WO2012161123A1 - 粘着剤層付偏光フィルムおよび画像表示装置 - Google Patents
粘着剤層付偏光フィルムおよび画像表示装置 Download PDFInfo
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- WO2012161123A1 WO2012161123A1 PCT/JP2012/062824 JP2012062824W WO2012161123A1 WO 2012161123 A1 WO2012161123 A1 WO 2012161123A1 JP 2012062824 W JP2012062824 W JP 2012062824W WO 2012161123 A1 WO2012161123 A1 WO 2012161123A1
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- Prior art keywords
- polarizing film
- adhesive layer
- sensitive adhesive
- pressure
- meth
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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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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/306—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/062—Copolymers with monomers not covered by C08L33/06
- C08L33/066—Copolymers with monomers not covered by C08L33/06 containing -OH groups
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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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- 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
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
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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
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
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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
- C09J7/29—Laminated material
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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]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/412—Transparent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/42—Polarizing, birefringent, filtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/514—Oriented
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/732—Dimensional properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
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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
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
-
- 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
- C09J2429/00—Presence of polyvinyl alcohol
- C09J2429/006—Presence of polyvinyl alcohol in the substrate
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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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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133528—Polarisers
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2201/00—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00
- G02F2201/50—Protective arrangements
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2202/00—Materials and properties
- G02F2202/28—Adhesive materials or arrangements
Definitions
- the present invention relates to a polarizing film and a polarizing film with an adhesive layer having an adhesive layer provided on the polarizing film. Furthermore, this invention relates to image display apparatuses, such as a liquid crystal display device using the said polarizing film with an adhesive layer, an organic electroluminescent display device, and PDP.
- polarizing films In liquid crystal display devices and the like, it is indispensable to dispose polarizing elements on both sides of the liquid crystal cell because of its image forming method, and generally a polarizing film is attached.
- an adhesive When sticking the said polarizing film to a liquid crystal cell, an adhesive is normally used.
- attachment of a polarizing film and a liquid crystal cell reduces the loss of light normally, each material is closely_contact
- the adhesive since the adhesive has the merit that a drying step is not required to fix the polarizing film, the adhesive is a polarizing film with an adhesive layer provided in advance as an adhesive layer on one side of the polarizing film.
- a film is generally used.
- a release film is usually attached to the pressure-sensitive adhesive layer of the polarizing film with a pressure-sensitive adhesive layer.
- the release film is peeled off from the pressure-sensitive adhesive layer of the polarizing film with the pressure-sensitive adhesive layer. Static electricity is generated.
- the static electricity generated in this way affects the orientation of the liquid crystal inside the liquid crystal display device, leading to defects. Further, display unevenness due to static electricity may occur when the liquid crystal display device is used.
- the generation of static electricity can be suppressed, for example, by forming an antistatic layer on the outer surface of the polarizing film, but the effect is small and there is a problem that static electricity generation cannot be fundamentally prevented.
- Patent Documents 1 and 2 As means for imparting an antistatic function to the pressure-sensitive adhesive layer, for example, blending an ionic compound with the pressure-sensitive adhesive forming the pressure-sensitive adhesive layer has been proposed (Patent Documents 1 and 2). Moreover, the durability in an adhesive state is calculated
- Patent Document 1 describes that an adhesive tape imparted with antistatic properties can be obtained by an acrylic adhesive containing a polyether polyol compound and at least one alkali metal salt.
- the acrylic pressure-sensitive adhesive containing the polyether polyol compound contains an isocyanate-based cross-linking agent as a cross-linking agent
- the cross-linking agent may greatly affect the cross-linking degree of the pressure-sensitive adhesive layer. Therefore, in Patent Document 1, as shown in the Examples, in forming the pressure-sensitive adhesive layer, first, the acrylic copolymer and the isocyanate-based crosslinking agent are crosslinked, and then dissolved again to form a polyether polyol compound and The method of mix
- the formation of the pressure-sensitive adhesive layer of Patent Document 1 is complicated and difficult to apply to actual processes. Further, the pressure-sensitive adhesive layer of Patent Document 1 does not have sufficient durability.
- Patent Document 2 describes that a pressure-sensitive adhesive layer formed by using a pressure-sensitive adhesive composition in which an acrylic copolymer and an ester plasticizer having an ether bond and an alkali metal salt are used in combination can achieve both durability and antistatic function.
- a pressure-sensitive adhesive layer described in Patent Document 2 has durability under the conditions of 1000 hours at 80 ° C., 1000 hours at 60 ° C. and 90% RH.
- an ester plasticizer having an ether bond is also blended in the pressure-sensitive adhesive layer described in Patent Document 2, and the preparation of the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive layer is complicated.
- An object of the present invention is to provide a polarizing film with an adhesive layer having an antistatic function and satisfying durability.
- Another object of the present invention is to provide an image display device using the polarizing film with the pressure-sensitive adhesive layer.
- the present invention is a polarizing film and a polarizing film with a pressure-sensitive adhesive layer having a pressure-sensitive adhesive layer provided on the polarizing film
- the polarizing film has a transparent protective film on one side or both sides of a polarizer having a thickness of 10 ⁇ m or less
- the pressure-sensitive adhesive layer contains a (meth) acrylic polymer (A) and an ionic compound (B). It is related with the polarizing film with an adhesive layer characterized by being formed from an adhesive composition.
- polarizing film with a pressure-sensitive adhesive layer as a polarizer having a thickness of 10 ⁇ m or less, it is a continuous web polarizing film made of a polyvinyl alcohol resin in which a dichroic substance is oriented, and is formed on a thermoplastic resin substrate.
- a laminate obtained by stretching a laminated body including a polyvinyl alcohol-based resin layer in a two-stage stretching process composed of air-assisted stretching and boric acid-water stretching can be used.
- the ionic compound (B) is preferably an alkali metal salt and / or an organic cation-anion salt.
- 0.0001 to 5 parts by weight of the ionic compound (B) is preferably contained with respect to 100 parts by weight of the (meth) acrylic polymer (A).
- the (meth) acrylic polymer (A) may preferably be one containing an alkyl (meth) acrylate and a hydroxyl group-containing monomer as monomer units.
- the (meth) acrylic polymer (A) may preferably be one containing an alkyl (meth) acrylate and a carboxyl group-containing monomer as monomer units.
- the pressure-sensitive adhesive composition may further contain a crosslinking agent.
- the crosslinking agent (C) is preferably contained in an amount of 0.01 to 20 parts by weight with respect to 100 parts by weight of the (meth) acrylic polymer (A).
- the crosslinking agent (C) is preferably at least one selected from an isocyanate compound and a peroxide.
- silane coupling agent (D) can be further contained with respect to 100 parts by weight of the (meth) acrylic polymer (A).
- the (meth) acrylic polymer (A) preferably has a weight average molecular weight of 500,000 to 3,000,000.
- the said polarizing film with an adhesive layer can have an easily bonding layer between a polarizing film and an adhesive layer.
- the present invention also relates to an image display device using at least one polarizing film with an adhesive layer.
- an antistatic function can be imparted by adding an ionic compound to the adhesive.
- the antistatic function is efficiently expressed by bleeding out of the ionic compound on the surface of the pressure-sensitive adhesive layer.
- an ionic compound is present on the surface of the pressure-sensitive adhesive layer, the adhesive force with the adherend is reduced.
- a polarizing film using a polarizer having a normal thickness for example, a thickness of 20 ⁇ m
- the dimensional change of the polarizer during heating and humidification is large, and the dimensional change influences, and peeling occurs in the heating and humidification tests. .
- the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive layer of the polarizing film with a pressure-sensitive adhesive layer of the present invention is an ion that can impart an antistatic function in addition to the (meth) acrylic polymer (A) that is a base polymer.
- the pressure-sensitive adhesive layer containing the adhesive compound (B) and formed of the pressure-sensitive adhesive composition has an excellent antistatic function.
- the polarizing film used in the polarizing film with the pressure-sensitive adhesive layer of the present invention uses a thin polarizer having a thickness of 10 ⁇ m or less, and can control the dimensional change of the polarizer during heating and humidification to be small. Even when the layer contains the ionic compound (B), peeling due to a decrease in durability can be suppressed.
- the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive layer of the polarizing film with a pressure-sensitive adhesive layer of the present invention contains a (meth) acrylic polymer (A) as a base polymer.
- the (meth) acrylic polymer (A) usually contains an alkyl (meth) acrylate as a main component as a monomer unit.
- (Meth) acrylate refers to acrylate and / or methacrylate, and (meth) of the present invention has the same meaning.
- alkyl (meth) acrylate constituting the main skeleton of the (meth) acrylic polymer (A) include linear or branched alkyl groups having 1 to 18 carbon atoms.
- the alkyl group includes methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, amyl group, hexyl group, cyclohexyl group, heptyl group, 2-ethylhexyl group, isooctyl group, nonyl group, decyl group.
- alkyl groups preferably have an average carbon number of 3 to 9.
- alkyl (meth) acrylates containing aromatic rings such as phenoxyethyl (meth) acrylate and benzyl (meth) acrylate are used from the viewpoints of adhesive properties, durability, retardation adjustment, refractive index adjustment, and the like. be able to.
- the alkyl (meth) acrylate containing an aromatic ring can be used by mixing a polymer obtained by polymerizing it with the (meth) acrylic polymer exemplified above, but from the viewpoint of transparency, it contains an aromatic ring.
- the alkyl (meth) acrylate is preferably copolymerized with the alkyl (meth) acrylate.
- the ratio of the alkyl (meth) acrylate containing the aromatic ring in the (meth) acrylic polymer (A) is 50 in the weight ratio of all the constituent monomers (100 wt%) of the (meth) acrylic polymer (A). It can contain in the ratio of the weight% or less. Further, the content of the alkyl (meth) acrylate containing an aromatic ring is preferably 1 to 35% by weight, more preferably 1 to 20% by weight, further preferably 7 to 18% by weight, and further preferably 10 to 16%. % By weight is preferred.
- the (meth) acrylic polymer (A) has a polymerizable functional group having an unsaturated double bond such as a (meth) acryloyl group or a vinyl group for the purpose of improving adhesiveness and heat resistance.
- One or more copolymerization monomers can be introduced by copolymerization.
- copolymerized monomers include, for example, 2-hydroxyethyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, (meth) acrylic acid 6 Hydroxyl-containing monomers such as hydroxyhexyl, 8-hydroxyoctyl (meth) acrylate, 10-hydroxydecyl (meth) acrylate, 12-hydroxylauryl (meth) acrylate and (4-hydroxymethylcyclohexyl) -methyl acrylate Carboxyl group-containing monomers such as (meth) acrylic acid, carboxyethyl (meth) acrylate, carboxypentyl (meth) acrylate, itaconic acid, maleic acid, fumaric acid and crotonic acid; acid anhydrides such as maleic anhydride and itaconic anhydride Monomer-containing monomer; Caprolac of acrylic acid Adducts such as styrene sulfonic acid
- (N-substituted) amides such as (meth) acrylamide, N, N-dimethyl (meth) acrylamide, N-butyl (meth) acrylamide, N-methylol (meth) acrylamide, N-methylolpropane (meth) acrylamide, etc.
- Further modifying monomers include vinyl acetate, vinyl propionate, N-vinyl pyrrolidone, methyl vinyl pyrrolidone, vinyl pyridine, vinyl piperidone, vinyl pyrimidine, vinyl piperazine, vinyl pyrazine, vinyl pyrrole, vinyl imidazole, vinyl oxazole, vinyl morpholine, N- Vinyl monomers such as vinylcarboxylic amides, styrene, ⁇ -methylstyrene, N-vinylcaprolactam; cyanoacrylate monomers such as acrylonitrile and methacrylonitrile; epoxy group-containing acrylic monomers such as glycidyl (meth) acrylate; (Meth) acrylic acid polyethylene glycol, (meth) acrylic acid polypropylene glycol, (meth) acrylic acid methoxyethylene glycol, (meth) acrylic acid meso Glycol acrylic ester monomers such as xypolypropylene glycol; acrylic ester monomers such as
- examples of copolymerizable monomers other than the above include silane-based monomers containing silicon atoms.
- examples of the silane monomer include 3-acryloxypropyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 4-vinylbutyltrimethoxysilane, 4-vinylbutyltriethoxysilane, and 8-vinyloctyltrimethoxysilane.
- copolymer monomers examples include tripropylene glycol di (meth) acrylate, tetraethylene glycol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, bisphenol A diglycidyl ether di (meth) acrylate, neo Pentyl glycol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, dipentaerythritol penta (meth) acrylate, dipentaerythritol hexa (meth) acrylate (Meth) acryloyl such as esterified product of (meth) acrylic acid and polyhydric alcohol such as caprolactone-modified dipentaerythritol hexa (meth) acrylate A polyfunctional monomer having
- the (meth) acrylic polymer (A) is mainly composed of alkyl (meth) acrylate in the weight ratio of all constituent monomers, and the proportion of the copolymerized monomer in the (meth) acrylic polymer (A) is particularly limited.
- the proportion of the copolymerization monomer is preferably about 0 to 20%, about 0.1 to 15%, and more preferably about 0.1 to 10% in the weight ratio of all the constituent monomers.
- hydroxyl group-containing monomers and carboxyl group-containing monomers are preferably used from the viewpoint of adhesion and durability.
- a hydroxyl group-containing monomer and a carboxyl group-containing monomer can be used in combination.
- These copolymerization monomers serve as reaction points with the crosslinking agent when the pressure-sensitive adhesive composition contains a crosslinking agent. Since a hydroxyl group-containing monomer, a carboxyl group-containing monomer, and the like are rich in reactivity with an intermolecular crosslinking agent, they are preferably used for improving the cohesiveness and heat resistance of the resulting pressure-sensitive adhesive layer.
- a hydroxyl group-containing monomer is preferable from the viewpoint of reworkability, and a carboxyl group-containing monomer is preferable from the viewpoint of achieving both durability and reworkability.
- the proportion is preferably 0.01 to 15% by weight, more preferably 0.03 to 10% by weight, and further preferably 0.05 to 7% by weight.
- the proportion is preferably 0.05 to 10% by weight, more preferably 0.1 to 8% by weight, and further preferably 0.2 to 6% by weight. .
- the (meth) acrylic polymer (A) of the present invention usually has a weight average molecular weight in the range of 500,000 to 3,000,000. In view of durability, particularly heat resistance, it is preferable to use those having a weight average molecular weight of 700,000 to 2,700,000. Further, it is preferably 800,000 to 2.5 million. A weight average molecular weight of less than 500,000 is not preferable in terms of heat resistance. On the other hand, if the weight average molecular weight is more than 3 million, a large amount of dilution solvent is required to adjust the viscosity for coating, which is not preferable.
- the weight average molecular weight is a value measured by GPC (gel permeation chromatography) and calculated in terms of polystyrene.
- the (meth) acrylic polymer (A) to be obtained may be any of a random copolymer, a block copolymer, a graft copolymer and the like.
- solution polymerization for example, ethyl acetate, toluene or the like is used as a polymerization solvent.
- the reaction is carried out under an inert gas stream such as nitrogen and a polymerization initiator is added, usually at about 50 to 70 ° C. under reaction conditions for about 5 to 30 hours.
- the polymerization initiator, chain transfer agent, emulsifier and the like used for radical polymerization are not particularly limited and can be appropriately selected and used.
- the weight average molecular weight of the (meth) acrylic polymer (A) can be controlled by the amount of polymerization initiator, the amount of chain transfer agent used, and the reaction conditions, and the amount used is appropriately adjusted according to these types.
- polymerization initiator examples include 2,2′-azobisisobutyronitrile, 2,2′-azobis (2-amidinopropane) dihydrochloride, 2,2′-azobis [2- (5-methyl-2 -Imidazolin-2-yl) propane] dihydrochloride, 2,2'-azobis (2-methylpropionamidine) disulfate, 2,2'-azobis (N, N'-dimethyleneisobutylamidine), 2,2 Azo initiators such as' -azobis [N- (2-carboxyethyl) -2-methylpropionamidine] hydrate (VA-057, manufactured by Wako Pure Chemical Industries, Ltd.), persulfates such as potassium persulfate and ammonium persulfate , Di (2-ethylhexyl) peroxydicarbonate, di (4-tert-butylcyclohexyl) peroxydicarbonate, di-sec-butyl Peroxydicarbonate, t
- the polymerization initiator may be used singly or as a mixture of two or more, but the total content is 0.005 to 1 part by weight with respect to 100 parts by weight of the monomer. Is preferably about 0.02 to 0.5 parts by weight.
- the amount of the polymerization initiator used Is preferably about 0.06 to 0.2 parts by weight, more preferably about 0.08 to 0.175 parts by weight, based on 100 parts by weight of the total amount of monomer components.
- chain transfer agent examples include lauryl mercaptan, glycidyl mercaptan, mercaptoacetic acid, 2-mercaptoethanol, thioglycolic acid, 2-ethylhexyl thioglycolate, and 2,3-dimercapto-1-propanol.
- the chain transfer agent may be used alone or in combination of two or more, but the total content is 0.1 parts by weight with respect to 100 parts by weight of the total amount of monomer components. Less than or equal to
- emulsifier used in emulsion polymerization examples include anionic emulsifiers such as sodium lauryl sulfate, ammonium lauryl sulfate, sodium dodecylbenzenesulfonate, ammonium polyoxyethylene alkyl ether sulfate, sodium polyoxyethylene alkyl phenyl ether sulfate, and polyoxy Nonionic emulsifiers such as ethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene fatty acid ester, polyoxyethylene-polyoxypropylene block polymer and the like can be mentioned. These emulsifiers may be used alone or in combination of two or more.
- reactive emulsifiers emulsifiers into which radical polymerizable functional groups such as propenyl groups and allyl ether groups are introduced, specifically, for example, Aqualon HS-10, HS-20, KH-10, BC-05 BC-10, BC-20 (all of which are manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), Adekaria soap SE10N (manufactured by Asahi Denka Kogyo Co., Ltd.), and the like.
- Reactive emulsifiers are preferable because they are incorporated into the polymer chain after polymerization and thus have improved water resistance.
- the amount of the emulsifier used is preferably 0.3 to 5 parts by weight with respect to 100 parts by weight of the total amount of monomer components, and more preferably 0.5 to 1 part by weight from the viewpoint of polymerization stability and mechanical stability.
- the pressure-sensitive adhesive composition of the present invention contains an ionic compound (B) in addition to the (meth) acrylic polymer (A).
- an ionic compound (B) an alkali metal salt and / or an organic cation-anion salt can be preferably used.
- an organic salt or inorganic salt of an alkali metal can be used.
- organic cation-anion salt refers to an organic salt whose cation part is composed of an organic substance, and the anion part may be an organic substance or an inorganic substance. There may be.
- Organic cation-anion salt is also called an ionic liquid or ionic solid.
- alkali metal salt examples include lithium, sodium, and potassium ions. Of these alkali metal ions, lithium ions are preferred.
- the anion part of the alkali metal salt may be composed of an organic material or an inorganic material.
- Examples of the anion part constituting the organic salt include CH 3 COO ⁇ , CF 3 COO ⁇ , CH 3 SO 3 ⁇ , CF 3 SO 3 ⁇ , (CF 3 SO 2 ) 3 C ⁇ , and C 4 F 9 SO 3.
- an anion moiety containing a fluorine atom is preferably used because an ionic compound having good ion dissociation properties can be obtained.
- the anion part constituting the inorganic salt includes Cl ⁇ , Br ⁇ , I ⁇ , AlCl 4 ⁇ , Al 2 Cl 7 ⁇ , BF 4 ⁇ , PF 6 ⁇ , ClO 4 ⁇ , NO 3 ⁇ , AsF 6 ⁇ , SbF. 6 ⁇ , NbF 6 ⁇ , TaF 6 ⁇ , (CN) 2 N ⁇ , and the like are used.
- (perfluoroalkylsulfonyl) imide represented by the general formula (1) such as (CF 3 SO 2 ) 2 N ⁇ , (C 2 F 5 SO 2 ) 2 N ⁇ , etc. is preferable, (Trifluoromethanesulfonyl) imide represented by CF 3 SO 2 ) 2 N ⁇ is preferable.
- alkali metal organic salt examples include sodium acetate, sodium alginate, sodium lignin sulfonate, sodium toluenesulfonate, LiCF 3 SO 3 , Li (CF 3 SO 2 ) 2 N, Li (CF 3 SO 2 ) 2 N, Li (C 2 F 5 SO 2 ) 2 N, Li (C 4 F 9 SO 2 ) 2 N, Li (CF 3 SO 2 ) 3 C, KO 3 S (CF 2 ) 3 SO 3 K, LiO 3 S (CF 2) 3 SO 3 K , and the like, among these LiCF 3 SO 3, Li (CF 3 SO 2) 2 N, Li (C 2 F 5 SO 2) 2 N, Li (C 4 F 9 SO 2 ) 2 N, Li (CF 3 SO 2 ) 3 C and the like are preferable, and Li (CF 3 SO 2 ) 2 N, Li (C 2 F 5 SO 2 ) 2 N, Li (C 4 F 9 SO 2) 2 Fluorine-containing lithium imide salt is more preferably equal, particularly (perfluoroal
- examples of the alkali metal inorganic salt include lithium perchlorate and lithium iodide.
- the organic cation-anion salt used in the present invention is composed of a cation component and an anion component, and the cation component is composed of an organic substance.
- the cation component specifically, pyridinium cation, piperidinium cation, pyrrolidinium cation, cation having pyrroline skeleton, cation having pyrrole skeleton, imidazolium cation, tetrahydropyrimidinium cation, dihydropyrimidinium cation, Examples include pyrazolium cation, pyrazolinium cation, tetraalkylammonium cation, trialkylsulfonium cation, and tetraalkylphosphonium cation.
- anion component examples include Cl ⁇ , Br ⁇ , I ⁇ , AlCl 4 ⁇ , Al 2 Cl 7 ⁇ , BF 4 ⁇ , PF 6 ⁇ , ClO 4 ⁇ , NO 3 ⁇ , CH 3 COO ⁇ , CF 3 COO.
- a compound comprising a combination of the above cation component and anion component is appropriately selected and used.
- CIL-314 manufactured by Nippon Carlit Co., Ltd.
- IVA2-1 manufactured by Guangei Chemical Co., Ltd.
- tetramethylammonium bis (trifluoromethanesulfonyl) imide trimethylethyl bis (trifluoromethanesulfonyl) imide, trimethylbutyl bis (trifluoromethanesulfonyl) imide, trimellimer pentyl bis (trifluoromethanesulfonyl) imide, trimethylheptyl bis (Trifluoromethanesulfonyl) imide, trimethyloctylbis (trifluoromethanesulfonyl) imide, tetraethylammonium bis (trifluoromethanesulfonyl) imide, triethylbutylbis (tri
- 1-dimethylpyrrolidinium bis (trifluoromethanesulfonyl) imide 1-methyl-1-ethylpyrrolidinium bis (trifluoromethanesulfonyl) imide, 1-methyl-1-propylpyrrolidinium bis (trifluoromethane) Sulfonyl) imide, 1-methyl-1-butylpyrrolidinium bis (trifluoromethanesulfonyl) imide, 1-methyl-1-pentylpyrrolidinium bis (trifluoromethanesulfonyl) imide, 1-methyl-1-hexylpyrrolidinium Bis (trifluoromethanesulfonyl) imide, 1-methyl-1-heptylpyrrolidinium bis (trifluoromethanesulfonyl) imide, 1-ethyl-1-propylpyrrolidinium bis (trifluoromethanesulfonyl) imide, 1-e
- bis (trifluoromethanesulfonyl) imide bis (pentafluorosulfonyl) imide, bis (heptafluoropropanesulfonyl) imide, bis (nonafluorobutanesulfonyl) imide, trifluoromethanesulfonylnonafluorobutanesulfonylimide, And compounds using heptafluoropropanesulfonyl trifluoromethanesulfonylimide, pentafluoroethanesulfonylnonafluorobutanesulfonylimide, cyclo-hexafluoropropane-1,3-bis (sulfonyl) imide anion, and the like.
- Examples of the ionic compound (B) include inorganic salts such as ammonium chloride, aluminum chloride, copper chloride, ferrous chloride, ferric chloride, ammonium sulfate, in addition to the alkali metal salts and organic cation-anion salts. Is mentioned. These ionic compounds (B) can be used alone or in combination.
- the proportion of the ionic compound (B) in the pressure-sensitive adhesive composition of the present invention is preferably 0.0001 to 5 parts by weight with respect to 100 parts by weight of the (meth) acrylic polymer (A).
- the compound (B) is preferably 0.01 parts by weight or more, and more preferably 0.1 parts by weight or more.
- the amount of the ionic compound (B) is more than 5 parts by weight, the durability may not be sufficient.
- the compound (B) is preferably 3 parts by weight or less, and more preferably 1 part by weight or less.
- the ratio of the said compound (B) can employ
- the pressure-sensitive adhesive composition of the present invention can contain a crosslinking agent (C).
- a crosslinking agent C
- an organic crosslinking agent or a polyfunctional metal chelate can be used as the crosslinking agent (C).
- the organic crosslinking agent include an isocyanate crosslinking agent, a peroxide crosslinking agent, an epoxy crosslinking agent, and an imine crosslinking agent.
- a polyfunctional metal chelate is one in which a polyvalent metal is covalently or coordinately bonded to an organic compound.
- polyvalent metal atoms include Al, Cr, Zr, Co, Cu, Fe, Ni, V, Zn, In, Ca, Mg, Mn, Y, Ce, Sr, Ba, Mo, La, Sn, Ti, and the like.
- Examples of the atom in the organic compound that is covalently bonded or coordinated include an oxygen atom, and examples of the organic compound include an alkyl ester, an alcohol compound, a carboxylic acid compound, an ether compound
- an isocyanate-based crosslinking agent and / or a peroxide-type crosslinking agent is preferable.
- the compound related to the isocyanate crosslinking agent include isocyanate monomers such as tolylene diisocyanate, chlorophenylene diisocyanate, tetramethylene diisocyanate, xylylene diisocyanate, diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, and these isocyanate monomers.
- a polyisocyanate compound which is one or a polyisocyanate compound derived from one selected from the group consisting of hexamethylene diisocyanate, hydrogenated xylylene diisocyanate, and isophorone diisocyanate.
- hexamethylene diisocyanate, hydrogenated xylylene diisocyanate, isophorone diisocyanate, polyol-modified is selected from the group consisting of hexamethylene diisocyanate, hydrogenated xylylene diisocyanate, and isophorone diisocyanate or a polyisocyanate compound derived therefrom.
- examples include hexamethylene diisocyanate, polyol-modified hydrogenated xylylene diisocyanate, trimer-type hydrogenated xylylene diisocyanate, and polyol-modified isophorone diisocyanate.
- the exemplified polyisocyanate compound is preferable because the reaction with a hydroxyl group proceeds rapidly, particularly using an acid or base contained in the polymer as a catalyst, and thus contributes to the speed of crosslinking.
- any radical active species can be used as long as it generates radical active species by heating or light irradiation to advance the crosslinking of the base polymer of the pressure-sensitive adhesive composition.
- peroxides examples include di (2-ethylhexyl) peroxydicarbonate (1 minute half-life temperature: 90.6 ° C.), di (4-t-butylcyclohexyl) peroxydicarbonate (1 Minute half-life temperature: 92.1 ° C.), di-sec-butyl peroxydicarbonate (1 minute half-life temperature: 92.4 ° C.), t-butyl peroxyneodecanoate (1 minute half-life temperature: 103 0.5 ° C.), t-hexyl peroxypivalate (1 minute half-life temperature: 109.1 ° C.), t-butyl peroxypivalate (1 minute half-life temperature: 110.3 ° C.), dilauroyl peroxide ( 1 minute half-life temperature: 116.4 ° C.), di-n-octanoyl peroxide (1 minute half-life temperature: 117.4 ° C.), 1,1,3,3-tetramethylbutyl
- di (4-t-butylcyclohexyl) peroxydicarbonate (1 minute half-life temperature: 92.1 ° C.)
- dilauroyl peroxide (1 minute half-life temperature: 116. 4 ° C)
- dibenzoyl peroxide (1 minute half-life temperature: 130.0 ° C) and the like are preferably used.
- the peroxide half-life is an index representing the decomposition rate of the peroxide, and means the time until the remaining amount of peroxide is reduced to half.
- the decomposition temperature for obtaining a half-life at an arbitrary time and the half-life time at an arbitrary temperature are described in the manufacturer catalog, for example, “Organic peroxide catalog 9th edition by Nippon Oil & Fats Co., Ltd.” (May 2003) ".
- the amount of the crosslinking agent (C) used is preferably 0.01 to 20 parts by weight, and more preferably 0.03 to 10 parts by weight with respect to 100 parts by weight of the (meth) acrylic polymer (A). If the crosslinking agent (C) is less than 0.01 parts by weight, the cohesive force of the pressure-sensitive adhesive tends to be insufficient, and foaming may occur during heating. On the other hand, if it exceeds 20 parts by weight, the moisture resistance is sufficient. Instead, peeling easily occurs in a reliability test or the like.
- the isocyanate-based crosslinking agent may be used singly or as a mixture of two or more, but the total content thereof is the (meth) acrylic polymer (A) 100
- the polyisocyanate compound crosslinking agent is preferably contained in an amount of 0.01 to 2 parts by weight, more preferably 0.02 to 2 parts by weight, and more preferably 0.05 to 1.5 parts by weight. More preferably, it is contained in parts by weight. It can be appropriately contained in consideration of cohesive force and prevention of peeling in a durability test.
- the peroxide may be used alone or as a mixture of two or more, but the total content is 100 weight of the (meth) acrylic polymer (A).
- the peroxide is 0.01 to 2 parts by weight, preferably 0.04 to 1.5 parts by weight, and more preferably 0.05 to 1 part by weight. . In order to adjust processability, reworkability, cross-linking stability, peelability, and the like, it is appropriately selected within this range.
- the peroxide decomposition amount remaining after the reaction treatment for example, it can be measured by HPLC (High Performance Liquid Chromatography).
- the pressure-sensitive adhesive composition after the reaction treatment is taken out, immersed in 10 ml of ethyl acetate, extracted by shaking at 25 ° C. and 120 rpm for 3 hours with a shaker, and then at room temperature. Leave for 3 days. Next, 10 ml of acetonitrile was added, shaken at 120 rpm at 25 ° C. for 30 minutes, and about 10 ⁇ l of the extract obtained by filtration through a membrane filter (0.45 ⁇ m) was injected into the HPLC for analysis. The amount of peroxide can be set.
- the pressure-sensitive adhesive composition of the present invention can contain a silane coupling agent (D).
- the durability can be improved by using the silane coupling agent (D).
- the silane coupling agent include 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 2- (3, Epoxy group-containing silane coupling agents such as 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-aminopropyltrimethoxysilane, N-2- (aminoethyl) -3-aminopropylmethyldimethoxysilane, 3-triethoxysilyl- Amino group-containing silane coupling agents such as N- (1,3-dimethylbutylidene) propylamine, N-phenyl- ⁇ -aminopropyltrimethoxysilane, 3-acryloxypropyltrimeth
- the silane coupling agent (D) may be used alone or as a mixture of two or more, but the total content thereof is the (meth) acrylic polymer (A) 100.
- the silane coupling agent is preferably 0.001 to 5 parts by weight, more preferably 0.01 to 1 part by weight, further preferably 0.02 to 1 part by weight, more preferably 0.05 to part by weight. ⁇ 0.6 parts by weight is preferred. It is an amount that improves durability and appropriately maintains the adhesive force to an optical member such as a liquid crystal cell.
- the pressure-sensitive adhesive composition of the present invention may contain other known additives, such as powders such as colorants and pigments, dyes, surfactants, plasticizers, tackifiers, Use surface lubricants, leveling agents, softeners, antioxidants, anti-aging agents, light stabilizers, UV absorbers, polymerization inhibitors, inorganic or organic fillers, metal powders, particles, foils, etc. It can be added appropriately depending on the application. Moreover, you may employ
- the pressure-sensitive adhesive composition forms a pressure-sensitive adhesive layer.
- it is necessary to fully consider the influence of the crosslinking treatment temperature and the crosslinking treatment time as well as adjusting the addition amount of the entire crosslinking agent. preferable.
- the crosslinking treatment temperature and crosslinking treatment time can be adjusted depending on the crosslinking agent used.
- the crosslinking treatment temperature is preferably 170 ° C. or lower.
- crosslinking treatment may be performed at the temperature during the drying step of the pressure-sensitive adhesive layer, or may be performed by providing a separate crosslinking treatment step after the drying step.
- the crosslinking treatment time can be set in consideration of productivity and workability, but is usually about 0.2 to 20 minutes, preferably about 0.5 to 10 minutes.
- the polarizing film with a pressure-sensitive adhesive layer of the present invention is one in which a pressure-sensitive adhesive layer is formed on at least one surface of the polarizing film with the pressure-sensitive adhesive composition.
- the pressure-sensitive adhesive layer for example, a method in which the pressure-sensitive adhesive composition is applied to a release-treated separator, and the polymerization solvent is dried and removed to form a pressure-sensitive adhesive layer, and then transferred to a polarizing film, or
- the pressure-sensitive adhesive composition is prepared by applying the pressure-sensitive adhesive composition to a polarizing film, drying and removing the polymerization solvent, and forming a pressure-sensitive adhesive layer on the polarizing film.
- one or more solvents other than the polymerization solvent may be added as appropriate.
- a silicone release liner is preferably used as the release-treated separator.
- a method for drying the pressure-sensitive adhesive is appropriately employed depending on the purpose. obtain.
- a method of heating and drying the coating film is used.
- the heating and drying temperature is preferably 40 ° C to 200 ° C, more preferably 50 ° C to 180 ° C, and particularly preferably 70 ° C to 170 ° C.
- the drying time is preferably 5 seconds to 20 minutes, more preferably 5 seconds to 10 minutes, and particularly preferably 10 seconds to 5 minutes.
- the pressure-sensitive adhesive layer can be formed after forming an anchor layer on the surface of the polarizing film or performing various easy adhesion treatments such as corona treatment and plasma treatment. Moreover, you may perform an easily bonding process on the surface of an adhesive layer.
- Various methods are used as a method for forming the pressure-sensitive adhesive layer. Specifically, for example, roll coat, kiss roll coat, gravure coat, reverse coat, roll brush, spray coat, dip roll coat, bar coat, knife coat, air knife coat, curtain coat, lip coat, die coater, etc. Examples thereof include an extrusion coating method.
- the thickness of the pressure-sensitive adhesive layer is not particularly limited, and is, for example, about 1 to 100 ⁇ m.
- the thickness is preferably 2 to 50 ⁇ m, more preferably 2 to 40 ⁇ m, and still more preferably 5 to 35 ⁇ m.
- the pressure-sensitive adhesive layer When the pressure-sensitive adhesive layer is exposed, the pressure-sensitive adhesive layer may be protected with a peeled sheet (separator) until practical use.
- constituent material of the separator examples include, for example, plastic films such as polyethylene, polypropylene, polyethylene terephthalate, and polyester films, porous materials such as paper, cloth, and nonwoven fabric, nets, foam sheets, metal foils, and laminates thereof.
- plastic films such as polyethylene, polypropylene, polyethylene terephthalate, and polyester films
- porous materials such as paper, cloth, and nonwoven fabric, nets, foam sheets, metal foils, and laminates thereof.
- a plastic film is used suitably from the point which is excellent in surface smoothness.
- the plastic film is not particularly limited as long as it can protect the pressure-sensitive adhesive layer.
- a polyethylene film, a polypropylene film, a polybutene film, a polybutadiene film, a polymethylpentene film, a polyvinyl chloride film, and a vinyl chloride co-polymer are used.
- examples thereof include a polymer film, a polyethylene terephthalate film, a polybutylene terephthalate film, a polyurethane film, and an ethylene-vinyl acetate copolymer film.
- the thickness of the separator is usually about 5 to 200 ⁇ m, preferably about 5 to 100 ⁇ m.
- mold release and antifouling treatment with a silicone type, fluorine type, long chain alkyl type or fatty acid amide type release agent, silica powder, etc., coating type, kneading type, vapor deposition type It is also possible to carry out antistatic treatment such as.
- the release property from the pressure-sensitive adhesive layer can be further improved by appropriately performing a release treatment such as silicone treatment, long-chain alkyl treatment, or fluorine treatment on the surface of the separator.
- seat which carried out the peeling process used in preparation of said polarizing film with an adhesive layer can be used as a separator of the polarizing film with an adhesive layer as it is, and can simplify in the surface of a process.
- a polarizing film having a transparent protective film on one side or both sides of a thin polarizer having a thickness of 10 ⁇ m or less is used.
- a thin polarizer having a thickness of 10 ⁇ m or less can be used.
- the thickness is preferably 1 to 7 ⁇ m.
- Such a thin polarizer is preferable in that the thickness unevenness is small, the visibility is excellent, the dimensional change is small, the durability is excellent, and the thickness of the polarizing film can be reduced.
- the polarizer is not particularly limited, and various types can be used.
- polarizers include dichroic iodine and dichroic dyes on hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene / vinyl acetate copolymer partially saponified films.
- hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene / vinyl acetate copolymer partially saponified films.
- examples thereof include polyene-based oriented films such as those obtained by adsorbing substances and uniaxially stretched, polyvinyl alcohol dehydrated products and polyvinyl chloride dehydrochlorinated products.
- a polarizer composed of a polyvinyl alcohol film and a dichroic material such as iodine is preferable.
- a polarizer obtained by dyeing a polyvinyl alcohol film with iodine and uniaxially stretching it can be prepared, for example, by dyeing a polyvinyl alcohol film in an aqueous solution of iodine and stretching it 3 to 7 times the original length. it can. If necessary, it can be immersed in an aqueous solution such as potassium iodide which may contain boric acid, zinc sulfate, zinc chloride or the like. Further, if necessary, the polyvinyl alcohol film may be immersed in water and washed before dyeing.
- Stretching may be performed after dyeing with iodine, may be performed while dyeing, or may be dyed with iodine after stretching.
- the film can be stretched even in an aqueous solution such as boric acid or potassium iodide or in a water bath.
- the thin polarizer typically, JP-A-51-069644, JP-A-2000-338329, WO2010 / 100917, PCT / JP2010 / 001460, or Japanese Patent Application No. 2010-
- the thin polarizing film (layer) described in the specification of 269002 and Japanese Patent Application No. 2010-263692 can be mentioned.
- These thin polarizing films can be obtained by a production method including a step of stretching a polyvinyl alcohol-based resin (hereinafter also referred to as PVA-based resin) layer and a stretching resin base material in a laminated state and a step of dyeing. With this manufacturing method, even if the PVA-based resin layer is thin, it can be stretched without problems such as breakage due to stretching by being supported by the stretching resin substrate.
- PVA-based resin polyvinyl alcohol-based resin
- the thin polarizing film among the production methods including the step of stretching in the state of a laminate and the step of dyeing, WO2010 / 100917 pamphlet, PCT / PCT / PCT / JP 2010/001460 specification, or Japanese Patent Application No. 2010-269002 and Japanese Patent Application No. 2010-263692, the one obtained by a production method including a step of stretching in a boric acid aqueous solution is preferable. What is obtained by the manufacturing method including the process of extending
- the thin high-performance polarizing film described in the specification of PCT / JP2010 / 001460 is a thin film having a thickness of 7 ⁇ m or less made of a PVA-based resin oriented with a dichroic material, which is integrally formed on a resin substrate. It is a high-functional polarizing film, and has optical properties such as a single transmittance of 42.0% or more and a degree of polarization of 99.95% or more.
- the thin high-performance polarizing film generates a PVA-based resin layer by applying and drying a PVA-based resin on a resin substrate having a thickness of at least 20 ⁇ m, and the generated PVA-based resin layer is used as a dichroic dyeing solution. So that the dichroic substance is adsorbed on the PVA resin layer, and the PVA resin layer on which the dichroic substance is adsorbed is integrated with the resin base material in the boric acid aqueous solution so that the total draw ratio is the original length. It can manufacture by extending
- a method for producing a laminate film including a thin high-performance polarizing film in which a dichroic substance is oriented and includes a resin base material having a thickness of at least 20 ⁇ m and a PVA resin on one side of the resin base material.
- the said laminated body containing the process of producing
- the polarizing film with the pressure-sensitive adhesive layer is a continuous web polarizing film made of a PVA resin in which a dichroic substance is oriented as a polarizer having a thickness of 10 ⁇ m or less, What was obtained by extending
- stretching process which consists of air auxiliary
- the thermoplastic resin substrate is preferably an amorphous ester thermoplastic resin substrate or a crystalline ester thermoplastic resin substrate.
- the thin polarizing films in the above-mentioned Japanese Patent Application Nos. 2010-269002 and 2010-263692 are continuous web polarizing films made of a PVA-based resin in which a dichroic material is oriented, and are amorphous.
- the laminate including the PVA-based resin layer formed on the ester-based thermoplastic resin base material was stretched in a two-stage stretching process consisting of air-assisted stretching and boric acid-water stretching, so that the thickness was 10 ⁇ m or less. Is.
- Such a thin polarizing film has P> ⁇ (10 0.929 T ⁇ 42.4 ⁇ 1) ⁇ 100 (where T ⁇ 42.3) and P ⁇ , where T is the single transmittance and P is the polarization degree. It is preferable that the optical properties satisfy 99.9 (where T ⁇ 42.3).
- the thin polarizing film is a stretch intermediate formed of an oriented PVA resin layer by high-temperature stretching in the air with respect to the PVA resin layer formed on the amorphous ester thermoplastic resin substrate of the continuous web.
- a colored intermediate product comprising a PVA-based resin layer in which a dichroic material (preferably iodine or a mixture of iodine and an organic dye) is oriented by adsorption of the dichroic material to the stretched intermediate product and a step of generating the product.
- a thin polarizing film comprising: a step of producing a product; and a step of producing a polarizing film having a thickness of 10 ⁇ m or less comprising a PVA resin layer in which a dichroic substance is oriented by stretching in a boric acid solution with respect to a colored intermediate product It can manufacture with the manufacturing method of.
- the total draw ratio of the PVA resin layer formed on the amorphous ester thermoplastic resin base material by high-temperature drawing in air and drawing in boric acid solution should be 5 times or more. desirable.
- stretching can be 60 degreeC or more.
- the colored intermediate product is added to the aqueous boric acid solution whose liquid temperature does not exceed 40 ° C. It is desirable to do so by dipping.
- the amorphous ester-based thermoplastic resin base material is amorphous polyethylene containing copolymerized polyethylene terephthalate copolymerized with isophthalic acid, copolymerized polyethylene terephthalate copolymerized with cyclohexanedimethanol, or other copolymerized polyethylene terephthalate. It can be terephthalate and is preferably made of a transparent resin, and the thickness thereof can be 7 times or more the thickness of the PVA resin layer to be formed.
- the draw ratio of high-temperature drawing in the air is preferably 3.5 times or less, and the drawing temperature of high-temperature drawing in the air is preferably not less than the glass transition temperature of the PVA resin, specifically in the range of 95 ° C to 150 ° C.
- the total stretching ratio of the PVA resin layer formed on the amorphous ester thermoplastic resin base material is preferably 5 to 7.5 times .
- the total stretching ratio of the PVA-based resin layer formed on the amorphous ester-based thermoplastic resin base material is 5 times or more and 8.5 times or less. Is preferred. More specifically, a thin polarizing film can be produced by the following method.
- a base material for a continuous web of isophthalic acid copolymerized polyethylene terephthalate (amorphous PET) in which 6 mol% of isophthalic acid is copolymerized is prepared.
- the glass transition temperature of amorphous PET is 75 ° C.
- a laminate comprising a continuous web of amorphous PET substrate and a polyvinyl alcohol (PVA) layer is prepared as follows. Incidentally, the glass transition temperature of PVA is 80 ° C.
- a 200 ⁇ m-thick amorphous PET base material and a 4-5% PVA aqueous solution in which PVA powder having a polymerization degree of 1000 or more and a saponification degree of 99% or more are dissolved in water are prepared.
- an aqueous PVA solution is applied to a 200 ⁇ m thick amorphous PET substrate and dried at a temperature of 50 to 60 ° C. to obtain a laminate in which a 7 ⁇ m thick PVA layer is formed on the amorphous PET substrate. .
- a thin and highly functional polarizing film having a thickness of 3 ⁇ m is manufactured from the laminate including the PVA layer having a thickness of 7 ⁇ m through the following steps including a two-stage stretching process of air-assisted stretching and boric acid water stretching.
- the laminate including the 7 ⁇ m-thick PVA layer is integrally stretched with the amorphous PET substrate to produce a stretched laminate including the 5 ⁇ m-thick PVA layer.
- a laminate including a 7 ⁇ m-thick PVA layer is subjected to a stretching apparatus disposed in an oven set to a stretching temperature environment of 130 ° C. so that the stretching ratio is 1.8 times. Are stretched uniaxially at the free end.
- the PVA layer contained in the stretched laminate is changed to a 5 ⁇ m thick PVA layer in which PVA molecules are oriented.
- this colored laminate has a single layer transmittance of the PVA layer constituting the high-performance polarizing film that is finally produced by using the stretched laminate in a staining solution containing iodine and potassium iodide at a liquid temperature of 30 ° C.
- Iodine is adsorbed to the PVA layer contained in the stretched laminate by dipping for an arbitrary period of time so as to be 40 to 44%.
- the staining solution uses water as a solvent, and an iodine concentration within the range of 0.12 to 0.30% by weight and a potassium iodide concentration within the range of 0.7 to 2.1% by weight.
- concentration ratio of iodine and potassium iodide is 1 to 7.
- potassium iodide is required to dissolve iodine in water. More specifically, by immersing the stretched laminate in a dyeing solution having an iodine concentration of 0.30% by weight and a potassium iodide concentration of 2.1% by weight for 60 seconds, iodine is applied to a 5 ⁇ m-thick PVA layer in which PVA molecules are oriented. A colored laminate is adsorbed on the substrate.
- the colored laminated body is further stretched integrally with the amorphous PET base material by the second stage boric acid underwater stretching step to produce an optical film laminate including a PVA layer constituting a highly functional polarizing film having a thickness of 3 ⁇ m.
- the optical film laminate is subjected to stretching by applying the colored laminate to a stretching apparatus provided in a treatment apparatus set to a boric acid aqueous solution having a liquid temperature range of 60 to 85 ° C. containing boric acid and potassium iodide. It is stretched uniaxially at the free end so that the magnification is 3.3 times. More specifically, the liquid temperature of the boric acid aqueous solution is 65 ° C.
- the colored laminate having an adjusted iodine adsorption amount is first immersed in an aqueous boric acid solution for 5 to 10 seconds. After that, the colored laminate is passed as it is between a plurality of sets of rolls with different peripheral speeds, which is a stretching apparatus installed in the processing apparatus, and the stretching ratio can be freely increased to 3.3 times over 30 to 90 seconds. Stretch uniaxially.
- the PVA layer contained in the colored laminate is changed into a PVA layer having a thickness of 3 ⁇ m in which the adsorbed iodine is oriented higher in one direction as a polyiodine ion complex.
- This PVA layer constitutes a highly functional polarizing film of the optical film laminate.
- the optical film laminate was removed from the boric acid aqueous solution and adhered to the surface of the 3 ⁇ m-thick PVA layer formed on the amorphous PET substrate by the washing step. It is preferable to wash boric acid with an aqueous potassium iodide solution. Thereafter, the washed optical film laminate is dried by a drying process using hot air at 60 ° C.
- the cleaning process is a process for eliminating appearance defects such as boric acid precipitation.
- an adhesive is applied to the surface of a 3 ⁇ m-thick PVA layer formed on an amorphous PET substrate by a bonding and / or transfer process.
- the amorphous PET substrate can be peeled off, and the 3 ⁇ m thick PVA layer can be transferred to the 80 ⁇ m thick triacetyl cellulose film.
- the manufacturing method of said thin-shaped polarizing film may include another process other than the said process.
- Examples of other steps include an insolubilization step, a crosslinking step, and a drying (adjustment of moisture content) step.
- the other steps can be performed at any appropriate timing.
- the insolubilization step is typically performed by immersing the PVA resin layer in a boric acid aqueous solution. By performing the insolubilization treatment, water resistance can be imparted to the PVA resin layer.
- the concentration of the boric acid aqueous solution is preferably 1 to 4 parts by weight with respect to 100 parts by weight of water.
- the liquid temperature of the insolubilizing bath (boric acid aqueous solution) is preferably 20 ° C.
- the insolubilization step is performed after the laminate is manufactured and before the dyeing step and the underwater stretching step.
- the crosslinking step is typically performed by immersing the PVA resin layer in an aqueous boric acid solution.
- the concentration of the boric acid aqueous solution is preferably 1 to 4 parts by weight with respect to 100 parts by weight of water.
- blend iodide it is preferable to mix
- the blending amount of iodide is preferably 1 to 5 parts by weight with respect to 100 parts by weight of water. Specific examples of the iodide are as described above.
- the liquid temperature of the crosslinking bath is preferably 20 ° C. to 50 ° C.
- the crosslinking step is performed before the second boric acid aqueous drawing step.
- the dyeing step, the crosslinking step, and the second boric acid aqueous drawing step are performed in this order.
- thermoplastic resin excellent in transparency, mechanical strength, thermal stability, moisture barrier property, isotropy and the like is used.
- thermoplastic resins include cellulose resins such as triacetyl cellulose, polyester resins, polyethersulfone resins, polysulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, (meth) acrylic resins, cyclic Examples thereof include polyolefin resins (norbornene resins), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof.
- One or more kinds of arbitrary appropriate additives may be contained in the transparent protective film.
- the additive examples include an ultraviolet absorber, an antioxidant, a lubricant, a plasticizer, a mold release agent, an anti-coloring agent, a flame retardant, a nucleating agent, an antistatic agent, a pigment, and a coloring agent.
- the content of the thermoplastic resin in the transparent protective film is preferably 50 to 100% by weight, more preferably 50 to 99% by weight, still more preferably 60 to 98% by weight, and particularly preferably 70 to 97% by weight. .
- content of the said thermoplastic resin in a transparent protective film is 50 weight% or less, there exists a possibility that the high transparency etc. which a thermoplastic resin originally has cannot fully be expressed.
- An adhesive is used for the adhesion treatment between the polarizer and the transparent protective film.
- the adhesive include isocyanate adhesives, polyvinyl alcohol adhesives, gelatin adhesives, vinyl latexes, and water-based polyesters.
- the adhesive is usually used as an adhesive made of an aqueous solution, and usually contains 0.5 to 60% by weight of a solid content.
- examples of the adhesive between the polarizer and the transparent protective film include an ultraviolet curable adhesive and an electron beam curable adhesive.
- the electron beam curable polarizing film adhesive exhibits suitable adhesiveness to the various transparent protective films.
- the adhesive used in the present invention can contain a metal compound filler.
- the polarizing film can be laminated with other optical films.
- other optical films include the formation of liquid crystal display devices such as reflectors, anti-transmission plates, retardation films (including wavelength plates such as 1/2 and 1/4), visual compensation films, and brightness enhancement films.
- the thing used as the optical layer which may be used is mentioned. These can be laminated on the polarizing film for practical use, and one layer or two or more layers can be used.
- An optical film obtained by laminating the optical layer on a polarizing film can be formed by a method of laminating separately sequentially in the manufacturing process of a liquid crystal display device or the like.
- an appropriate adhesive means such as an adhesive layer can be used for the lamination.
- the polarizing film with an adhesive layer of the present invention can be preferably used for forming various image display devices such as a liquid crystal display device.
- the liquid crystal display device can be formed according to the conventional method. That is, the liquid crystal display device is generally formed by appropriately assembling components such as a display panel such as a liquid crystal cell, a polarizing film with an adhesive layer, and an illumination system as required, and incorporating a drive circuit.
- a display panel such as a liquid crystal cell
- a polarizing film with an adhesive layer such as a liquid crystal cell
- an illumination system as required
- As the liquid crystal cell an arbitrary type such as an arbitrary type such as a TN type, STN type, ⁇ type, VA type, or IPS type can be used.
- liquid crystal display devices such as a liquid crystal display device in which a polarizing film with an adhesive layer is disposed on one or both sides of a display panel such as a liquid crystal cell, or a lighting system using a backlight or a reflecting plate can be formed.
- the polarizing film with an adhesive layer by this invention can be installed in the one side or both sides of display panels, such as a liquid crystal cell.
- optical films are provided on both sides, they may be the same or different.
- a liquid crystal display device for example, a single layer or a suitable layer such as a diffusion layer, an antiglare layer, an antireflection film, a protective plate, a prism array, a lens array sheet, a light diffusion sheet, a backlight, etc. Two or more layers can be arranged.
- a laminated body in which a PVA layer having a thickness of 9 ⁇ m is formed on an amorphous PET substrate is produced by air-assisted stretching at a stretching temperature of 130 ° C., and then stretched.
- a colored laminate is produced by dyeing the laminate, and the colored laminate is further stretched integrally with an amorphous PET substrate so that the total draw ratio is 5.94 times by stretching in boric acid water at a stretching temperature of 65 degrees.
- An optical film laminate including a 4 ⁇ m thick PVA layer was produced.
- the PVA molecules in the PVA layer formed on the amorphous PET substrate by such two-stage stretching are oriented in the higher order, and the iodine adsorbed by the dyeing is oriented in the one direction as the polyiodine ion complex. It was possible to produce an optical film laminate including a PVA layer having a thickness of 4 ⁇ m and constituting a highly functional polarizing film.
- a thin polarizing film (1) After applying the polyvinyl alcohol adhesive to the surface of the polarizing film of the optical film laminate, after laminating the saponified 40 ⁇ m thick triacetyl cellulose film, after peeling the amorphous PET substrate, A norbornene-based film having a thickness of 33 ⁇ m was bonded to the other surface with a polyvinyl alcohol-based adhesive, thereby producing a polarizing film using a thin polarizing film.
- this is referred to as a thin polarizing film (1).
- ⁇ Creation of polarizing film (2)> A polyvinyl alcohol film having a thickness of 80 ⁇ m was stretched up to 3 times while being dyed for 1 minute in an iodine solution of 0.3% concentration at 30 ° C. between rolls having different speed ratios. Thereafter, the total draw ratio was stretched to 6 times while being immersed in an aqueous solution containing 60% at 4% concentration of boric acid and 10% concentration of potassium iodide for 0.5 minutes. Next, after washing by immersing in an aqueous solution containing potassium iodide at 30 ° C. and 1.5% concentration for 10 seconds, drying was performed at 50 ° C. for 4 minutes to obtain a polarizer having a thickness of 20 ⁇ m.
- a polarizing film was prepared by laminating a saponified 40 ⁇ m thick triacetyl cellulose film on both sides of the polarizer and a 33 ⁇ m thick norbornene film on the other side with a polyvinyl alcohol adhesive.
- TAC polarizing film (2) a polarizing film
- Production Example 2 ⁇ Preparation of acrylic polymer (A-2)>
- a monomer mixture containing 76.8 parts of butyl acrylate, 10 parts of benzyl acrylate, 10 parts of phenoxyethyl acrylate, 3 parts of 4-hydroxybutyl acrylate and 0.2 part of acrylic acid was used as the monomer mixture. Except for the above, a solution of an acrylic polymer (A-2) having a weight average molecular weight of 1,000,000 was prepared in the same manner as in Production Example 1.
- Example 1 (Preparation of adhesive composition) To 100 parts of the solid content of the acrylic polymer (A-1) solution obtained in Production Example 1, 0.002 part of lithium bis (trifluoromethanesulfonyl) imide (manufactured by Nippon Carlit) was blended. 0.1 part of methylolpropane xylylene diisocyanate (Mitsui Chemical Co., Ltd .: Takenate D110N), 0.3 part of dibenzoyl peroxide, and ⁇ -glycidoxypropylmethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd .: KBM-403) 0 0.075 parts was blended to prepare an acrylic pressure-sensitive adhesive solution.
- methylolpropane xylylene diisocyanate Mitsubishi Chemical Co., Ltd .: Takenate D110N
- dibenzoyl peroxide 0.3 part of dibenzoyl peroxide
- the acrylic pressure-sensitive adhesive solution is uniformly applied to the surface of a polyethylene terephthalate film (separator film) treated with a silicone-based release agent with a fountain coater and dried in an air circulation type thermostatic oven at 155 ° C. for 2 minutes. Then, an adhesive layer having a thickness of 20 ⁇ m was formed on the surface of the separator film. Next, the pressure-sensitive adhesive layer formed on the separator film was transferred to the norbornene-based film side of the thin polarizing film (1) prepared above to produce a polarizing film with a pressure-sensitive adhesive layer.
- Example 2 Comparative Examples 1 to 8
- the amount of each component used was changed as shown in Table 1 in the preparation of the pressure-sensitive adhesive composition, and the type of polarizing film was changed as shown in Table 1 in preparing the polarizing film with the pressure-sensitive adhesive layer.
- a polarizing film with an adhesive layer was produced in the same manner as in Example 1 except that.
- B-1 is lithium bis (trifluoromethanesulfonyl) imide manufactured by Nippon Carlit
- B-2 lithium perchlorate manufactured by Nippon Carlit
- B -3 is 1-hexyl-4-methylpyridinium hexafluorophosphate manufactured by Kanto Chemical Co., Inc.
- B-4 is 1-methyl-1-propylpyrrolidinium bis (trifluoromethanesulfonyl) imide
- B- “5” represents trimethylbutylammonium bis (trifluoromethanesulfonyl) imide.
- C-1 is an isocyanate cross-linking agent (Takenate D110N, trimethylolpropane xylylene diisocyanate) manufactured by Mitsui Takeda Chemical Co.
- C-2 is a benzoyl peroxide (Nyper) manufactured by NOF Corporation. BMT).
- D-1 in the silane coupling agent (D) represents KBM403 manufactured by Shin-Etsu Chemical Co., Ltd.
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Abstract
Description
前記偏光フィルムは、厚みが10μm以下の偏光子の片側または両側に透明保護フィルムを有し、かつ
前記粘着剤層は、(メタ)アクリル系ポリマー(A)およびイオン性化合物(B)を含有する粘着剤組成物から形成されたものであることを特徴とする粘着剤層付偏光フィルム、に関する。
アルカリ金属塩のカチオン部を構成するアルカリ金属イオンとしては、リチウム、ナトリウム、カリウムの各イオンが挙げられる。これらアルカリ金属イオンのなかでもリチウムイオンが好ましい。
(1):(CnF2n+1SO2)2N- (但し、nは1~10の整数)、
(2):CF2(CmF2mSO2)2N- (但し、mは1~10の整数)、
(3):-O3S(CF2)lSO3 - (但し、lは1~10の整数)、
(4):(CpF2p+1SO2)N-(CqF2q+1SO2)、(但し、p、qは1~10の整数)、で表わされるものなどが用いられる。特に、フッ素原子を含むアニオン部は、イオン解離性の良いイオン化合物が得られることから好ましく用いられる。無機塩を構成するアニオン部としては、Cl-、Br-、I-、AlCl4 -、Al2Cl7 -、BF4 -、PF6 -、ClO4 -、NO3 -、AsF6 -、SbF6 -、NbF6 -、TaF6 -、(CN)2N-、などが用いられる。アニオン部としては、(CF3SO2)2N-、(C2F5SO2)2N-、等の前記一般式(1)で表わされる、(ペルフルオロアルキルスルホニル)イミドが好ましく、特に(CF3SO2)2N-、で表わされる(トリフルオロメタンスルホニル)イミドが好ましい。
本発明で用いられる有機カチオン-アニオン塩は、カチオン成分とアニオン成分とから構成されており、前記カチオン成分は有機物からなるものである。カチオン成分として、具体的には、ピリジニウムカチオン、ピペリジニウムカチオン、ピロリジニウムカチオン、ピロリン骨格を有するカチオン、ピロール骨格を有するカチオン、イミダゾリウムカチオン、テトラヒドロピリミジニウムカチオン、ジヒドロピリミジニウムカチオン、ピラゾリウムカチオン、ピラゾリニウムカチオン、テトラアルキルアンモニウムカチオン、トリアルキルスルホニウムカチオン、テトラアルキルホスホニウムカチオンなどが挙げられる。
(1):(CnF2n+1SO2)2N- (但し、nは1~10の整数)、
(2):CF2(CmF2mSO2)2N- (但し、mは1~10の整数)、
(3):-O3S(CF2)lSO3 - (但し、lは1~10の整数)、
(4):(CpF2p+1SO2)N-(CqF2q+1SO2)、(但し、p、qは1~10の整数)、で表わされるものなどが用いられる。なかでも特に、フッ素原子を含むアニオン成分は、イオン解離性の良いイオン化合物が得られることから好ましく用いられる。
例えば、1-ブチルピリジニウムテトラフルオロボレート、1-ブチルピリジニウムヘキサフルオロホスフェート、1-ブチル-3-メチルピリジニウムテトラフルオロボレート、1-ブチル-3-メチルピリジニウムトリフルオロメタンスルホネート、1-ブチル-3-メチルピリジニウムビス(トリフルオロメタンスルホニル)イミド、1-ブチル-3-メチルピリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-へキシルピリジニウムテトラフルオロボレート、2-メチル-1-ピロリンテトラフルオロボレート、1-エチル-2-フェニルインドールテトラフルオロボレート、1,2-ジメチルインドールテトラフルオロボレート、1-エチルカルバゾールテトラフルオロボレート、1-エチル-3-メチルイミダゾリウムテトラフルオロボレート、1-エチル-3-メチルイミダゾリウムアセテート、1-エチル-3-メチルイミダゾリウムトリフルオロアセテート、1-エチル-3-メチルイミダゾリウムヘプタフルオロブチレート、1-エチル-3-メチルイミダゾリウムトリフルオロメタンスルホネート、1-エチル-3-メチルイミダゾリウムペルフルオロブタンスルホネート、1-エチル-3-メチルイミダゾリウムジシアナミド、1-エチル-3-メチルイミダゾリウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-3-メチルイミダゾリウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-3-メチルイミダゾリウムトリス(トリフルオロメタンスルホニル)メチド、1-ブチル-3-メチルイミダゾリウムテトラフルオロボレート、1-ブチル-3-メチルイミダゾリウムヘキサフルオロホスフェート、1-ブチル-3-メチルイミダゾリウムトリフルオロアセテート、1-ブチル-3-メチルイミダゾリウムヘプタフルオロブチレート、1-ブチル-3-メチルイミダゾリウムトリフルオロメタンスルホネート、1-ブチル-3-メチルイミダゾリウムペルフルオロブタンスルホネート、1-ブチル-3-メチルイミダゾリウムビス(トリフルオロメタンスルホニル)イミド、1-へキシル-3-メチルイミダゾリウムブロミド、1-へキシル-3-メチルイミダゾリウムクロライド、1-へキシル-3-メチルイミダゾリウムテトラフルオロボレート、1-へキシル-3-メチルイミダゾリウムヘキサフルオロホスフェート、1-へキシル-3-メチルイミダゾリウムトリフルオロメタンスルホネート、1-オクチル-3-メチルイミダゾリウムテトラフルオロボレート、1-オクチル-3-メチルイミダゾリウムヘキサフルオロホスフェート、1-へキシル-2,3-ジメチルイミダゾリウムテトラフルオロボレート、1,2-ジメチル-3-プロピルイミダゾリウムビス(トリフルオロメタンスルホニル)イミド、1-メチルピラゾリウムテトラフルオロボレート、3-メチルピラゾリウムテトラフルオロボレート、テトラヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、ジアリルジメチルアンモニウムテトラフルオロボレート、ジアリルジメチルアンモニウムトリフルオロメタンスルホネート、ジアリルジメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、ジアリルジメチルアンモニウムビス(ペンタフルオロエタンスルホニル)イミド、N,N―ジエチル―N―メチル―N-(2-メトキシエチル)アンモニウムテトラフルオロボレート、N,N―ジエチル―N―メチル―N-(2-メトキシエチル)アンモニウムトリフルオロメタンスルホネート、N,N―ジエチル―N―メチル―N-(2-メトキシエチル)アンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N―ジエチル―N―メチル―N-(2-メトキシエチル)アンモニウムビス(ペンタフルオロエタンスルホニル)イミド、グリシジルトリメチルアンモニウムトリフルオロメタンスルホネート、グリシジルトリメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、グリシジルトリメチルアンモニウムビス(ペンタフルオロエタンスルホニル)イミド、1-ブチルピリジニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、1-ブチル-3-メチルピリジニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、1-エチル-3-メチルイミダゾリウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、N,N―ジエチル―N―メチル―N-(2-メトキシエチル)アンモニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、ジアリルジメチルアンモニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、グリシジルトリメチルアンモニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、N,N-ジメチル-N-エチル-N-プロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-エチル-N-ブチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-エチル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-エチル-N-へキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-エチル-N-ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-エチル-N-ノニルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N,N-ジプロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-プロピル-N-ブチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-プロピル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-プロピル-N-ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-プロピル-N-ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-ブチル-N-ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-ブチル-N-ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N-ペンチル-N-ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジメチル-N,N-ジヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリメチルヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジエチル-N-メチル-N-プロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジエチル-N-メチル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジエチル-N-メチル-N-ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジエチル-N-プロピル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルプロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジプロピル-N-メチル-N-エチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジプロピル-N-メチル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジプロピル-N-ブチル-N-へキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジプロピル-N,N-ジヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジブチル-N-メチル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N-ジブチル-N-メチル-N-ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリオクチルメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N-メチル-N-エチル-N-プロピル-N-ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、1-ブチル-3-メチルピリジン-1-イウムトリフルオロメタンスルホナートなどが挙げられる。これらの市販品として、例えば、「CIL-314」(日本カーリット社製)、「ILA2-1」(広栄化学社製)などが使用可能である。
また、例えば、テトラメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリメチルエチルビス(トリフルオロメタンスルホニル)イミド、トリメチルブチルビス(トリフルオロメタンスルホニル)イミド、トリメリメルペンチルビス(トリフルオロメタンスルホニル)イミド、トリメチルヘプチルビス(トリフルオロメタンスルホニル)イミド、トリメチルオクチルビス(トリフルオロメタンスルホニル)イミド、テトラエチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルブチルビス(トリフルオロメタンスルホニル)イミド、テトラブチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、テトラヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、などが挙げられる。
また、例えば、1-ジメチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-エチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-プロピルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-ブチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-ペンチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-ヘキシルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-へプチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-プロピルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-ブチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-ペンチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-へキシルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-へプチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1,1-ジプロピルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-プロピル-1-ブチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1,1-ジブチルピロリジニウムビス(トリフルオロメタンスルホニル)イミド、1-プロピルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-ペンチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1,1-ジメチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-エチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1―プロピルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-ブチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-ペンチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-ヘキシルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-メチル-1-へプチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-プロピルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-ブチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-ペンチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-エチル-1-ヘキシルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1―エチル-1-ヘプチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1,1-ジプロピルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1-プロピル-1-ブチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1,1-ジブチルピペリジニウムビス(トリフルオロメタンスルホニル)イミド、1,1-ジメチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-エチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-プロピルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1―ブチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-ペンチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-ヘキシルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1―へプチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-プロピルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-ブチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-ペンチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-ヘキシルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-へプチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1,1-ジプロピルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1―プロピル-1-ブチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1,1-ジブチルピロリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-プロピルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-ペンチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1,1-ジメチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル‐1-エチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-プロピルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-ブチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-ペンチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1-ヘキシルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-メチル-1へプチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-プロピルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-ヘプチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド,1-エチル-1-ペンチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-エチル-1-ヘキシルピペリジニウムビス(ペンタフルオロエタンスルポニル)イミド、1-エチル-1-へプチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1-プロピル-1-ブチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1,1-ジプロピルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミド、1,1―ジブチルピペリジニウムビス(ペンタフルオロエタンスルホニル)イミドなどが挙げられる。
また、上記化合物のカチオン成分の代わりに、トリメチルスルホニウムカチオン、トリエチルスルホニウムカチオン、トリブチルスルホニウムカチオン、トリヘキシルスルホニウムカチオン、ジエチルメチルスルホニウムカチオン、ジブチルエチルスルホニウムカチオン、ジメチルデシルスルホニウムカチオン、テトラメチルホスホニウムカチオン、テトラエチルホスホニウムカチオン、テトラブチルホスホニウムカチオン、テトラヘキシルホスホニウムカチオンを用いた化合物などが挙げられる。
また、上記のビス(トリフルオロメタンスルホニル)イミドの代わりに、ビス(ペンタフルオロスルホニル)イミド、ビス(ヘプタフルオロプロパンスルホニル)イミド、ビス(ノナフルオロブタンスルホニル)イミド、トリフルオロメタンスルホニルノナフルオロブタンスルホニルイミド、ヘプタフルオロプロパンスルホニルトリフルオロメタンスルホニルイミド、ペンタフルオロエタンスルホニルノナフルオロブタンスルホニルイミド、シクロ-ヘキサフルオロプロパン-1,3-ビス(スルホニル)イミドアニオンなどを用いた化合物などが挙げられる。
更に具体的には、次のような方法により、薄型偏光膜を製造することができる。
上記の薄型偏光膜の製造方法は、上記工程以外に、その他の工程を含み得る。その他の工程としては、例えば、不溶化工程、架橋工程、乾燥(水分率の調節)工程等が挙げられる。その他の工程は、任意の適切なタイミングで行い得る。
上記不溶化工程は、代表的には、ホウ酸水溶液にPVA系樹脂層を浸漬させることにより行う。不溶化処理を施すことにより、PVA系樹脂層に耐水性を付与することができる。当該ホウ酸水溶液の濃度は、水100重量部に対して、好ましくは1重量部~4重量部である。不溶化浴(ホウ酸水溶液)の液温は、好ましくは20℃~50℃である。好ましくは、不溶化工程は、積層体作製後、染色工程や水中延伸工程の前に行う。
上記架橋工程は、代表的には、ホウ酸水溶液にPVA系樹脂層を浸漬させることにより行う。架橋処理を施すことにより、PVA系樹脂層に耐水性を付与することができる。当該ホウ酸水溶液の濃度は、水100重量部に対して、好ましくは1重量部~4重量部である。また、上記染色工程後に架橋工程を行う場合、さらに、ヨウ化物を配合することが好ましい。ヨウ化物を配合することにより、PVA系樹脂層に吸着させたヨウ素の溶出を抑制することができる。ヨウ化物の配合量は、水100重量部に対して、好ましくは1重量部~5重量部である。ヨウ化物の具体例は、上述のとおりである。架橋浴(ホウ酸水溶液)の液温は、好ましくは20℃~50℃である。好ましくは、架橋工程は上記第2のホウ酸水中延伸工程の前に行う。好ましい実施形態においては、染色工程、架橋工程および第2のホウ酸水中延伸工程をこの順で行う。
(メタ)アクリル系ポリマー(A)の重量平均分子量は、GPC(ゲル・パーミエーション・クロマトグラフィー)により測定した。
・分析装置:東ソー社製、HLC-8120GPC
・カラム:東ソー社製、G7000HXL+GMHXL+GMHXL
・カラムサイズ:各7.8mmφ×30cm 計90cm
・カラム温度:40℃
・流量:0.8ml/min
・注入量:100μl
・溶離液:テトラヒドロフラン
・検出器:示差屈折計(RI)
・標準試料:ポリスチレン
薄型偏光膜を作製するため、まず、非晶性PET基材に9μm厚のPVA層が製膜された積層体を延伸温度130℃の空中補助延伸によって延伸積層体を生成し、次に、延伸積層体を染色によって着色積層体を生成し、さらに着色積層体を延伸温度65度のホウ酸水中延伸によって総延伸倍率が5.94倍になるように非晶性PET基材と一体に延伸された4μm厚のPVA層を含む光学フィルム積層体を生成した。このような2段延伸によって非晶性PET基材に製膜されたPVA層のPVA分子が高次に配向され、染色によって吸着されたヨウ素がポリヨウ素イオン錯体として一方向に高次に配向された高機能偏光膜を構成する、厚さ4μmのPVA層を含む光学フィルム積層体を生成することができた。更に、当該光学フィルム積層体の偏光膜の表面にポリビニルアルコール系接着剤を塗布しながら、けん化処理した40μm厚のトリアセチルセルロースフィルムを貼合せたのち、非晶性PET基材を剥離した後、他の片面に厚さ33μmのノルボルネン系フィルムを、それぞれ、ポリビニルアルコール系接着剤により貼り合せて、薄型偏光膜を用いた偏光フィルムを作製した。以下、これを薄型偏光フィルム(1)という。
厚さ80μmのポリビニルアルコールフィルムを、速度比の異なるロール間において、30℃、0.3%濃度のヨウ素溶液中で1分間染色しながら、3倍まで延伸した。その後、60℃、4%濃度のホウ酸、10%濃度のヨウ化カリウムを含む水溶液中に0.5分間浸漬しながら総合延伸倍率が6倍まで延伸した。次いで、30℃、1.5%濃度のヨウ化カリウムを含む水溶液中に10秒間浸漬することで洗浄した後、50℃で4分間乾燥を行い、厚さ20μmの偏光子を得た。当該偏光子の両面に、けん化処理した厚さ40μmのトリアセチルセルロースフィルムを、他の片面に厚さ33μmのノルボルネン系フィルムを、それぞれ、ポリビニルアルコール系接着剤により貼り合せて偏光フィルムを作成した。以下、これをTAC系偏光フィルム(2)という。
<アクリル系ポリマー(A-1)の調製>
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート82部、ベンジルアクリレート15部、4-ヒドロキシブチルアクリレート3部を含有するモノマー混合物を仕込んだ。さらに、前記モノマー混合物(固形分)100部に対して、重合開始剤として2,2’-アゾビスイソブチロニトリル0.1部を酢酸エチルと共に仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を60℃付近に保って7時間重合反応を行った。その後、得られた反応液に、酢酸エチルを加えて、固形分濃度30%に調整した、重量平均分子量100万のアクリル系ポリマー(A-1)の溶液を調製した。
<アクリル系ポリマー(A-2)の調製>
製造例1において、モノマー混合物として、ブチルアクリレート76.8部、ベンジルアクリレート10部、フェノキシエチルアクリレート10部、4-ヒドロキシブチルアクリレート3部およびアクリル酸0.2部を含有するモノマー混合物を用いたこと以外は、製造例1と同様にして、重量平均分子量100万のアクリル系ポリマー(A-2)の溶液を調製した。
(粘着剤組成物の調製)
製造例1で得られたアクリル系ポリマー(A-1)溶液の固形分100部に対して、リチウムビス(トリフルオロメタンスルホニル)イミド(日本カーリット社製)0.002部を配合し、さらに、トリメチロールプロパンキシリレンジイソシアネート(三井化学社製:タケネートD110N)0.1部と、ジベンゾイルパーオキサイド0.3部と、γ-グリシドキシプロピルメトキシシラン(信越化学工業社製:KBM-403)0.075部を配合して、アクリル系粘着剤溶液を調製した。
次いで、上記アクリル系粘着剤溶液を、シリコーン系剥離剤で処理されたポリエチレンテレフタレートフィルム(セパレータフィルム)の表面に、ファウンテンコータで均一に塗工し、155℃の空気循環式恒温オーブンで2分間乾燥し、セパレータフィルムの表面に厚さ20μmの粘着剤層を形成した。次いで、上記で作成した薄型偏光フィルム(1)のノルボルネン系フィルムの側に、セパレータフィルム上に形成した粘着剤層を転写して、粘着剤層付偏光フィルムを作製した。
実施例1において、粘着剤組成物の調製にあたり、各成分の使用量を表1に示すように変えたこと、粘着剤層付偏光フィルムの作製にあたり偏光フィルムの種類を表1に示すように変えたこと以外は、実施例1と同様にして、粘着剤層付偏光フィルムを作製した。
粘着剤層付偏光フィルムのセパレータフィルムを剥がした後、粘着剤表面の表面抵抗値(Ω/□)を三菱化学アナリテック社製MCP-HT450を用いて測定した。
作製された粘着剤層付偏光フィルムを100mm×100mmの大きさに切断し、液晶パネルに貼り付けた。このパネルを10000cdの輝度を持つバックライト上に置き、静電気発生装置であるESD(SANKI社製,ESD-8012A)を用いて5kvの静電気を発生させることで液晶の配向乱れを起こした。その配向不良による表示不良の回復時間(秒)を、瞬間マルチ測光検出器(大塚電子社製,MCPD-3000)を用いて測定し、下記基準で評価した。
◎:表示不良が1秒未満で消失した。
○:表示不良が1秒以上10秒未満で消失した。
×:表示不良が10秒以上で消失した。
粘着剤層付偏光フィルムのセパレータフィルムを剥がし、厚さ0.7mmの無アルカリガラス(コーニング社製,1737)にラミネーターを用いて貼着した。次いで、50℃、0.5MPaで、15分間のオートクレーブ処理を行って、上記粘着剤層付偏光フィルムを完全に無アルカリガラスに密着させた。次いで、これを、80℃の加熱オーブン(加熱)および60℃/90%RHの恒温恒湿機(加湿)の条件下にそれぞれ投入して、500時間後の偏光フィルムの剥がれの有無を、下記基準で評価した。
◎:全く剥がれが認められなかった。
○:目視では確認できない程度の剥がれが認められた。
△:目視で確認できる小さな剥がれが認められた。
×:明らかな剥がれが認められた。
架橋剤(C)における、「C-1」は三井武田ケミカル社製のイソシアネート架橋剤(タケネートD110N,トリメチロールプロパンキシリレンジイソシアネート)、「C-2」は日本油脂社製のベンゾイルパーオキサイド(ナイパーBMT)、を示す。
シランカップリング剤(D)における「D-1」は信越化学工業社製のKBM403を示す。
Claims (13)
- 偏光フィルムと、当該偏光フィルムに設けられた粘着剤層を有する粘着剤層付偏光フィルムであって、
前記偏光フィルムは、厚みが10μm以下の偏光子の片側または両側に透明保護フィルムを有し、かつ
前記粘着剤層は、(メタ)アクリル系ポリマー(A)およびイオン性化合物(B)を含有する粘着剤組成物から形成されたものであることを特徴とする粘着剤層付偏光フィルム。 - 厚みが10μm以下の偏光子が、二色性物質を配向させたポリビニルアルコール系樹脂からなる連続ウェブの偏光膜であって、熱可塑性樹脂基材に製膜されたポリビニルアルコール系樹脂層を含む積層体が空中補助延伸とホウ酸水中延伸とからなる2段延伸工程で延伸されることにより得られたものであることを特徴とする請求項1記載の粘着剤層付偏光フィルム。
- イオン性化合物(B)が、アルカリ金属塩及び/または有機カチオン-アニオン塩であることを特徴とする請求項1または2記載の粘着剤層付偏光フィルム。
- (メタ)アクリル系ポリマー(A)100重量部に対して、イオン性化合物(B)を0.0001~5重量部含有することを特徴とする請求項1~3のいずれかに記載の粘着剤層付偏光フィルム。
- (メタ)アクリル系ポリマー(A)が、モノマー単位として、アルキル(メタ)アクリレートおよびヒドロキシル基含有モノマーを含有することを特徴とする請求項1~4のいずれかに記載の粘着剤層付偏光フィルム。
- (メタ)アクリル系ポリマー(A)が、モノマー単位として、アルキル(メタ)アクリレートおよびカルボキシル基含有モノマーを含有することを特徴とする請求項1~4のいずれかに記載の粘着剤層付偏光フィルム。
- 前記粘着剤組成物が、さらに、架橋剤を含有することを特徴とする請求項1~6のいずれかに記載の粘着剤層付偏光フィルム。
- 架橋剤(C)は、(メタ)アクリル系ポリマー(A)100重量部に対して、0.01~20重量部含有することを特徴とする請求項7記載の粘着剤層付偏光フィルム。
- 架橋剤(C)が、イソシアネート系化合物および過酸化物から選ばれるいずれか少なくとも1種であることを特徴とする請求項7または8記載の粘着剤層付偏光フィルム。
- (メタ)アクリル系ポリマー(A)100重量部に対して、さらに、シランカップリング剤(D)を0.001~5重量部含有することを特徴とする請求項1~9のいずれかに記載の粘着剤層付偏光フィルム。
- (メタ)アクリル系ポリマー(A)の重量平均分子量が、50万~300万であることを特徴とする請求項1~10のいずれかに記載の粘着剤層付偏光フィルム。
- 偏光フィルムと、粘着剤層の間に、易接着層を有することを特徴とする請求項1~11のいずれかに記載の粘着剤層付偏光フィルム。
- 請求項1~12のいずれかに記載の粘着剤層付偏光フィルムを少なくとも1つ用いたことを特徴とする画像表示装置。
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Also Published As
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KR20140031885A (ko) | 2014-03-13 |
CN107057591B (zh) | 2021-10-26 |
TWI619791B (zh) | 2018-04-01 |
US20140085722A1 (en) | 2014-03-27 |
TWI631204B (zh) | 2018-08-01 |
TW201307513A (zh) | 2013-02-16 |
KR102054096B1 (ko) | 2019-12-09 |
KR20180118239A (ko) | 2018-10-30 |
CN107057591A (zh) | 2017-08-18 |
US9377570B2 (en) | 2016-06-28 |
TW201720893A (zh) | 2017-06-16 |
KR101912968B1 (ko) | 2018-10-29 |
JP2013008019A (ja) | 2013-01-10 |
CN103562759B (zh) | 2016-11-16 |
CN103562759A (zh) | 2014-02-05 |
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