04 to 1 part by weight with respect to 100 parts by weight of the monomer component.
- the emulsifier is not particularly limited, and a known emulsifier usually used for emulsion polymerization is used.
- a known emulsifier usually used for emulsion polymerization is used.
- sodium lauryl sulfate, ammonium lauryl sulfate, sodium dodecylbenzene sulfonate sodium polyoxyethylene lauryl sulfate, sodium polyoxyethylene alkyl ether sulfate, ammonium polyoxyethylene alkyl phenyl ether sulfate, sodium polyoxyethylene alkyl phenyl ether sulfate, polyoxyethylene Anionic emulsifiers such as sodium alkylsulfosuccinate, for example, nonionic emulsifiers such as polyoxyethylene alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene fatty acid ester, and polyoxyethylene polyoxypropylene block polymer.
- an emulsifier for example, a radical polymerizable emulsifier in which a radical polymerizable functional group (reactive group) such as a propenyl group or an allyl ether group is introduced into the anionic emulsifier or nonionic emulsifier described above (for example, Aqualon HS- 10 (reactive emulsifiers such as Daiichi Kogyo Seiyaku Co., Ltd.).
- a radical polymerizable emulsifier in which a radical polymerizable functional group (reactive group) such as a propenyl group or an allyl ether group is introduced into the anionic emulsifier or nonionic emulsifier described above (for example, Aqualon HS- 10 (reactive emulsifiers such as Daiichi Kogyo Seiyaku Co., Ltd.).
- emulsifiers can be used alone or in combination of two or more.
- a reactive emulsifier is used.
- the blending ratio of the emulsifier is, for example, 0.2 to 10 parts by weight, preferably 0.5 to 5 parts by weight with respect to 100 parts by weight of the monomer component.
- the water-dispersed acrylic polymer obtained by such emulsion polymerization is prepared as an emulsion (water-dispersed), that is, an aqueous dispersion of an acrylic polymer.
- the water-dispersed acrylic polymer is obtained by, for example, polymerizing the above-described monomer component by a method other than emulsion polymerization, for example, solution polymerization or bulk polymerization, and after removing the solvent or crushing the bulk as necessary. It can also be prepared by dispersing in water with an emulsifier.
- the solid content concentration in the water-dispersed acrylic polymer is, for example, 10 to 90% by weight, and preferably 20 to 80% by weight.
- the thickener is blended in the water-dispersed pressure-sensitive adhesive composition in order to set the viscosity of the water-dispersed pressure-sensitive adhesive composition in a desired range (described later), for example, polyacrylic acid-based thickener, urethane-based A thickener, a cellulose thickener, a natural polymer thickener, etc. are mentioned.
- polyacrylic acid thickener examples include polyacrylic acid, polyacrylic acid-poly (meth) acrylic acid alkyl ester copolymer (acrylic acid copolymer), and the like.
- group thickener the neutralized material by which the above-mentioned polyacrylic acid was neutralized previously, ie, polyacrylate, etc. are mentioned.
- the polyacrylate examples include sodium polyacrylate and potassium polyacrylate.
- the polyacrylic acid thickener examples include hydrophobic group-modified polyacrylic acid in which a part of the carboxyl group is modified with a hydrophobic group such as a styrene group or an alkyl group.
- the acid value of the polyacrylic acid thickener is, for example, 30 to 300 mg / KOH, and preferably 80 to 280 mg / KOH.
- the urethane-based thickener is, for example, a urethane compound having a urethane bond and a polyether chain in the molecule, and can exhibit a thickening action when the urethane bonds are associated with each other in water.
- cellulose-based thickener examples include methyl cellulose, ethyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and carboxymethyl cellulose.
- Examples of natural polymer thickeners include xanthan gum, gellan gum, guar gum, sodium alginate, carrageenan, and pectin.
- thickener examples include polyacrylamide, polyethylene oxide, polyvinyl alcohol and the like.
- thickeners can be used alone or in combination of two or more.
- the thickener is preferably a polyacrylic acid thickener or a urethane thickener, from the viewpoint of improving the appearance of the pressure-sensitive adhesive layer.
- polyacrylic acid thickeners for example, primal ASE-60, primal TT-615, primal ASE-75, primal ASE-95, Primal ASE-108, Primal RM-5 (above Rohm and Haas), Zogen 100, Zogen 150, Zogen 200, Zogen 250, Zogen 350 (above RHEOX), SN thickener A-815, SN thickener A -818, SN thickener A-850 (manufactured by San Nopco), RHEOVIS CR (manufactured by Yushi Co., Ltd.), Aron B-300K, Aron B-500 (acrylic acid copolymer), Aron A-7070 (above Toago) Synthetic Co., Ltd.), Chikuzol K-150B (manufactured by Kyoeisha Oil Chemical Co., Ltd.) Reset WR-503, ACRYSET WR-650 (all manufactured by Nippon Sho
- Urethane thickeners include, for example, Adecanol UH-462, Adecanol UH-752, Adecanol UH-140S, Adecanol UH-420, Adecanol UH-438, Adecanol UH-472, Adecanol UH-450, Adecanol UH- 540, Adecanol UH-550, Adecanol UH-541VF, Adecanol UH-526, Adecanol UH-530 (Adeka) SN thickener A-804, SN thickener A-807, SN thickener A-812, SN thickener A-814 Company, Ltd.) and the like.
- the above thickener is prepared in the form of, for example, a powder (particle) type, an aqueous solution type, an emulsion type, and the like.
- the thickener is prepared as a 1 wt% aqueous solution, and the turbidity when adjusted to pH 8 is, for example, 100 NTU or less, preferably 50 NTU or less, more preferably 20 NTU or less. 1 NTU or more.
- an alkaline aqueous solution such as an aqueous ammonia solution having a concentration of 5 to 15 wt% is added to the 1 wt% aqueous solution of the thickener.
- the addition amount of the alkaline aqueous solution is adjusted so that the reduction rate of the concentration of the thickener is within 1%, for example.
- the turbidity is measured with a turbidimeter, and NTU is a unit of turbidity (Nephelometric Turbidity Unit).
- the turbidity of the 1% by weight aqueous solution of the thickener after pH adjustment exceeds the above range, the insoluble matter (particles) of the thickener remains, and the thickener is compared as it is in the adhesive layer. May be present as large particles, and the transparency of the pressure-sensitive adhesive layer may be reduced, causing white turbidity.
- the blending ratio of the thickener (solid content thereof) is, for example, 0.01 to 20 parts by weight, preferably 0.1 to 10 parts by weight with respect to 100 parts by weight of the solid content of the water-dispersed acrylic polymer. More preferably, it is 0.5 to 5 parts by weight.
- the blending ratio of the thickener (solid content thereof) is other than the solid content of the water-dispersed pressure-sensitive adhesive composition, that is, for example 0.01 to 20 parts by weight, preferably 100 parts by weight of water, It can also be set to 0.1 to 10 parts by weight, more preferably 0.5 to 5 parts by weight.
- the viscosity of the water-dispersed pressure-sensitive adhesive composition can be set to a desired range (described later).
- a water-dispersed acrylic polymer and a thickener are blended in the above blending ratio. Specifically, a water-dispersed acrylic polymer and a thickener are blended and stirred uniformly to prepare a water-dispersed mixed liquid.
- the solid content concentration of the water-dispersed pressure-sensitive adhesive composition is, for example, 5 to 32% by weight, preferably 7 to 29% by weight, more preferably Adjust to 10-25 wt%.
- the handling property during coating can be improved, and the thickness T1 (described later) of the coating liquid layer 2 can be set within a specific range.
- the number of recesses 5 may exceed the desired range.
- the pH of the water-dispersed pressure-sensitive adhesive composition whose solid content is adjusted is adjusted to, for example, 7 to 10, preferably 7 to 9.
- the pH of the water-dispersed pressure-sensitive adhesive composition is adjusted, for example, by adding an aqueous alkaline solution such as an aqueous ammonia solution having a concentration of 5 to 15% by weight to the water-dispersed pressure-sensitive adhesive composition having a solid content adjusted. .
- the addition amount of the aqueous alkali solution is adjusted so that the reduction rate of the solid content concentration in the water-dispersed pressure-sensitive adhesive composition is, for example, within 1%.
- the pH of the water-dispersed pressure-sensitive adhesive composition whose solid content concentration has been adjusted usually exceeds 10 when the thickener is a polyacrylic acid-based thickener, the water-dispersed type By adjusting the pH of the pressure-sensitive adhesive composition within the above-described range and neutralizing the carboxyl group, a thickening effect is exhibited.
- the viscosity of the water-dispersed pressure-sensitive adhesive composition thus prepared at 30 ° C. and a shear rate of 1 sec ⁇ 1 is, for example, 0.1 to 50 Pa ⁇ s, preferably 0.2 to 20 Pa ⁇ s.
- the viscosity of the water-dispersed pressure-sensitive adhesive composition at 30 ° C. and a shear rate of 1 sec ⁇ 1 is measured with a cone / plate viscometer (rheometer).
- the viscosity of the water-dispersed pressure-sensitive adhesive composition When the viscosity of the water-dispersed pressure-sensitive adhesive composition is less than the above-mentioned range, the water-dispersed pressure-sensitive adhesive composition will repel on the coated member (described later) during application, making it difficult to apply. There is. On the other hand, when the viscosity of the water-dispersed pressure-sensitive adhesive composition exceeds the above range, the number of recesses 5 may exceed the desired range.
- FIG. 1 is a process diagram for explaining a production method of an embodiment of the pressure-sensitive adhesive layer of the present invention
- FIGS. 2 and 3 are cases where foreign matter exists between the back surface of the release film and the surface of the support member. It is process drawing explaining the manufacturing method of an adhesive layer.
- a member to be coated for example, a film, specifically, a release film 1 is prepared.
- the release film 1 is made of, for example, a soft material.
- synthetic resin films such as polyethylene, polypropylene, and polyethylene terephthalate (PET), for example, metal foil (such as cloth, nonwoven fabric, net, foam film)
- metal foil such as cloth, nonwoven fabric, net, foam film
- an aluminum foil or a laminated film in which a plurality of them is used can be used.
- the surface of the release film 1 is subjected to treatment (peeling treatment) such as silicone treatment, long-chain alkyl treatment, and fluorine treatment as necessary in order to enhance the peelability.
- the thickness of the release film 1 is not particularly limited, and is, for example, 1 to 1000 ⁇ m, preferably 10 to 100 ⁇ m.
- a water-dispersed pressure-sensitive adhesive composition is applied to the surface of the release film 1 to form a coating liquid layer 2.
- the water-dispersed pressure-sensitive adhesive composition is applied to the surface of the release film 1 by a known application method such as kiss coating, gravure coating, bar coating, spray coating, knife coating, wire coating, or comma coating.
- the water-dispersed pressure-sensitive adhesive composition When the water-dispersed pressure-sensitive adhesive composition is applied to the surface of the release film 1, for example, as shown in FIGS. 2 (a) and 3 (a), the back surface of the release film 1 is attached to the support member 7. The release film 1 is supported in contact with the surface.
- examples of the support member 7 include a coating roll.
- the coating roll is disposed in the middle of the release film 1 in the longitudinal direction, and the water-dispersed pressure-sensitive adhesive composition is applied to the surface of the release film 1 while the release film 1 passes through the coating roll.
- the release film 1 to which the water-dispersed pressure-sensitive adhesive composition has been applied leaves the coating roll after passing through the coating roll.
- examples of the support member 7 include a flat support plate.
- a support plate is disposed on the entire back surface of the release film 1, and after the formation of the coating liquid layer, the release film 1 is pulled away from the support plate 7.
- the above-described support member 7 is made of, for example, a hard material harder than the soft material forming the release film 1, and specifically, a hard material such as a metal such as iron or stainless steel.
- the thickness T1 of the coating liquid layer 2 is, for example, 5 to 2000 ⁇ m, preferably 10 to 1000 ⁇ m. If the thickness T1 of the coating liquid layer 2 is in the above-described range, the thickness T2 (described later) of the pressure-sensitive adhesive layer 6 can be set to a desired range, and the number of recesses 5 (described later, see FIG. 3) is set to a desired number or less. be able to.
- the coating liquid layer 2 is dried as shown in FIG.
- the drying temperature is, for example, 90 to 150 ° C., for example, 100 to 140 ° C., and the drying temperature is, for example, 0.5 to 30 minutes, preferably 1 to 10 minutes.
- the pressure-sensitive adhesive layer 6 can be obtained. That is, the moisture in the coating liquid layer 2 is distilled off by the above-described drying, and the pressure-sensitive adhesive layer 6 composed of the solid content of the water-dispersed pressure-sensitive adhesive composition (mainly a mixture of an acrylic polymer and a thickener) is formed.
- the water-dispersed pressure-sensitive adhesive composition mainly a mixture of an acrylic polymer and a thickener
- the thickness T2 of the pressure-sensitive adhesive layer 6 thus obtained is, for example, 10 to 60%, preferably, for example, 20 to 50% with respect to the thickness T1 of the coating liquid layer 2. Specifically, 3 to 100 ⁇ m, preferably 20 to 40 ⁇ m.
- a base material specifically, an optical film 11 (see FIG. 4) and the like
- an adherend specifically, a glass substrate of an optical device, etc.
- the haze value of the pressure-sensitive adhesive layer 6 having a thickness of 23 ⁇ m is, for example, 1.0% or less, preferably 0.9% or less, and usually 0.1% or more.
- the haze value of the pressure-sensitive adhesive layer 6 is measured with a haze meter in accordance with JIS K7136.
- the haze value of the pressure-sensitive adhesive layer 6 exceeds the above-described range, the transparency of the pressure-sensitive adhesive layer 6 may be lowered, and a good appearance of the pressure-sensitive adhesive layer 6 may not be ensured.
- the pressure-sensitive adhesive layer 6 has 5 or less, preferably 1 or less, the number of recesses 5 to be described below per 1 m 2 on its surface.
- the recess 5 is a portion (defect portion) that is recessed from the front surface to the back surface of the pressure-sensitive adhesive layer 6 and has a depth D in the thickness direction of 0.2 to 20 ⁇ m.
- the maximum length along the surface (for example, in the case of a circular plan view, the inner diameter at the upper end) L2 is defined as a defective portion having a size of 1 to 10 mm.
- the foreign material 8 has a maximum length of, for example, 1 to 1000 ⁇ m, and further 10 to 100 ⁇ m.
- the release film 1 curves (projects) the back surface of the part (projection part 13) which opposes the foreign material 8 in the thickness direction toward the front side (upper side).
- the surface of the protruding portion 13 is also formed so as to bend (project) toward the front side (upper side).
- the release film 1 is formed so that thickness may become fixed in the protrusion part 13 and the surrounding part.
- the coating liquid layer 2 is composed of a water-dispersed pressure-sensitive adhesive composition prepared as an emulsion, the surface of the coating liquid layer 2 is formed flat, while the back surface of the coating liquid layer 2, that is, On the surface facing the release film 1, a back side recess 9 corresponding to the protruding portion 13 on the surface of the release film 1 is formed.
- the size and number of the back side recesses 9 correspond to the size and number of the protruding portions 13 on the surface of the release film 1 described above.
- the above-described back-side recess 9 is formed flat along with its periphery and disappears.
- the above-described back-side recess 9 (FIG. ) And the front side recess 4 corresponding to FIG. 3A) is formed.
- the front side recesses 4 are recessed from the surface of the coating liquid layer 2 toward the back side, and the size and number thereof substantially correspond to the size and number of the protruding portions 13 described above.
- the pressure-sensitive adhesive layer 6 is formed by drying the coating liquid layer 2.
- concentration is FIG.2 (b).
- the coating liquid layer 2 is formed to be significantly thinner. That is, since the ratio (T2 / T1) of the thickness T2 of the pressure-sensitive adhesive layer 6 to the thickness T1 of the coating liquid layer 2 is remarkably small, it is not easily affected by the front-side concave portion 4, and therefore the concave portion 5 in FIG. Is smaller than the lower limit of the size defined above (maximum depth D) (shallow).
- the thickness T2 ′ of the pressure-sensitive adhesive layer 6 obtained from the water-dispersed pressure-sensitive adhesive composition having a solid content concentration higher than the solid content concentration (for example, a concentration exceeding 32% by weight) is the thickness of the coating liquid layer 2.
- the ratio (T2 ′ / T1 ′) of the thickness T2 ′ of the pressure-sensitive adhesive layer 6 to the thickness T1 ′ of the coating liquid layer 2 is relatively large, and the application of the thickness T2 of the pressure-sensitive adhesive layer 6 in FIG. Since it is larger than the ratio (T2 / T1) to the thickness T1 of the liquid layer 2, it is easily affected by the front side recess 4. Therefore, the recess 5 in FIG. 3 (c) is formed at least deeper than the recess 5 in FIG. 2 (c), specifically, within the size defined above (maximum depth D).
- the solid content concentration of the water-dispersed pressure-sensitive adhesive composition is set to a specific concentration, the number of the recessed portions 5 after drying is small. Since 5 is less than the desired number, it has an excellent appearance. Therefore, it is used for various industrial uses, preferably optical uses that require excellent appearance.
- FIG. 4 shows a cross-sectional view of an adhesive optical film which is an embodiment of the adhesive film of the present invention.
- this adhesive optical film 10 includes an optical film 11 as a substrate, an undercoat layer 12 laminated on the surface of the optical film 11, and an adhesive layer 6 laminated on the surface of the undercoat layer 12. I have.
- the optical film 11 is a film having optical characteristics, and is used as an optical layer in an image display device, for example, used in an image display device described in detail later.
- Examples of the optical film 11 include a polarizing film, a retardation film, a brightness enhancement film, a viewing angle widening film (viewing compensation film), a surface treatment film, and the like.
- polarizing film for example, a film in which a transparent protective film is provided on one side or both sides of a polarizer is used.
- the polarizer is not particularly limited, and examples thereof include hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, ethylene / vinyl acetate copolymer partially saponified films, iodine and dichroism. Examples thereof include uniaxially stretched films dyed with dichroic substances such as dyes, and polyene-based oriented films such as polyvinyl alcohol dehydrated products and polyvinyl chloride dehydrochlorinated products. Preferably, a polarizer obtained by uniaxially stretching a polyvinyl alcohol film with iodine is used.
- the transparent protective film examples include polyester polymer films such as polyethylene terephthalate and polyethylene naphthalate, cellulose polymer films such as diacetylcellulose and triacetylcellulose, acrylic polymer films such as polymethylmethacrylate, polystyrene, acrylonitrile and styrene.
- polyester polymer films such as polyethylene terephthalate and polyethylene naphthalate
- cellulose polymer films such as diacetylcellulose and triacetylcellulose
- acrylic polymer films such as polymethylmethacrylate, polystyrene, acrylonitrile and styrene.
- styrene polymer film such as a polymer (AS resin), a polycarbonate polymer film, and the like.
- the transparent protective film can also be formed as a cured layer of thermosetting or ultraviolet curable resin such as acrylic, urethane, acrylurethane, epoxy, and silicone.
- the transparent protective film is preferably a cellulose polymer.
- the thickness of the transparent protective film is not particularly limited, and is, for example, 500 ⁇ m or less, preferably 1 to 300 ⁇ m, and more preferably 5 to 200 ⁇ m.
- an isocyanate-based adhesive for example, an isocyanate-based adhesive, a polyvinyl alcohol-based adhesive, a gelatin-based adhesive, a vinyl-based adhesive, a latex-based adhesive, a water-based polyester adhesive, or the like is used. Glue.
- the retardation film examples include a wavelength plate such as a ⁇ / 2 wavelength plate or a ⁇ / 4 wavelength plate. Specifically, a birefringent film formed by uniaxially or biaxially stretching a polymer material. , A liquid crystal polymer alignment film, and a liquid crystal polymer alignment layer supported by a film.
- the thickness of the retardation film is not particularly limited and is, for example, 20 to 150 ⁇ m.
- polymer material examples include polyvinyl alcohol, polyvinyl butyral, polymethyl vinyl ether, polyhydroxyethyl acrylate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, polycarbonate, polyarylate, polysulfone, polyethylene terephthalate, polyethylene naphthalate, polyether sulfone, Polyphenylene sulfide, polyphenylene oxide, polyallylsulfone, polyvinyl alcohol, polyamide, polyimide, polyolefin, polyvinyl chloride, cellulose polymer, or binary, ternary copolymers, graft copolymers, blends Such as things. These polymer materials become an oriented product (stretched film) by stretching or the like.
- liquid crystalline polymer examples include various main chain types and side chain types in which a conjugated linear atomic group (mesogen) imparting liquid crystal orientation is introduced into the main chain or side chain of the polymer. It is done.
- main chain type liquid crystalline polymer for example, a structure in which a mesogenic group is bonded at a spacer portion imparting flexibility, specifically, a nematic orientation polyester-based liquid crystalline polymer, a discotic polymer or a cholesteric polymer. Etc.
- the side chain type liquid crystalline polymer for example, polysiloxane, polyacrylate, polymethacrylate or polymalonate is used as the main chain skeleton, and the side chain is substituted by a nematic orientation-imparting para-substitution through a spacer portion composed of a conjugated atomic group.
- examples thereof include those having a mesogenic part composed of a cyclic compound unit.
- These liquid crystalline polymers are prepared by, for example, applying a solution of a liquid crystalline polymer on an alignment-treated surface such as a surface of a thin film such as polyimide or polyvinyl alcohol formed on a glass plate, or an oblique deposition of silicon oxide. It is obtained by developing and heat treatment.
- the retardation film may be, for example, a film for the purpose of expanding coloring or viewing angle due to birefringence of various wavelength films or liquid crystal layers, or may have a retardation depending on the purpose of use. What laminated
- brightness enhancement films are those that transmit linearly polarized light with a predetermined polarization axis and reflect other light, such as dielectric multilayer thin films and multilayer laminates of thin film films with different refractive index anisotropies. , Cholesteric liquid crystal polymer alignment films and those whose alignment liquid crystal layer is supported on a film substrate, such as those that reflect either left-handed or right-handed circularly polarized light and transmit other light, etc. Is mentioned.
- the thickness of the brightness enhancement film is, for example, 10 to 200 ⁇ m.
- the viewing angle widening film is a film that widens the viewing angle so that the image can be seen relatively clearly even when the screen of the liquid crystal display is viewed from a slightly oblique direction rather than perpendicular to the screen.
- Examples thereof include an alignment film such as a film and a liquid crystal polymer, and a support in which an alignment layer such as a liquid crystal polymer is supported on a transparent substrate.
- Retardation films used as viewing angle widening films include birefringent polymer films stretched biaxially in the plane direction and thickness direction refractions stretched uniaxially in the plane direction and stretched in the thickness direction.
- a birefringent film such as a polymer having birefringence with a controlled rate or a tilted orientation film is used.
- the thickness of the viewing angle widening film is, for example, 10 to 200 ⁇ m.
- a hard coat film for imparting scratch resistance to the surface of the image display device for example, an antiglare treatment film for preventing reflection on the image display device, an antireflective film, etc.
- a film for example, a reflection reducing film such as a low reflective film for reducing reflection on an image display device.
- examples of the optical film include a reflecting plate and a semi-transmissive plate.
- Each optical film described above can be used in one layer or two or more layers.
- the optical film 11 is prepared, and then the undercoat layer 12 is provided on the surface of the optical film 11.
- the undercoat layer 12 contains, for example, an oxazoline group-containing polymer and / or a water-soluble or water-dispersible conductive material.
- the oxazoline group-containing polymer includes, for example, a main chain composed of an acrylic skeleton or a styrene skeleton, and has an oxazoline group in the side chain of the main chain, and preferably includes a main chain composed of an acrylic skeleton. And an oxazoline group-containing acrylic polymer having an oxazoline group in the side chain of the main chain.
- oxazoline group examples include 2-oxazoline group, 3-oxazoline group, 4-oxazoline group, and preferably 2-oxazoline group.
- the 2-oxazoline group is generally represented by the following general formula (1).
- R1, R2, R3 and R4 each independently represents a hydrogen atom, a halogen atom, an alkyl group, an aralkyl group, a phenyl group or a substituted phenyl group.
- the oxazoline group-containing polymer has an oxazoline value of, for example, 1500 g solid / eq. Hereinafter, preferably, 1200 g solid / eq. It is as follows.
- oxazoline group-containing polymer As the oxazoline group-containing polymer, a commercially available product is used. Specifically, Epocros WS-500 (aqueous solution type, solid content 40%, main chain: acrylic, pH 7 to 9, oxazoline value 220 g solid / eq., Nippon Shokubai) Oxazoline group-containing acrylic polymers such as Epocross WS-700 (aqueous solution type, solid content 25%, main chain: acrylic, pH 7-9, oxazoline number 220 g solid / eq., Manufactured by Nippon Shokubai Co., Ltd.) Epocross K-1000 series (emulsion type, solid content 40%, main chain: styrene / acrylic, oxazoline value 1100 g solid / eq., PH 7-9, manufactured by Nippon Shokubai Co., Ltd.), Epocross K-2000 series (emulsion type, Solid content 40%, main chain: styrene
- oxazoline group-containing polymers can be used alone or in combination of two or more.
- water-soluble or water-dispersible conductive materials include conductive polymers and organometallic compounds.
- a conductive polymer is used.
- Examples of the conductive polymer include polyaniline, polythiophene, polypyrrole, and polyquinoxaline. Of these, polyaniline or polythiophene is preferable from the viewpoint of coatability.
- Polyaniline has a weight average molecular weight in terms of polystyrene (PS) measured by GPC measurement of, for example, 500,000 or less, and preferably 300,000 or less.
- Polythiophene has a polystyrene-reduced weight average molecular weight of, for example, 400000 or less, preferably 300000 or less as measured by GPC.
- water-soluble or water-dispersible conductive polymer a commercially available product is used.
- the water-soluble conductive polymer include polyaniline sulfonic acid (Mitsubishi Rayon Co., Ltd.).
- examples thereof include polythiophene-based conductive polymers (trade name “Denatron”: manufactured by Nagase ChemteX Corporation, product name “Orgacon LBS”: manufactured by Agfa Materials Co., Ltd.), and the like.
- These conductive materials can be used alone or in combination of two or more.
- Each of the above components (oxazoline group-containing polymer and / or conductive material) is dissolved or dispersed in a solvent and prepared as a solution or dispersion of each component.
- each component is prepared as an aqueous solution or aqueous dispersion (hereinafter, simply referred to as “coating liquid”) in which each component is dissolved or dispersed in water. ing.
- the coating solution may further contain alcohols as an aqueous solvent.
- alcohols include methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, tert-butanol, n-amyl alcohol, isoamyl alcohol, sec-amyl alcohol, tert-amyl alcohol, Examples include 1-ethyl-1-propanol, 2-ethyl-1-butanol, n-hexanol, and cyclohexanol.
- the blending ratio of the oxazoline group-containing polymer and the conductive material is, for example, 0.05 to 80% by weight, preferably 0.1 to 50% by weight.
- the surface of the optical film 11 is directly coated with the above-described coating solution by a known coating method such as wire coating or knife coating, and dried.
- the thickness of the undercoat layer 12 is, for example, 10 to 1000 nm, preferably 20 to 500 nm.
- the release film 1 is peeled off from the pressure-sensitive adhesive layer 6 as shown by the phantom lines in FIG.
- the pressure-sensitive adhesive optical film 10 in which the undercoat layer 12 and the pressure-sensitive adhesive layer 6 are sequentially laminated on the surface of the optical film 11 can be obtained.
- the pressure-sensitive adhesive optical film 10 includes the pressure-sensitive adhesive layer 6 having an excellent appearance. Therefore, an optical device, for example, an image display device, specifically a liquid crystal display (liquid crystal display) that requires an excellent appearance.
- an optical device for example, an image display device, specifically a liquid crystal display (liquid crystal display) that requires an excellent appearance.
- Devices organic electroluminescence devices (organic EL display devices), organic light emitting diodes (organic LEDs, Organic Light Emitting Diode: OLED), plasma display panels (PDP), cathode ray tube display devices (CRT), etc. In these optical devices, a good appearance can be ensured.
- the adhesive optical film 10 is used as a front plate of the optical device described above.
- the front plate is attached to the front surface (surface) of the optical device in order to protect the front portion of the optical device or to give the optical device a high-class feeling (texture or design). Provided.
- the front plate is used as a support for a ⁇ / 4 wavelength plate in, for example, a stereoscopic display device (a so-called 3D image display device such as a 3D display device).
- a stereoscopic display device a so-called 3D image display device such as a 3D display device.
- the front plate is provided on the viewing side (that is, the front side) surface of the optical device, for example.
- the adhesive optical film 10 is also applied to a front part containing a plastic (resin) such as a polycarbonate and / or an acrylic polymer film (specifically, polymethyl methacrylate) in an optical device.
- a plastic such as a polycarbonate and / or an acrylic polymer film (specifically, polymethyl methacrylate)
- acrylic polymer film specifically, polymethyl methacrylate
- the pressure-sensitive adhesive layer 6 is provided by transferring it to the surface of the undercoat layer 12, but it can also be provided directly on the surface of the undercoat layer 12, for example, as shown in FIG.
- the pressure-sensitive adhesive layer 6 on the surface of the undercoat layer 12
- an optical film 11 having the undercoat layer 12 formed on the surface is prepared, and then water-dispersed
- the coating liquid layer 2 is directly formed on the surface of the undercoat layer 12 by applying the mold pressure-sensitive adhesive composition to the surface of the undercoat layer 12.
- the pressure-sensitive adhesive layer 6 is directly provided on the surface of the undercoat layer 12 by drying the coating liquid layer 2.
- the number of recesses 5 due to foreign matters 8 existing on the surface of the undercoat layer 12 or the surface of the optical film 11 can be reduced to a desired number or less.
- the adhesive layer 6 is provided on the surface of the optical film 11 via the undercoat layer 12.
- the adhesive layer 6 is not provided with the undercoat layer 12.
- the agent layer 6 can also be provided directly on the surface of the optical film 11.
- the pressure-sensitive adhesive film of the present invention is described as the pressure-sensitive adhesive optical film 10 including the optical film 11.
- optical characteristics such as a nonwoven fabric and a metal foil (metal film) are provided. It can also form as an adhesive film provided with the base film 11 which does not have and has a mechanical characteristic.
- Example 1 Preparation of water-dispersed pressure-sensitive adhesive composition
- a container 88 parts by weight of butyl acrylate, 5 parts by weight of acrylic acid, 2 parts by weight of mono [poly (propylene oxide) methacrylate] phosphate, 3-methacryloxypropyl-trimethoxysilane (KBM-503, manufactured by Shin-Etsu Silicone)
- KBM-503, manufactured by Shin-Etsu Silicone manufactured by Shin-Etsu Silicone
- emulsion was cooled to room temperature, 10% by weight aqueous ammonia was added to adjust the pH to 8, and SN thickener 640 (hydrophobic group-modified polymer) was added to 100 parts by weight of the solid content of the emulsion. 2 parts by weight of acrylic acid (manufactured by San Nopco) was added, and ion-exchanged water was further added to adjust the solid content concentration to 25% by weight to prepare a water-dispersed pressure-sensitive adhesive composition.
- SN thickener 640 hydrophobic group-modified polymer
- a peeled PET film (release film) having a thickness of 38 ⁇ m is prepared (see FIG. 1A), and then the water-dispersed pressure-sensitive adhesive composition is applied to the surface (treated surface) of the PET sheet.
- a uniform coating was performed using a comma coater to form a coating solution layer having a thickness of 92 ⁇ m (see FIG. 1B).
- the formed coating solution layer was dried by heating at 120 ° C. for 2 minutes to form an adhesive layer having a thickness of 23 ⁇ m (see FIG. 1C).
- Epocross WS-700 aqueous solution type, solid content 25%, main chain: acrylic, pH 7-9, oxazoline value 220 g solid / eq., Manufactured by Nippon Shokubai Co., Ltd.
- Olgacon LBS conductive polythiophene, manufactured by Agfa Materials
- an undercoat coating solution was prepared. This coating solution was applied to the surface of a polarizing film having a thickness of 180 ⁇ m so that the thickness after drying was 20-30 nm. 5 and then dried. This produced the polarizing film by which the undercoat layer was laminated
- Example 2 The amount of SN thickener 640 (hydrophobic group-modified polyacrylic acid) blended to 100 parts by weight of the emulsion is changed to 1 part by weight, and the water-dispersed pressure-sensitive adhesive composition is adjusted by adding ion-exchanged water.
- a water-dispersed pressure-sensitive adhesive composition was prepared in the same manner as in Example 1 except that the solid content concentration was changed to 30% by weight. Subsequently, a coating liquid layer having a thickness of 77 ⁇ m was formed, and then a coating having a thickness of 23 ⁇ m was formed. A liquid layer was formed, and then an adhesive layer and an adhesive optical film including the same were obtained.
- Example 3 Instead of SN thickener 640 (hydrophobic group-modified polyacrylic acid), Aron B-500 (acrylic acid copolymer, manufactured by Toagosei Co., Ltd.) was added, and Aron B-500 was added to 100 parts by weight of the solid content of the emulsion.
- a water-dispersed pressure-sensitive adhesive composition was prepared in the same manner as in Example 1 except that the number of parts was changed to 2.6 parts by weight, and subsequently a coating liquid layer having a thickness of 92 ⁇ m was formed. A pressure-sensitive adhesive layer and a pressure-sensitive adhesive optical film including the same were obtained.
- Example 4 Instead of SN thickener 640 (hydrophobic group-modified polyacrylic acid), Aron B-500 (acrylic acid copolymer) was added, and 2 parts by weight of Aron B-500 was added to 100 parts by weight of the solid content of the emulsion.
- the water-dispersed pressure-sensitive adhesive composition was changed in the same manner as in Example 1 except that the solid content concentration of the water-dispersed pressure-sensitive adhesive composition adjusted by adding ion-exchanged water was changed to 30% by weight. Subsequently, a coating liquid layer having a thickness of 77 ⁇ m was formed, and then a pressure-sensitive adhesive layer having a thickness of 23 ⁇ m and a pressure-sensitive adhesive optical film including the same were obtained.
- Example 5 Instead of SN thickener 640 (hydrophobic group-modified polyacrylic acid), Adecanol UH-541VF (urethane thickener, manufactured by ADEKA) was added, and the number of blending parts of Adecanol UH-541VF with respect to 100 parts by weight of the solid content of the emulsion was increased.
- the water-dispersed type was the same as in Example 1, except that the solid content concentration of the water-dispersed pressure-sensitive adhesive composition adjusted to 2 parts by weight was adjusted to 30% by weight.
- a pressure-sensitive adhesive composition was prepared, and subsequently a coating liquid layer having a thickness of 77 ⁇ m was formed.
- Comparative Example 1 SN thickener 640 (hydrophobic group-modified polyacrylic acid) was not added, and the adjustment of the solid content concentration (dilution) of the water-dispersed pressure-sensitive adhesive composition by addition of ion-exchanged water was not performed. Similarly, a water-dispersed pressure-sensitive adhesive composition having a solid content concentration of 40% by weight was prepared, and subsequently a coating liquid layer having a thickness of 58 ⁇ m was formed. Thereafter, a pressure-sensitive adhesive layer having a thickness of 23 ⁇ m and a pressure-sensitive adhesive optical film including the same Got.
- Comparative Example 2 A water-dispersed pressure-sensitive adhesive composition was prepared in the same manner as in Example 1 except that SN thickener 640 (hydrophobic group-modified polyacrylic acid) was not added.
- SN thickener 640 hydrophobic group-modified polyacrylic acid
- Comparative Example 3 A water-dispersed pressure-sensitive adhesive composition in which the blending number of SN thickener 640 (hydrophobic group-modified polyacrylic acid) with respect to 100 parts by weight of the emulsion is changed to 0.5 parts by weight and further adjusted by adding ion-exchanged water.
- a water-dispersed pressure-sensitive adhesive composition was prepared in the same manner as in Example 1 except that the solid content concentration of the product was changed to 35% by weight. Subsequently, a coating liquid layer having a thickness of 66 ⁇ m was formed, and then a thickness of 23 ⁇ m. The pressure-sensitive adhesive layer and the pressure-sensitive adhesive optical film including the same were obtained.
- the size of the recess was measured with a non-contact three-dimensional surface shape roughness meter (WykoNT9100, manufactured by Veeco).
- Viscosity of water-dispersed pressure-sensitive adhesive composition The viscosity of the water-dispersed pressure-sensitive adhesive compositions of Examples 1 to 5 and Comparative Examples 1 to 3 at 30 ° C. and a shear rate of 1 sec ⁇ 1 was measured using a cone / plate viscometer. (Reostress RS-1 type, manufactured by HAAKE). The results are shown in Table 1.
- the thickener (SN thickener 640) used in Example 1 and having the turbidity of 100 NTU or less is uniformly dispersed in the water-dispersed polymer.
- the thickener (Aron B-500) used in Example 3 and having a turbidity exceeding 100 NTU is relatively insoluble (particles) in the water-dispersed polymer. It remains as large particles.
- SN thickener 640 * 1 trade name, hydrophobic group-modified polyacrylic acid, Sanronco Aron B-500 * 2: trade name, acrylic acid copolymer, Toagosei Co., Ltd.
- Adecanol UH-541VF * 3 trade name, Urethane thickener, ADEKA NTU * 4: unit of turbidity, Nephelometric Turbidity Unit
- the adhesive layer is used for adhesive films that are widely used in various industrial fields.
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Abstract
Description
オキサゾリン基含有ポリマーは、そのオキサゾリン価が、例えば、1500g solid/eq.以下、好ましくは、1200g solid/eq.以下である。
(水分散型粘着剤組成物の調製)
容器に、アクリル酸ブチル88重量部、アクリル酸5重量部、モノ[ポリ(プロピレンオキシド)メタクリレート]リン酸エステル2重量部、3-メタクリルオキシプロピル-トリメトキシシラン(KBM-503、信越シリコーン社製)0.03重量部を配合してモノマー成分を調製した。
まず、剥離処理した厚み38μmのPETフィルム(離型フィルム)を用意し(図1(a)参照)、次いで、上記の水分散型粘着剤組成物を、PETシートの表面(処理面)に、コンマコーターを用いて均一に塗布して、厚み92μmの塗布液層を形成した(図1(b)参照)。
まず、下塗り層が積層された偏光フィルムを用意した(図5(a)参照)。
エマルションの固形分100重量部に対するSNシックナー640(疎水基変性ポリアクリル酸)の配合部数を、1重量部に変更し、さらに、イオン交換水の追加により調整される水分散型粘着剤組成物の固形分濃度を30重量%に変更した以外は、実施例1と同様にして水分散型粘着剤組成物を調製し、続けて、厚み77μmの塗布液層を形成し、その後、厚み23μmの塗布液層を形成し、その後、粘着剤層およびそれを備える粘着型光学フィルムを得た。
SNシックナー640(疎水基変性ポリアクリル酸)に代えて、アロンB-500(アクリル酸系共重合体、東亞合成社製)を添加し、エマルションの固形分100重量部に対するアロンB-500の配合部数を、2.6重量部に変更した以外は、実施例1と同様にして水分散型粘着剤組成物を調製し、続けて、厚み92μmの塗布液層を形成し、その後、厚み23μmの粘着剤層およびそれを備える粘着型光学フィルムを得た。
SNシックナー640(疎水基変性ポリアクリル酸)に代えて、アロンB-500(アクリル酸系共重合体)を添加し、エマルションの固形分100重量部に対するアロンB-500の配合部数を、2重量部に変更し、さらに、イオン交換水の追加により調整される水分散型粘着剤組成物の固形分濃度を30重量%に変更した以外は、実施例1と同様にして水分散型粘着剤組成物を調製し、続けて、厚み77μmの塗布液層を形成し、その後、厚み23μmの粘着剤層およびそれを備える粘着型光学フィルムを得た。
SNシックナー640(疎水基変性ポリアクリル酸)に代えて、アデカノールUH-541VF(ウレタン系増粘剤、ADEKA社製)を添加し、エマルションの固形分100重量部に対するアデカノールUH-541VFの配合部数を、2重量部に変更し、さらに、イオン交換水の追加により調整される水分散型粘着剤組成物の固形分濃度を30重量%に変更した以外は、実施例1と同様にして水分散型粘着剤組成物を調製し、続けて、厚み77μmの塗布液層を形成し、その後、厚み23μmの粘着剤層およびそれを備える粘着型光学フィルムを得た。
SNシックナー640(疎水基変性ポリアクリル酸)を添加せず、イオン交換水の追加による水分散型粘着剤組成物の固形分濃度の調整(希釈)を実施しなかった以外は、実施例1と同様にして固形分濃度40重量%の水分散型粘着剤組成物を調製し、続けて、厚み58μmの塗布液層を形成し、その後、厚み23μmの粘着剤層およびそれを備える粘着型光学フィルムを得た。
SNシックナー640(疎水基変性ポリアクリル酸)を添加しなかった以外は、実施例1と同様にして水分散型粘着剤組成物を調製した。
エマルションの固形分100重量部に対するSNシックナー640(疎水基変性ポリアクリル酸)の配合部数を、0.5重量部に変更し、さらに、イオン交換水の追加により調整される水分散型粘着剤組成物の固形分濃度を35重量%に変更した以外は、実施例1と同様にして水分散型粘着剤組成物を調製し、続けて、厚み66μmの塗布液層を形成し、その後、厚み23μmの粘着剤層およびそれを備える粘着型光学フィルムを得た。
(1)外観観察
実施例1~5、比較例1および3の粘着型光学フィルムの粘着剤層を、PETフィルム側から目視により観察することにより、上記した定義の凹部の有無を観察するとともに、1m2当たりの凹部の個数を勘定した。それらの結果を、表1に示す。
実施例1~5および比較例1~3の水分散型粘着剤組成物の30℃、せん断速度1sec-1における粘度を、コーン/プレート型粘度計(レオストレスRS-1型、HAAKE社製)により測定した。その結果を、表1に示す。
実施例1~5および比較例3で使用した増粘剤を、水に配合して1重量%水溶液を調製し、さらに、アンモニア水にてpH8に調整して、増粘剤水溶液を調製した。次いで、調製した増粘剤水溶液の濁度を濁度計(LaMotte2020型、オルガノ社製)にて測定した。その結果を表1に示す。
実施例1~5、比較例1および3の「粘着剤層の形成」において得られた厚み23μmの粘着剤層を、スライドガラス板(マイクロスライドガラス、厚み1.3mm、マツナミガラス社製)に転写し、かかる粘着剤層のヘイズ値を、JIS K7136に準拠して、ヘイズメーター(HM-150、村上色彩技術研究所社)により、測定した。その結果を表1に示す。
実施例1および3の粘着剤層の表面を、TEM(透過型電子顕微鏡)にて観察した。実施例1および3の粘着剤層のTEM写真の画像処理図を、図6および7に、それぞれ示す。
SNシックナー640*1:商品名、疎水基変性ポリアクリル酸、サンノプコ社製
アロンB-500*2:商品名、アクリル酸系共重合体、東亞合成社製
アデカノールUH-541VF*3:商品名、ウレタン系増粘剤、ADEKA社製
NTU*4:濁度の単位、Nephelometric Turbidity Unit
なお、上記発明は、本発明の例示の実施形態として提供したが、これは単なる例示にすぎず、限定的に解釈してはならない。当該技術分野の当業者によって明らかな本発明の変形例は、後記特許請求の範囲に含まれるものである。
Claims (8)
- 水分散型粘着剤組成物を塗布および乾燥させることにより得られる粘着剤層であって、
前記粘着剤層の表面において、厚み方向の深さが0.2~20μmであり、前記表面に沿う最大長さが1~10mmである凹部の数が、1m2当たり5個以下であることを特徴とする、粘着剤層。 - 前記水分散型粘着剤組成物の固形分濃度が5~32重量%であり、
前記粘着剤層の厚みが3~100μmであることを特徴とする、請求項1に記載の粘着剤層。 - 水分散型アクリル系ポリマーと増粘剤とを含有し、
前記水分散型粘着剤組成物の30℃、せん断速度1sec-1における粘度が、0.1~50Pa・sであることを特徴とする、請求項1に記載の粘着剤層。 - 前記増粘剤は、1重量%水溶液として調製し、さらにpH8に調整したときの濁度が、100NTU以下であることを特徴とする、請求項3に記載の粘着剤層。
- 厚み23μmの前記粘着剤層のヘイズ値が、1.0%以下であることを特徴とする、請求項1に記載の粘着剤層。
- 基材と、
前記基材の表面に積層される粘着剤層と
を備え、
前記接着剤層は、水分散型粘着剤組成物を塗布および乾燥させることにより得られ、
前記粘着剤層の表面において、厚み方向の深さが0.2~20μmであり、前記表面に沿う最大長さが1~10mmである凹部の数が、1m2当たり5個以下であることを特徴とする、粘着フィルム。 - 前記基材が、光学フィルムであることを特徴とする、請求項6に記載の粘着フィルム。
- 光学フィルムと、
前記光学フィルムの表面に積層される粘着剤層と
を備え、
前記接着剤層は、水分散型粘着剤組成物を塗布および乾燥させることにより得られ、前記粘着剤層の表面において、厚み方向の深さが0.2~20μmであり、前記表面に沿う最大長さが1~10mmである凹部の数が、1m2当たり5個以下であることを特徴とする、光学装置。
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