WO2014065425A1 - 偏光性積層フィルムの製造方法および偏光板の製造方法 - Google Patents

偏光性積層フィルムの製造方法および偏光板の製造方法 Download PDF

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WO2014065425A1
WO2014065425A1 PCT/JP2013/079061 JP2013079061W WO2014065425A1 WO 2014065425 A1 WO2014065425 A1 WO 2014065425A1 JP 2013079061 W JP2013079061 W JP 2013079061W WO 2014065425 A1 WO2014065425 A1 WO 2014065425A1
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Prior art keywords
film
stretching
polyvinyl alcohol
layer
laminated film
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PCT/JP2013/079061
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English (en)
French (fr)
Japanese (ja)
Inventor
河村　真一
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住友化学株式会社
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Priority to KR1020157009261A priority Critical patent/KR102091301B1/ko
Priority to CN201380054755.3A priority patent/CN104737042A/zh
Publication of WO2014065425A1 publication Critical patent/WO2014065425A1/ja

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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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00—Coating compositions 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00—Coating compositions 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C09D129/02—Homopolymers or copolymers of unsaturated alcohols
    • C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids

Definitions

  • the present invention relates to a method for producing a polarizing laminated film and a method for producing a polarizing plate.
  • the polarizing plate is widely used as a polarized light supplying element and a polarized light detecting element in a liquid crystal display device.
  • a polarizing plate a polarizing film made of a polyvinyl alcohol-based resin and a protective film made of triacetyl cellulose or the like bonded via an adhesive have been used.
  • the polarizing film is produced by stretching and dyeing a polyvinyl alcohol-based resin film (usually about 75 ⁇ m thick), and the thickness of the stretched film is usually about 30 ⁇ m.
  • a polarizing film is produced from the original film of the polyvinyl alcohol resin. Since a thinner polarizer layer can be obtained, it is advantageous from the viewpoint of reducing the thickness and weight of the polarizing plate.
  • a laminated film having a polyvinyl alcohol-based resin layer is stretched, wrinkles are generated in the stretched film, or stretching unevenness (non-uniform stretching) occurs in the film width direction. There was a problem that unevenness in thickness occurred in the film width direction.
  • an object of the present invention is to form a polyvinyl alcohol-based resin layer by coating a base film with a coating liquid containing a polyvinyl alcohol-based resin, to obtain a laminated film, and then by stretching and dyeing the laminated film.
  • a method for producing a polarizing laminated film or polarizing plate using a polyvinyl alcohol-based resin layer as a polarizer layer the laminated film can be stretched while suppressing wrinkles and stretching unevenness, and thus the appearance and optical properties of
  • An object of the present invention is to provide a method capable of producing a good thin polarizing laminate film or polarizing plate with a high yield.
  • the present invention includes the following.
  • the stretching step includes two or more stretching treatment steps, The ratio of the stretching ratio in the first stretching process to the stretching ratio in the second stretching process is 0.5 or more, The method for producing a polarizing laminated film, wherein the total draw ratio of the polarizer layer is more than 5 times based on the polyvinyl alcohol resin layer of the laminated film.
  • FIG. 1 is a flowchart showing a preferred embodiment of a method for producing a polarizing laminate film and a method for producing a polarizing plate according to the present invention.
  • FIG. 2 is a schematic diagram showing an example of multistage stretching in the stretching step S20.
  • FIG. 3 is a schematic diagram showing another example of multistage stretching in the stretching step S20.
  • FIG. 4 is a schematic diagram for explaining a longitudinal uniaxial stretching method using a chuck.
  • FIG. 1 is a flowchart showing a preferred embodiment of a method for producing a polarizing laminate film and a method for producing a polarizing plate according to the present invention.
  • the manufacturing method of the light-polarizing laminated film of this embodiment includes the following steps: Resin layer forming step S10 to obtain a laminated film by forming a polyvinyl alcohol-based resin layer by applying a coating liquid containing a polyvinyl alcohol-based resin on at least one surface of the base film, followed by drying.
  • Dyeing step S30 to obtain a polarizing laminated film by dyeing a polyvinyl alcohol resin layer of a stretched film with a dichroic dye to form a polarizer layer are included in this order.
  • the polarizing plate is bonded to a protective film on the polarizer layer of the polarizing laminate film obtained by carrying out the dyeing step S30 (bonding step S40). ), And then the substrate film is peeled and removed from the bonded film (peeling step S50).
  • Resin layer forming step S10 This step is a step of obtaining a laminated film by forming a polyvinyl alcohol-based resin layer on at least one surface of the base film.
  • This polyvinyl alcohol-based resin layer is a layer that becomes a polarizer layer through the stretching step S20 and the dyeing step S30.
  • a polyvinyl alcohol-type resin layer can be formed by applying the coating liquid containing a polyvinyl alcohol-type resin to the single side
  • the base film can be composed of a thermoplastic resin, and among them, it is preferably composed of a thermoplastic resin excellent in transparency, mechanical strength, thermal stability, stretchability and the like.
  • thermoplastic resins include, for example, polyolefin resins such as chain polyolefin resins and cyclic polyolefin resins (norbornene resins, etc.); polyester resins; (meth) acrylic resins; cellulose triacetate, Cellulose ester resins such as cellulose diacetate; Polycarbonate resins; Polyvinyl alcohol resins; Polyvinyl acetate resins; Polyarylate resins; Polystyrene resins; Polyethersulfone resins; Polysulfone resins; Polyamide resins; Resin, and mixtures and copolymers thereof.
  • polyolefin resins such as chain polyolefin resins and cyclic polyolefin resins (norbornene resins, etc.
  • polyester resins include, for example, polyolefin resins such as chain polyolefin resins and cyclic polyolefin resins (norbornene resins, etc.); polyester resins; (meth
  • the base film may have a single-layer structure composed of one resin layer composed of one or two or more thermoplastic resins, or a plurality of resin layers composed of one or two or more thermoplastic resins are laminated. It may be a multilayer structure.
  • the chain polyolefin-based resin include homopolymers of chain olefins such as polyethylene resins and polypropylene resins, and copolymers composed of two or more chain olefins.
  • a base film made of a chain polyolefin-based resin is preferable in that it is easily stretched stably at a high magnification.
  • the base film is composed mainly of polypropylene resin (polypropylene resin which is a homopolymer of propylene or a copolymer mainly composed of propylene), polyethylene resin (polyethylene resin which is a homopolymer of ethylene or ethylene). It is more preferable to consist of a copolymer).
  • a copolymer mainly composed of propylene which is one of the examples suitably used as the thermoplastic resin constituting the base film, is a copolymer of propylene and another monomer copolymerizable therewith. Examples of other monomers copolymerizable with propylene include ethylene and ⁇ -olefin.
  • an ⁇ -olefin having 4 or more carbon atoms is preferably used, and more preferably an ⁇ -olefin having 4 to 10 carbon atoms.
  • Specific examples of the ⁇ -olefin having 4 to 10 carbon atoms include, for example, linear monoolefins such as 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene and 1-decene; 3 -Branched monoolefins such as methyl-1-butene, 3-methyl-1-pentene, 4-methyl-1-pentene; and vinylcyclohexane.
  • the copolymer of propylene and other monomers copolymerizable therewith may be a random copolymer or a block copolymer.
  • the content of the other monomer in the copolymer is, for example, 0.1% by weight to 20% by weight, and preferably 0.5% by weight to 10% by weight.
  • the content of other monomers in the copolymer can be determined by measuring infrared (IR) spectrum according to the method described on page 616 of "Polymer Analysis Handbook" (1995, published by Kinokuniya Shoten). Can be sought.
  • the polypropylene resin a propylene homopolymer, a propylene-ethylene random copolymer, a propylene-1-butene random copolymer or a propylene-ethylene-1-butene random copolymer is preferably used.
  • the stereoregularity of the polypropylene resin is preferably substantially isotactic or syndiotactic.
  • a base film made of a polypropylene-based resin having substantially isotactic or syndiotactic stereoregularity has relatively good handleability and excellent mechanical strength in a high temperature environment.
  • the base film may be composed of one type of chain polyolefin-based resin, may be composed of a mixture of two or more types of chain polyolefin-based resins, or may be composed of two or more types of chain polyolefin-based resins. You may be comprised from the copolymer of resin.
  • the cyclic polyolefin resin is a general term for resins that are polymerized using a cyclic olefin as a polymerization unit, and is described, for example, in JP-A-1-240517, JP-A-3-14882, JP-A-3-122137, and the like. Resin.
  • cyclic polyolefin resins include ring-opening (co) polymers of cyclic olefins, addition polymers of cyclic olefins, copolymers of cyclic olefins and chain olefins such as ethylene and propylene (typically Are random copolymers), graft polymers obtained by modifying them with unsaturated carboxylic acids or derivatives thereof, and hydrides thereof.
  • norbornene resins using norbornene monomers such as norbornene and polycyclic norbornene monomers as cyclic olefins are preferably used.
  • Various products are commercially available for the cyclic polyolefin resin.
  • Examples of commercial products of cyclic polyolefin resins are trade names, “Topas” (manufactured by TOPAS ADVANCED POLYMERS GmbH, available from Polyplastics), “Arton” (manufactured by JSR), Includes “ZEONOR” (manufactured by Nippon Zeon Co., Ltd.), “ZEONEX” (manufactured by Nippon Zeon Co., Ltd.), and “Apel” (manufactured by Mitsui Chemicals, Inc.).
  • the base film may be composed of one kind of cyclic polyolefin-based resin, may be composed of a mixture of two or more kinds of cyclic polyolefin-based resins, or may be composed of two or more kinds of cyclic polyolefin-based resins. It may be composed of a polymer.
  • the polyester-based resin is a resin having an ester bond, and is generally made of a polycondensate of a polyvalent carboxylic acid or a derivative thereof and a polyhydric alcohol.
  • a polyvalent carboxylic acid or a derivative thereof a divalent dicarboxylic acid or a derivative thereof can be used, and examples thereof include terephthalic acid, isophthalic acid, dimethyl terephthalate, and dimethyl naphthalenedicarboxylate.
  • a divalent diol can be used, and examples thereof include ethylene glycol, propanediol, butanediol, neopentyl glycol, and cyclohexanedimethanol.
  • polyester resin is polyethylene terephthalate which is a polycondensate of terephthalic acid and ethylene glycol.
  • Polyethylene terephthalate is a crystalline resin, but the one in a state before crystallization treatment is more easily subjected to treatment such as stretching. If necessary, it can be crystallized during stretching or by heat treatment after stretching.
  • a copolymerized polyester having a crystallinity lowered (or made amorphous) by further copolymerizing another monomer with a polyethylene terephthalate skeleton is also preferably used.
  • examples of such resins include those obtained by copolymerizing cyclohexanedimethanol and isophthalic acid.
  • polyester resins other than polyethylene terephthalate and copolymers thereof include, for example, polybutylene terephthalate, polyethylene naphthalate, polybutylene naphthalate, polytrimethylene terephthalate, polytrimethylene naphthalate, polycyclohexanedimethyl terephthalate, Examples include polycyclohexanedimethyl naphthalate.
  • the base film may be composed of one kind of polyester resin, may be composed of a mixture of two or more kinds of polyester resins, or may be composed of a copolymer of two or more kinds of polyester resins. It may be configured.
  • the (meth) acrylic resin is a resin containing a compound having a (meth) acryloyl group as a main constituent monomer.
  • Specific examples of (meth) acrylic resins include, for example, poly (meth) acrylic acid esters such as polymethyl methacrylate; methyl methacrylate- (meth) acrylic acid copolymer; methyl methacrylate- (meth) acrylic acid Ester copolymer; methyl methacrylate-acrylic ester- (meth) acrylic acid copolymer; (meth) methyl acrylate-styrene copolymer (MS resin etc.); methyl methacrylate and alicyclic hydrocarbon group And a copolymer (for example, methyl methacrylate-cyclohexyl methacrylate copolymer, methyl methacrylate- (meth) acrylate norbornyl copolymer).
  • poly (meth) acrylic acid C such as methyl poly (meth) acrylate 1-6
  • a polymer having an alkyl ester as a main component is used, more preferably, a methyl methacrylate-based resin having methyl methacrylate as a main component (50 wt% to 100 wt%, preferably 70 wt% to 100 wt%).
  • the base film may be composed of one (meth) acrylic resin, may be composed of a mixture of two or more (meth) acrylic resins, or may be composed of two or more (meth) acrylic resins. ) It may be composed of a copolymer of acrylic resin.
  • the cellulose ester resin is an ester of cellulose and a fatty acid.
  • cellulose ester resin examples include cellulose triacetate, cellulose diacetate, cellulose tripropionate, and cellulose dipropionate.
  • these copolymers and those in which a part of the hydroxyl group is modified with another substituent are also included.
  • cellulose triacetate triacetyl cellulose
  • Many products of cellulose triacetate are commercially available, which is advantageous in terms of availability and cost.
  • Examples of commercially available cellulose triacetate are “Fujitac TD80” (manufactured by Fuji Film Co., Ltd.), “Fujitac TD80UF” (manufactured by Fuji Film Co., Ltd.), “Fujitac TD80UZ” (Fuji Film ( Co., Ltd.), “Fujitac TD40UZ” (Fuji Film Co., Ltd.), “KC8UX2M” (Konica Minolta Opto Co., Ltd.), “KC4UY” (Konica Minolta Opto Co., Ltd.), and the like.
  • the base film may be composed of one kind of cellulose ester resin, may be composed of a mixture of two or more kinds of cellulose ester resins, or may be composed of two or more kinds of cellulose ester resins. It may be composed of a polymer.
  • the polycarbonate-based resin is an engineering plastic made of a polymer in which monomer units are bonded via a carbonate group, and is a resin having high impact resistance, heat resistance, flame retardancy, and transparency.
  • the polycarbonate-based resin constituting the base film may be a resin called a modified polycarbonate in which the polymer skeleton is modified in order to lower the photoelastic coefficient, a copolymer polycarbonate having improved wavelength dependency, or the like.
  • Various products are commercially available for polycarbonate resins.
  • the base film may be composed of one type of polycarbonate-based resin, may be composed of a mixture of two or more types of polycarbonate-based resins, or may be composed of a copolymer of two or more types of polycarbonate-based resins. It may be configured. Arbitrary appropriate additives other than said thermoplastic resin may be added to the base film.
  • thermoplastic resin in the base 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% by weight. % To 97% by weight. When the content of the thermoplastic resin in the base film is less than 50% by weight, the high transparency inherent in the thermoplastic resin may not be sufficiently exhibited.
  • the thickness of the base film can be determined as appropriate, but in general, from the viewpoint of workability such as strength and handleability, 1 ⁇ m to 500 ⁇ m is preferable, 1 ⁇ m to 300 ⁇ m is more preferable, 5 ⁇ m to 200 ⁇ m is further preferable, and 5 ⁇ m to 150 ⁇ m is preferable. Is most preferred.
  • the coating liquid is preferably a polyvinyl alcohol resin solution obtained by dissolving a polyvinyl alcohol resin powder in a good solvent (for example, water).
  • a good solvent for example, water.
  • the polyvinyl alcohol resin include polyvinyl alcohol resins and derivatives thereof.
  • Polyvinyl alcohol resin derivatives include polyvinyl formal, polyvinyl acetal, etc., as well as polyvinyl alcohol resins modified with olefins such as ethylene and propylene; unsaturated carboxylic acids such as acrylic acid, methacrylic acid and crotonic acid. Denatured; modified with alkyl ester of unsaturated carboxylic acid; modified with acrylamide.
  • the proportion of modification is preferably less than 30 mol%, and more preferably less than 10 mol%. When the modification exceeding 30 mol% is performed, it is difficult to adsorb the dichroic dye, which may cause a problem that the polarization performance is lowered.
  • the average degree of polymerization of the polyvinyl alcohol-based resin is preferably in the range of 100 to 10000, more preferably in the range of 1000 to 10000, still more preferably in the range of 1500 to 8000, and in the range of 2000 to 5000. Most preferably.
  • the average degree of polymerization can be determined by a method defined in JIS K 6726-1994 “Testing method for polyvinyl alcohol”.
  • the polyvinyl alcohol resin is preferably a saponified product of a polyvinyl acetate resin.
  • the range of the saponification degree is preferably 80 mol% or more, more preferably 90 mol% or more, and particularly preferably 94 mol% or more. If the degree of saponification is too low, the water resistance and heat-and-moisture resistance may not be sufficient when a polarizing laminate film or a polarizing plate is formed.
  • the saponification degree is preferably 99.5 mol% or less, more preferably 99.0 mol% or less.
  • the degree of saponification refers to an acetate group (acetoxy group: —OCOCH) contained in a polyvinyl acetate resin, which is a raw material for a polyvinyl alcohol resin.
  • Saponification degree (mol%) [(Number of hydroxyl groups) ⁇ (number of hydroxyl groups + number of acetate groups)] ⁇ 100 Defined by The higher the degree of saponification, the greater the proportion of hydroxyl groups, and hence the smaller the proportion of acetate groups that inhibit crystallization.
  • the saponification degree can be determined by a method defined in JIS K 6726-1994 “Testing method for polyvinyl alcohol”.
  • polyvinyl acetate resin examples include polyvinyl acetate, which is a homopolymer of vinyl acetate, and copolymers with other monomers copolymerizable with vinyl acetate.
  • examples of other monomers copolymerizable with vinyl acetate include unsaturated carboxylic acids, olefins, vinyl ethers, unsaturated sulfonic acids, and acrylamides having an ammonium group.
  • polyvinyl alcohol resins examples include trade names, “PVA124” (degree of saponification: 98.0 mol% to 99.0 mol%) manufactured by Kuraray Co., Ltd., “PVA117 (Saponification degree: 98.0 mol% to 99.0 mol%), “PVA117H” (saponification degree: 99.5 mol% or more), “PVA624" (saponification degree: 95.0 mol% to 96 0.0 mol%) and “PVA617” (degree of saponification: 94.5 mol% to 95.5 mol%); “AH-26” (degree of saponification: 97.0 mol) manufactured by Nippon Synthetic Chemical Industry Co., Ltd.
  • the coating liquid may contain additives such as a plasticizer and a surfactant as necessary.
  • a plasticizer a polyol or a condensate thereof can be used, and examples thereof include glycerin, diglycerin, triglycerin, ethylene glycol, propylene glycol, and polyethylene glycol.
  • the blending amount of the additive is preferably 20% by weight or less of the polyvinyl alcohol resin.
  • the drying temperature and drying time of the coating layer are set according to the type of solvent contained in the coating solution.
  • the drying temperature is, for example, 50 ° C. to 200 ° C., preferably 60 ° C. to 150 ° C.
  • the drying temperature is preferably 80 ° C. or higher.
  • the drying time is, for example, 2 minutes to 20 minutes.
  • the polyvinyl alcohol-based resin layer may be formed on only one surface of the base film, or may be formed on both surfaces. When it is formed on both sides, curling of the polarizing laminate film and the film that may occur during the production of the polarizing plate can be suppressed, and two polarizing plates can be obtained from one polarizing laminated film.
  • the thickness of the polyvinyl alcohol-based resin layer in the laminated film is preferably 3 ⁇ m to 30 ⁇ m, and more preferably 5 ⁇ m to 20 ⁇ m. If the polyvinyl alcohol-based resin layer has a thickness within this range, the dichroic dye has good dyeability and excellent polarization performance through a stretching step S20 and a dyeing step S30, which will be described later. A child layer can be obtained. When the thickness of the polyvinyl alcohol-based resin layer exceeds 30 ⁇ m, the thickness of the polarizer layer may exceed 10 ⁇ m. Moreover, when the thickness of the polyvinyl alcohol-based resin layer is less than 3 ⁇ m, the film becomes too thin after stretching and the dyeability tends to deteriorate.
  • At least the surface of the base film on which the polyvinyl alcohol resin layer is formed is subjected to corona treatment and plasma. You may perform a process, a flame
  • a polyvinyl alcohol resin layer is formed on the base film via a primer layer or an adhesive layer. It may be formed.
  • the primer layer can be formed by applying a primer layer forming coating solution to the surface of the substrate film and then drying it.
  • the primer layer forming coating solution contains a component that exhibits a certain degree of strong adhesion to both the base film and the polyvinyl alcohol-based resin layer.
  • the primer layer-forming coating solution usually contains a resin component that imparts such adhesion and a solvent.
  • a resin component a thermoplastic resin excellent in transparency, thermal stability, stretchability, and the like is preferably used, and examples thereof include (meth) acrylic resins and polyvinyl alcohol resins. Among these, polyvinyl alcohol resins that give good adhesion are preferably used. Examples of the polyvinyl alcohol resin include polyvinyl alcohol resins and derivatives thereof.
  • Polyvinyl alcohol resin derivatives include polyvinyl formal, polyvinyl acetal, etc., as well as polyvinyl alcohol resins modified with olefins such as ethylene and propylene; unsaturated carboxylic acids such as acrylic acid, methacrylic acid and crotonic acid. Denatured; modified with alkyl ester of unsaturated carboxylic acid; modified with acrylamide.
  • a polyvinyl alcohol resin it is preferable to use a polyvinyl alcohol resin.
  • the solvent a general organic solvent or an aqueous solvent capable of dissolving the resin component is usually used.
  • solvents include, for example, aromatic hydrocarbons such as benzene, toluene and xylene; ketones such as acetone, methyl ethyl ketone and methyl isobutyl ketone; esters such as ethyl acetate and isobutyl acetate; Chlorinated hydrocarbons such as trichlorethylene and chloroform; alcohols such as ethanol, 1-propanol, 2-propanol and 1-butanol.
  • aromatic hydrocarbons such as benzene, toluene and xylene
  • ketones such as acetone, methyl ethyl ketone and methyl isobutyl ketone
  • esters such as ethyl acetate and isobutyl acetate
  • Chlorinated hydrocarbons such as trichlorethylene and chloroform
  • alcohols such as ethanol, 1-propanol, 2-propanol and 1-butanol.
  • the primer layer
  • the primer layer is preferably formed from a coating solution containing water as a solvent.
  • a crosslinking agent may be added to the primer layer forming coating solution.
  • a suitable crosslinking agent is appropriately selected from known ones such as organic and inorganic based on the type of thermoplastic resin used. Examples of the crosslinking agent include epoxy-based, isocyanate-based, dialdehyde-based, and metal-based crosslinking agents.
  • the epoxy-based crosslinking agent either one-component curable type or two-component curable type can be used.
  • Ethylene glycol diglycidyl ether polyethylene glycol diglycidyl ether, glycerin di- or tri-glycidyl ether, 1,6-hexane
  • Examples include diol diglycidyl ether, trimethylolpropane triglycidyl ether, diglycidyl aniline, diglycidyl amine and the like.
  • Isocyanate-based crosslinking agents include tolylene diisocyanate, hydrogenated tolylene diisocyanate, trimethylolpropane-tolylene diisocyanate adduct, triphenylmethane triisocyanate, methylenebis (4-phenylmethane) triisocyanate, isophorone diisocyanate, and ketoximes thereof.
  • a block thing or a phenol block thing etc. are mentioned.
  • Examples of the dialdehyde-based crosslinking agent include glyoxal, malondialdehyde, succindialdehyde, glutardialdehyde, maleidialdehyde, phthaldialdehyde and the like.
  • metal-based crosslinking agent examples include metal salts, metal oxides, metal hydroxides, and organometallic compounds.
  • metal salt, metal oxide, and metal hydroxide include divalent or higher valent metals such as magnesium, calcium, aluminum, iron, nickel, zirconium, titanium, silicon, boron, zinc, copper, vanadium, chromium, and tin. Examples thereof include salts, oxides and hydroxides of metals having a valence.
  • An organometallic compound is a compound having in its molecule at least one structure in which an organic group is bonded directly to a metal atom or an organic group is bonded through an oxygen atom, a nitrogen atom, or the like.
  • the organic group means a monovalent or polyvalent group containing at least a carbon element, and can be, for example, an alkyl group, an alkoxy group, an acyl group, or the like. Further, the bond does not mean only a covalent bond, but may be a coordinate bond by coordination of a chelate compound or the like.
  • Suitable examples of the organometallic compound include an organotitanium compound, an organozirconium compound, an organoaluminum compound, and an organosilicon compound.
  • An organometallic compound may be used individually by 1 type, and may use 2 or more types together.
  • organic titanium compounds examples include titanium orthoesters such as tetranormal butyl titanate, tetraisopropyl titanate, butyl titanate dimer, tetra (2-ethylhexyl) titanate, tetramethyl titanate; titanium acetylacetonate, titanium tetraacetylacetonate , Titanium chelates such as polytitanium acetylacetonate, titanium octylene glycolate, titanium lactate, titanium triethanolamate, and titanium ethyl acetoacetate; and titanium acylates such as polyhydroxytitanium stearate.
  • titanium orthoesters such as tetranormal butyl titanate, tetraisopropyl titanate, butyl titanate dimer, tetra (2-ethylhexyl) titanate, tetramethyl titanate
  • titanium acetylacetonate titanium tetraacetylacetonate
  • Examples of the organic zirconium compound include zirconium normal propionate, zirconium normal butyrate, zirconium tetraacetylacetonate, zirconium monoacetylacetonate, zirconium bisacetylacetonate, zirconium acetylacetonate bisethylacetoacetate and the like.
  • Examples of the organoaluminum compound include aluminum acetylacetonate and aluminum organic acid chelate.
  • Examples of the organosilicon compound include compounds in which the ligands exemplified above for the organotitanium compound and the organozirconium compound are bonded to silicon.
  • high molecular weight crosslinking agents such as methylolated melamine resins and polyamide epoxy resins can also be used.
  • polyamide epoxy resins include “Smiles Resin 650 (30)” and “Smiles Resin 675” (both trade names) sold by Taoka Chemical Co., Ltd.
  • a polyvinyl alcohol-based resin is used as the resin component forming the primer layer
  • a polyamide epoxy resin, a methylolated melamine resin, a dialdehyde-based crosslinking agent, a metal chelate compound-based crosslinking agent, or the like is preferably used as the crosslinking agent.
  • the ratio of the resin component and the crosslinking agent in the primer layer forming coating solution is within the range of about 0.1 to 100 parts by weight of the crosslinking agent with respect to 100 parts by weight of the resin component. It may be determined appropriately according to the type of the material, and is particularly preferably selected from the range of about 0.1 to 50 parts by weight. Further, the primer layer forming coating solution preferably has a solid content concentration of about 1 to 25% by weight. The thickness of the primer layer is preferably about 0.05 ⁇ m to 1 ⁇ m, and more preferably 0.1 ⁇ m to 0.4 ⁇ m.
  • the method for applying the primer layer forming coating solution to the substrate film can be the same as the coating solution for forming the polyvinyl alcohol-based resin layer.
  • the primer layer is applied to the surface (one side or both sides of the base film) to which the coating liquid for forming the polyvinyl alcohol-based resin layer is applied.
  • the drying temperature and drying time of the coating layer comprising the primer layer forming coating solution are set according to the type of solvent contained in the coating solution.
  • Stretching step S20 This step is a step of obtaining a stretched film by longitudinally uniaxially stretching a laminated film composed of a base film and a polyvinyl alcohol-based resin layer. In this invention, extending
  • “including two or more steps of stretching treatment” means that the first stage (first) stretching treatment step in which the laminated film is longitudinally uniaxially stretched at a certain draw ratio, and the laminated film is not stretched (in the film transport direction). It means that it has at least a second-stage stretching treatment step in which the laminated film subjected to the first-stage stretching treatment is stretched uniaxially at a certain stretching ratio through a section (time zone) that does not stretch).
  • the stretching step S20 can include three or more steps of stretching treatment. In this case as well, a section (time zone) in which the laminated film is not stretched is interposed between the stretching treatment steps of each step.
  • the longitudinal uniaxial stretching in each stage of the stretching treatment step can be, for example, stretching between rolls, rolling, hot roll stretching, stretching using a chuck, or the like.
  • the stretching methods at each stage may all be the same, or different stretching methods may be combined.
  • it is preferable that at least one step of the stretching process is performed by stretching between rolls which is free end stretching.
  • W1 is the width of the laminated film before being subjected to the stretching step S20.
  • W2 is the minimum width of the film after all stretching processes have been performed on the laminated film. For example, when the stretching process is performed on the laminated film only in the stretching step S20, W2 is the minimum width of the stretched film finally obtained in the stretching step S20. As will be described later, an additional stretching process can also be performed in the dyeing step S30. In this case, W2 is the minimum width of the polarizing laminated film after the additional stretching process.
  • the neck-in rate is preferably about 50% or more.
  • FIG. 2 shows an example in which the stretching step S20 includes a two-stage stretching process, and both of these stretching processes are a roll-to-roll stretching system, that is, a system in which stretching is performed between nip rolls having different peripheral speeds. It is. Specifically, the conveyed laminated film 10 is first stretched between the nip roll 1 and the nip roll 2 having different peripheral speeds while being heated by passing through the heating furnace 20 set to a desired temperature ( First stage stretching process).
  • the first-stage stretched film is further conveyed by the guide roll 5 and heated by passing through the heating furnace 30 set to a desired temperature, while the nip roll 3 and the nip roll 4 having different peripheral speeds are mutually connected. Is stretched (second-stage stretching process) to become a stretched film 15.
  • the stretching step S20 includes a three-stage stretching process, and each of these stretching processes is a hot roll stretching method, that is, a method of stretching between heated rolls. It is.
  • the transported laminated film 10 is first stretched while the surface is adjusted to a desired temperature and passes between the hot rolls 6 to 7 having different peripheral speeds (first-stage stretching). Processing step). Next, the surface is adjusted to a desired temperature through a section where no stretching occurs, that is, a section in contact with the heat roll 7, and the surface is stretched while passing between the heat roll 7 and the heat roll 8 having different peripheral speeds. (Second-stage stretching process).
  • the film subjected to the second-stage stretching treatment has a section in which stretching does not occur, that is, a section in contact with the heat roll 8, the surface is adjusted to a desired temperature, and the heat roll 8-heat having different peripheral speeds.
  • FIG. 4 is a schematic diagram for explaining a longitudinal uniaxial stretching method using a chuck (clip), and is a view when a laminated film to be stretched is viewed from above.
  • a longitudinal uniaxial stretching method using a chuck as shown in the drawing, a plurality of chucks 40 are attached to both ends of the laminated film 10 in the width direction (usually at regular intervals), and the laminated film 10 heated to a desired temperature is attached.
  • a method of stretching by gradually increasing the inter-chuck distance R in the film transport direction while transporting.
  • the inter-chuck distance R is widened and the stretching process (first stretching process step) is performed, and then the inter-chuck distance R is fixed. After passing through the section in which the laminated film 10 is conveyed, the inter-chuck distance R may be increased again to perform the stretching process (second-stage stretching process).
  • the method for controlling the inter-chuck distance R during stretching is not particularly limited, and various methods can be used. For example, each chuck can be driven independently, and each chuck may be controlled independently to control the distance R between chucks, or the chucks are connected to each other. The chuck distance may be controlled to control the inter-chuck distance R.
  • any method can be suitably used in the present invention.
  • Specific methods for independently driving individual chucks include a method using magnetic force as typified by a linear motor drive system, a method of attaching a rotary drive motor or the like to each chuck, and the like. Instead of independently driving all the chucks, only a part of the chucks can be independently driven, and the other remaining chucks can be controlled not to be specially controlled.
  • a pantograph method or the like is typical.
  • the pantograph system is a system that controls the distance R between chucks by opening and closing the pantograph by controlling the distance between two rails. None of the above-described multistage stretching illustrated with reference to FIGS.
  • the present invention is not limited to the above example, and the film may be wound up every time one step of the stretching process is completed, and unwound again when the next stretching process is performed.
  • the ratio of the draw ratio in the first drawing process to the draw ratio in the second drawing process (hereinafter also referred to as “stretch ratio”) is 0.5 or more.
  • the draw ratio in the first stretching step means that the length in the longitudinal direction (stretched direction) of the polyvinyl alcohol-based resin layer of the laminated film before being subjected to the stretching step S20 is 1.
  • paragraph the length in the longitudinal direction of the polyvinyl alcohol-based resin layer (or the length of the portion having the polyvinyl alcohol-based resin layer) of the laminated film before being subjected to the stretching step S20 is 1, and the first-stage stretching process When the length of the polyvinyl alcohol-based resin layer (or the length of the certain portion) is 2 by the process, the stretching ratio in the first stretching process is doubled.
  • the “stretch ratio in the second stage stretching process” is the second stage stretching process when the length in the longitudinal direction of the polyvinyl alcohol-based resin layer at the end of the first stage stretching process is 1. It is the length of the longitudinal direction of the polyvinyl alcohol-type resin layer at the time of completion
  • the stretching film S20 is divided into two or more stretching process steps, and the first and second stretching process steps are performed so as to satisfy the above-described stretching ratio, thereby obtaining a laminated film up to a desired total stretching ratio.
  • a stretched film having a thickness difference in the film width direction of less than 5 ⁇ m, and further less than 4 ⁇ m can be produced, and thus a polarizing laminated film and a polarizing plate having uniform polarization performance and transmittance are produced.
  • Thinness difference in the film width direction means that the film thickness is measured at one point at a position of 50 mm from one end in the film width direction, and the film thickness at the center position in the film width direction is measured at one point. It means the absolute value of the difference in thickness.
  • the draw ratio is preferably 0.6 or more, more preferably 0.7 or more, and particularly preferably 1.0 or more in order to obtain the above-described effects more effectively.
  • the stretch ratio is preferably 5 or less, more preferably 4 or less, and particularly preferably 3 or less.
  • the draw ratio in the first drawing step is preferably less than 5 times, more preferably 4 times or less. Wrinkles tend to occur when the draw ratio is 5 times or more. That is, in order to impart good polarization performance to the polarizer layer obtained through the dyeing step S30, it is desirable that the total stretching ratio of the stretching treatment performed on the laminated film is 5 times or more as described later. When such a high-magnification stretching process is performed in one stage, wrinkles are generated.
  • the stretching process is performed in two or more stages in consideration of the above.
  • the above-mentioned “total stretching ratio” means each stage of the stretching process (as will be described later, an additional stretching process can also be performed in the dyeing process S30. In this case, the additional stretching process is included.
  • the total draw ratio of the polarizer layer is preferably more than 5 times based on the polyvinyl alcohol resin layer of the laminated film.
  • the draw ratio is 5 times or less, the polyvinyl alcohol-based resin layer is not sufficiently oriented, and thus the degree of polarization of the polarizer layer tends not to be sufficiently high.
  • the total draw ratio is preferably 8 times or less. When the total draw ratio exceeds 8 times, the film is likely to be broken during stretching, and the thickness of the stretched film becomes unnecessarily thin, and the workability and handleability in the subsequent process may be reduced.
  • the stretching temperature in each stage of the stretching step S20 is set to be higher than the temperature at which the polyvinyl alcohol-based resin layer and the entire substrate film can be stretched, and preferably from the melting point of the substrate film to ⁇ 30 ° C. It is in the range of + 30 ° C., more preferably in the range of the melting point ⁇ 30 ° C. to the melting point + 5 ° C., and still more preferably in the range of the melting point ⁇ 25 ° C. to the melting point + 0 ° C.
  • the melting point means the highest melting point among melting points of the plurality of resin layers.
  • the stretching temperature is lower than the melting point of the base film ⁇ 30 ° C., the fluidity of the base film is too low and the stretching process tends to be difficult.
  • the stretching temperature exceeds the melting point + 30 ° C., the fluidity of the base film is too high and the stretching treatment tends to be difficult.
  • the stretching temperature is within the above range, and more preferably 120 ° C. or higher.
  • a zone heating method for example, a method of heating in a stretching zone such as a heating furnace in which hot air is blown and adjusted to a predetermined temperature; see FIG.
  • the zone heating method is preferable from the viewpoint of the uniformity of the stretching temperature.
  • the two nip roll pairs may be installed in the temperature-controlled stretching zone or outside the stretching zone, but are installed outside the stretching zone to prevent adhesion between the laminated film and the nip roll. Is preferred (see FIG. 2).
  • the stretching temperature means the atmospheric temperature in the zone (for example, in the heating furnace) in the case of the zone heating method, and also means the atmospheric temperature in the furnace in the case of heating in the furnace even in the heater heating method. Moreover, in the case of the method of heating roll itself, the surface temperature of a roll is meant.
  • a preheat treatment step for preheating the laminated film may be provided prior to the stretching step S20.
  • the preheating method the same method as the heating method in the stretching process can be used.
  • preheating may be performed at any timing before passing through the upstream nip roll, during passing, or after passing.
  • preheating is hot roll stretching, preheating is preferably performed at a timing before passing through the hot roll.
  • preheating is preferably performed at a timing before increasing the distance between chucks.
  • the preheating temperature is preferably in the range of stretching temperature ⁇ 50 ° C. to stretching temperature ⁇ 0 ° C., and more preferably in the range of stretching temperature ⁇ 40 ° C. to stretching temperature ⁇ 10 ° C.
  • the heat setting process is a process of performing a heat treatment at a temperature equal to or higher than the crystallization temperature while maintaining the tensioned state with the end of the stretched film held by a clip.
  • the temperature of the heat setting treatment is preferably in the range of stretching temperature ⁇ 0 ° C. to stretching temperature ⁇ 80 ° C., more preferably in the range of stretching temperature ⁇ 0 ° C. to stretching temperature ⁇ 50 ° C.
  • Dyeing step S30 the polyvinyl alcohol-based resin layer of the stretched film is dyed with a dichroic dye and adsorbed and oriented to form a polarizer layer. Through this step, a polarizing laminated film in which a polarizer layer is laminated on one side or both sides of a base film is obtained.
  • dichroic dye examples include iodine and dichroic organic dyes.
  • dichroic organic dye examples include, for example, Red BR, Red LR, Red R, Pink LB, Rubin BL, Bordeaux GS, Sky Blue LG, Lemon Yellow, Blue BR, Blue 2R, Navy RY, Green LG, Violet LB, Violet B, Black H, Black B, Black GSP, Yellow 3G, Yellow R, Orange LR, Orange 3R, Scarlet GL, Scarlet KGL, Congo Red, Brilliant Violet BK, Splat Blue G, Splat Blue GL, Splat Orange GL , Direct Sky Blue, Direct First Orange S, First Black, etc.
  • a dichroic dye may be used individually by 1 type, and may use 2 or more types together.
  • the dyeing step can be performed by immersing the entire stretched film in a solution (dyeing solution) containing a dichroic dye.
  • a solution in which the above dichroic dye is dissolved in a solvent can be used.
  • a solvent for the dyeing solution water is generally used, but an organic solvent compatible with water may be further added.
  • the concentration of the dichroic dye in the dyeing solution is preferably 0.01% by weight to 10% by weight, more preferably 0.02% by weight to 7% by weight, and 0.025% by weight to 5% by weight. % Is more preferable.
  • iodine When iodine is used as the dichroic dye, it is preferable to further add iodide to the dyeing solution containing iodine because the dyeing efficiency can be further improved.
  • iodide include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and titanium iodide. Is mentioned.
  • the concentration of iodide in the dyeing solution is preferably 0.01% by weight to 20% by weight. Of the iodides, it is preferable to add potassium iodide.
  • the ratio of iodine to potassium iodide is preferably in the range of 1: 5 to 1: 100, more preferably in the range of 1: 6 to 1:80, by weight. Preferably, it is in the range of 1: 7 to 1:70.
  • the immersion time of the stretched film in the dyeing solution is usually in the range of 15 seconds to 15 minutes, preferably 30 seconds to 3 minutes.
  • the temperature of the dyeing solution is preferably in the range of 10 ° C. to 60 ° C., more preferably in the range of 20 ° C. to 40 ° C. In addition, you may perform a extending
  • Embodiments in this case are as follows: 1) In the stretching step S20, after the stretching process is performed at a lower ratio than the target, the stretching process is performed so that the total stretching ratio becomes the target ratio during the dyeing process in the dyeing process S30. In the case of performing the crosslinking treatment after the dyeing treatment, as described later, 2) In the drawing step S20, after the drawing treatment at a lower magnification than the target in the drawing step S20, during the dyeing treatment in the dyeing step S30 Examples include a mode in which the stretching process is performed to such an extent that the total stretching ratio does not reach the target ratio, and then the stretching process is performed during the crosslinking process so that the final total stretching ratio becomes the target ratio.
  • the dyeing step S30 may include a crosslinking treatment step that is performed subsequent to the dyeing treatment.
  • the crosslinking treatment can be performed by immersing the dyed film in a solution containing a crosslinking agent (crosslinking solution).
  • crosslinking agent conventionally known substances can be used, and examples thereof include boron compounds such as boric acid and borax, glyoxal, and glutaraldehyde.
  • a crosslinking agent may be used individually by 1 type, and may use 2 or more types together.
  • the crosslinking solution can be a solution in which a crosslinking agent is dissolved in a solvent.
  • the solvent for example, water can be used, but an organic solvent compatible with water may be further included.
  • the concentration of the crosslinking agent in the crosslinking solution is preferably in the range of 1% by weight to 20% by weight, and more preferably in the range of 6% by weight to 15% by weight.
  • the cross-linking solution can contain iodide. By adding iodide, the polarization performance in the plane of the polarizer layer can be made more uniform.
  • iodide include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and titanium iodide. Is mentioned.
  • the concentration of iodide in the crosslinking solution is preferably 0.05% by weight to 15% by weight, and more preferably 0.5% by weight to 8% by weight.
  • the immersion time of the dyed film in the crosslinking solution is usually 15 seconds to 20 minutes, and preferably 30 seconds to 15 minutes.
  • the temperature of the crosslinking solution is preferably in the range of 10 ° C to 90 ° C.
  • a crosslinking process can also be performed simultaneously with a dyeing
  • a stretching process may be performed during the crosslinking process. The specific mode for carrying out the stretching treatment during the crosslinking treatment is as described above.
  • the washing process usually includes a water washing process.
  • the water washing treatment can be performed by immersing the film after the dyeing treatment or after the crosslinking treatment in pure water such as ion exchange water or distilled water.
  • the water washing temperature is usually in the range of 3 ° C to 50 ° C, preferably 4 ° C to 20 ° C.
  • the immersion time in water is usually 2 seconds to 300 seconds, preferably 3 seconds to 240 seconds.
  • the washing step may be a combination of a water washing step and a washing step with an iodide solution.
  • liquids such as methanol, ethanol, isopropyl alcohol, butanol, and propanol can be appropriately contained in the cleaning liquid used in the water cleaning step and / or the cleaning process using the iodide solution.
  • any appropriate method such as natural drying, air drying, and heat drying can be adopted.
  • the drying temperature is usually 20 to 95 ° C.
  • the drying time is usually about 1 to 15 minutes.
  • the polarizing laminated film obtained as described above can be used as a polarizing element as it is, and is also useful as an intermediate for producing a polarizing plate comprising a polarizer layer and a protective film.
  • the thickness of the polarizer layer of the polarizing laminate film is 10 ⁇ m or less, preferably 7 ⁇ m or less. By setting the thickness of the polarizer layer to 10 ⁇ m or less, a thin polarizing laminated film can be formed.
  • the manufacturing method of the polarizing plate of this invention is the process of preparing the above-mentioned polarizing laminated film, bonding process S40 which bonds a protective film on the polarizer layer of a polarizing laminated film, and obtains a bonding film, bonding The peeling process S50 which peels and removes the base film from the film is included in this order.
  • Pasting step S40 This step is a step of obtaining a bonding film by bonding a protective film on the polarizer layer of the polarizing laminated film, that is, on the surface opposite to the substrate film side of the polarizer layer.
  • the protective film can be bonded to the polarizer layer using an adhesive or a pressure-sensitive adhesive.
  • a protective film is normally bonded on the polarizer layers on both surfaces. In this case, these protective films may be the same type of protective film or different types of protective films.
  • the protective film is, for example, a polyolefin resin such as a chain polyolefin resin (such as a polypropylene resin) or a cyclic polyolefin resin (such as a norbornene resin); a cellulose ester resin such as cellulose triacetate or cellulose diacetate;
  • the film may be a polyester resin such as terephthalate, polyethylene naphthalate or polybutylene terephthalate; a polycarbonate resin; a (meth) acrylic resin; or a mixture or copolymer thereof. Examples of commercially available products such as cyclic polyolefin resins and films thereof, and cellulose triacetate are as described above.
  • the protective film can also be a protective film having an optical function such as a retardation film and a brightness enhancement film.
  • a retardation film provided with an arbitrary retardation value by stretching a resin film made of the above material (uniaxial stretching or biaxial stretching) or forming a liquid crystal layer or the like on the film; can do.
  • An optical layer such as a hard coat layer, an antiglare layer, or an antireflection layer can be formed on the surface of the protective film opposite to the polarizer layer.
  • the method for forming these optical layers on the surface of the protective film is not particularly limited, and a known method can be used.
  • the optical layer may be formed in advance on the protective film prior to the bonding step S40, or may be formed after the bonding step S40 or after the peeling step S50 described later.
  • plasma treatment, corona treatment, ultraviolet irradiation treatment, flame (flame) is applied to the surface of the protective film on the polarizer layer side in order to improve adhesion to the polarizer layer.
  • Treatment, saponification treatment, and other surface treatments can be performed, and among these, plasma treatment, corona treatment, or saponification treatment is preferably performed.
  • plasma treatment or corona treatment is usually performed.
  • the thickness of the protective film is preferably thin, but if it is too thin, the strength is lowered and the processability is poor. On the other hand, when too thick, problems, such as transparency falling and the curing time required after bonding, will arise. Therefore, the thickness of the protective film is preferably 90 ⁇ m or less, more preferably 5 ⁇ m to 60 ⁇ m, and still more preferably 5 ⁇ m to 50 ⁇ m.
  • the total thickness of the polarizer layer and the protective film is preferably 100 ⁇ m or less, more preferably 90 ⁇ m or less, and further preferably 80 ⁇ m or less.
  • a water-based adhesive or a photocurable adhesive can be used as the adhesive.
  • the water-based adhesive include an adhesive made of a polyvinyl alcohol-based resin aqueous solution and a water-based two-component urethane emulsion adhesive.
  • a water-based adhesive composed of an aqueous polyvinyl alcohol resin solution.
  • Polyvinyl alcohol resins include vinyl alcohol homopolymers obtained by saponifying polyvinyl acetate, which is a homopolymer of vinyl acetate, and copolymers of vinyl acetate and other monomers copolymerizable therewith.
  • a polyvinyl alcohol copolymer obtained by saponifying a polymer or a modified polyvinyl alcohol polymer obtained by partially modifying the hydroxyl group thereof can be used.
  • the water-based adhesive can include additives such as polyvalent aldehydes, water-soluble epoxy compounds, melamine compounds, zirconia compounds, and zinc compounds.
  • the thickness of the adhesive layer obtained therefrom is usually 1 ⁇ m or less.
  • a water-based adhesive is applied onto the polarizer layer and / or protective film of the polarizing laminated film, and these films are bonded through the adhesive layer, preferably pressed and bonded using a bonding roll or the like. A pasting process is carried out by making it.
  • the coating method of the water-based adhesive is not particularly limited, and casting method, Meyer bar coating method, gravure coating method, comma coater method, doctor plate method, die coating method, dip coating method A conventionally known method such as a spraying method can be used.
  • aqueous adhesive it is preferable to implement the drying process which dries a film, in order to remove the water contained in an aqueous adhesive, after implementing the above-mentioned bonding. Drying can be performed, for example, by introducing the film into a drying furnace.
  • the drying temperature temperature of the drying furnace
  • the drying temperature is preferably 30 ° C to 90 ° C.
  • the drying temperature exceeds 90 ° C., the polarizing performance of the polarizer layer may be deteriorated by heat.
  • the drying time can be about 10 seconds to 1000 seconds, and is preferably 60 seconds to 750 seconds, more preferably 150 seconds to 600 seconds from the viewpoint of productivity.
  • a curing step of curing at room temperature or slightly higher temperature for example, at a temperature of about 20 ° C. to 45 ° C. for about 12 hours to 600 hours may be provided.
  • the curing temperature is generally set lower than the drying temperature.
  • the photocurable adhesive refers to an adhesive that cures when irradiated with active energy rays such as ultraviolet rays.
  • an adhesive containing a polymerizable compound and a photopolymerization initiator, an adhesive containing a photoreactive resin, and a binder examples include those containing a resin and a photoreactive cross-linking agent.
  • the polymerizable compound include photopolymerizable monomers such as a photocurable epoxy monomer, a photocurable acrylic monomer, and a photocurable urethane monomer, and oligomers derived from the photopolymerizable monomer.
  • a photoinitiator what contains the substance which generate
  • a photocurable adhesive containing a polymerizable compound and a photopolymerization initiator an adhesive containing a photocurable epoxy monomer and a photocationic polymerization initiator can be preferably used.
  • a drying process is performed as necessary (such as when the photocurable adhesive contains a solvent), and then light is irradiated by activating active energy rays.
  • a curing step for curing the curable adhesive is performed.
  • the light source of the active energy ray is not particularly limited, but an active energy ray having a light emission distribution at a wavelength of 400 nm or less is preferable.
  • the low-pressure mercury lamp, the medium-pressure mercury lamp, the high-pressure mercury lamp, the ultrahigh-pressure mercury lamp, the chemical lamp, and the black light lamp A microwave excitation mercury lamp, a metal halide lamp and the like are preferably used.
  • the light irradiation intensity to the photocurable adhesive is appropriately determined depending on the composition of the photocurable adhesive, and the irradiation intensity in the wavelength region effective for activating the polymerization initiator is 0.1 mW / cm.
  • Irradiation intensity is 0.1 mW / cm 2 If it is above, the reaction time does not become too long, 6000 mW / cm 2 In the case of the following, there is little possibility of causing yellowing of the photocurable adhesive or deterioration of the polarizer layer due to heat radiated from the light source and heat generated when the photocurable adhesive is cured.
  • the light irradiation time to the photocurable adhesive is also determined appropriately depending on the composition of the photocurable adhesive, and the integrated light amount expressed as the product of the irradiation intensity and the irradiation time is 10 mJ / cm.
  • Integrated light quantity is 10mJ / cm 2
  • a sufficient amount of active species derived from the polymerization initiator can be generated to allow the curing reaction to proceed more reliably.
  • 10,000 mJ / cm 2 In the case of the following, the irradiation time does not become too long and good productivity can be maintained.
  • the thickness of the adhesive layer after irradiation with active energy rays is usually about 0.001 ⁇ m to 5 ⁇ m, preferably 0.01 ⁇ m to 2 ⁇ m, more preferably 0.01 ⁇ m to 1 ⁇ m.
  • the pressure-sensitive adhesive that can be used for bonding the protective film is usually based on an acrylic resin, styrene resin, silicone resin, or the like, and a crosslinking agent such as an isocyanate compound, an epoxy compound, or an aziridine compound. It consists of the added adhesive composition. Furthermore, it can also be set as the adhesive layer which contains microparticles
  • the thickness of the pressure-sensitive adhesive layer can be 1 ⁇ m to 40 ⁇ m, but it is preferably applied thinly, as long as it does not impair the workability and durability characteristics, specifically 3 ⁇ m to 25 ⁇ m.
  • a thickness of 3 ⁇ m to 25 ⁇ m has good processability and is suitable for suppressing dimensional changes of the polarizer layer.
  • the pressure-sensitive adhesive layer is less than 1 ⁇ m, the tackiness is lowered, and when it exceeds 40 ⁇ m, problems such as the pressure-sensitive adhesive protruding easily occur.
  • the protective film after the pressure-sensitive adhesive layer is provided on the protective film surface, it may be bonded to the polarizer layer, or the pressure-sensitive adhesive layer on the surface of the polarizer layer. After providing, you may paste a protective film here.
  • the method for forming the pressure-sensitive adhesive layer is not particularly limited, and a pressure-sensitive adhesive composition (pressure-sensitive adhesive solution) containing each component including the above-mentioned base polymer is applied to the protective film surface or the polarizer layer surface.
  • a pressure-sensitive adhesive composition pressure-sensitive adhesive solution
  • the protective film and the polarizer layer may be bonded together, or after forming the pressure-sensitive adhesive layer on the separator (release film), the pressure-sensitive adhesive layer is applied to the surface of the protective film.
  • it may be transferred to the polarizing film surface, the separator is peeled off from the pressure-sensitive adhesive layer, and then the protective film and the polarizer layer are bonded together.
  • peeling step S50 This step is a step of peeling and removing the base film from the bonded film obtained by bonding the protective film. Through this step, a polarizing plate in which a protective film is laminated on the polarizer layer can be obtained.
  • the polarizing laminated film has a polarizer layer on both sides of the base film, and a protective film is bonded to both of these polarizer layers, this peeling step S50 allows the two polarizing laminate films to be removed.
  • a sheet of polarizing plate is obtained.
  • the method of peeling and removing the base film is not particularly limited, and the peeling can be performed by the same method as the separator (peeling film) peeling step performed by a normal pressure-sensitive adhesive polarizing plate.
  • the base film may be peeled off as it is, or after the bonding step S40, it may be wound up into a roll and peeled off in the subsequent step.
  • the polarizing plate produced as described above can be used as an optical film in which other optical layers are laminated in practical use.
  • the protective film may have the function of such an optical layer.
  • a reflective polarizing film that transmits a certain kind of polarized light and reflects polarized light having the opposite properties
  • a film with an antiglare function having an uneven shape on the surface
  • a film with a surface antireflection function A reflective film having a reflective function on the surface
  • a transflective film having both a reflective function and a transmissive function
  • DBEF “manufactured by 3M, Sumitomo 3M Co., Ltd. in Japan) can be used as a commercial product corresponding to a reflective polarizing film that transmits certain types of polarized light and reflects polarized light that exhibits the opposite properties.
  • the viewing angle compensation film examples include an optical compensation film in which a liquid crystal compound is applied to the substrate surface, and is oriented / fixed, a retardation film made of a polycarbonate resin, a retardation film made of a cyclic polyolefin resin, and the like.
  • Commercially available products corresponding to the optical compensation film in which a liquid crystal compound is applied to the substrate surface and aligned and fixed are “WV film” (manufactured by Fujifilm Corporation), “NH film” (JX Nippon Mining & Metals).
  • the total thickness of the base film was 100 ⁇ m, and the thickness ratio (FLX80E4 / W151 / FLX80E4) of each layer was 3/4/3.
  • Polyvinyl alcohol powder (“Z-200” manufactured by Nippon Synthetic Chemical Industry Co., Ltd., average polymerization degree 1100, average saponification degree 99.5 mol%) was dissolved in hot water at 95 ° C. An aqueous alcohol solution was prepared.
  • the resulting aqueous solution was mixed with a crosslinking agent (“Smiles Resin 650” manufactured by Taoka Chemical Industry Co., Ltd.) at a ratio of 1 part by weight with respect to 2 parts by weight of the polyvinyl alcohol powder to form a primer layer forming coating solution.
  • a crosslinking agent (“Smiles Resin 650” manufactured by Taoka Chemical Industry Co., Ltd.) at a ratio of 1 part by weight with respect to 2 parts by weight of the polyvinyl alcohol powder to form a primer layer forming coating solution.
  • a crosslinking agent (“Smiles Resin 650” manufactured by Taoka Chemical Industry Co., Ltd.)
  • PVA124 manufactured by Kuraray Co., Ltd., average polymerization degree 2400, average saponification degree 98.0 mol% to 99.0 mol%
  • Polyvinyl alcohol aqueous solution was prepared, and this was used as a coating liquid for forming a polyvinyl alcohol-based resin layer.
  • a two-stage longitudinal uniaxial stretching process (free-end uniaxial stretching in the film transport direction) by a nip roll stretching method. )
  • the stretching temperature atmospheric temperature in the heating furnaces 20 and 30
  • the draw ratio in the first and second steps was adjusted to 2.00 times and 2.90 times by adjusting the peripheral speeds of the nip rolls 1, 2, 3, and 4, respectively.
  • the total draw ratio is 5.80 times.
  • the thickness of the polyvinyl alcohol-type resin layer in a stretched film one side was 4.6 micrometers and the other was 4.8 micrometers. The resulting stretched film was not wrinkled by stretching.
  • a crosslinking treatment was performed by dipping in a crosslinking solution at 76 ° C. containing boric acid and potassium iodide so that the residence time was 600 seconds. Thereafter, the film was washed with pure water at 10 ° C. for 4 seconds and dried at 80 ° C. for 300 seconds to prepare a polarizing laminated film.
  • polarizing plate Bonding process and peeling process
  • Polyvinyl alcohol powder (“KL-318” manufactured by Kuraray Co., Ltd., average polymerization degree 1800) was dissolved in hot water at 95 ° C. to prepare a polyvinyl alcohol aqueous solution having a concentration of 3% by weight.
  • the resulting aqueous solution was mixed with a crosslinking agent (“Smile Resin 650” manufactured by Taoka Chemical Co., Ltd.) at a ratio of 1 part by weight to 2 parts by weight of the polyvinyl alcohol powder to obtain an aqueous adhesive solution.
  • a crosslinking agent (“Smile Resin 650” manufactured by Taoka Chemical Co., Ltd.) at a ratio of 1 part by weight to 2 parts by weight of the polyvinyl alcohol powder
  • Example 2 A polarizing plate was produced in the same manner as in Example 1 except that the draw ratios in the first and second steps were 2.50 times and 2.32 times (total draw ratio 5.80 times), respectively. did.
  • the thickness of the polyvinyl alcohol-type resin layer in a stretched film one was 4.8 micrometers and the other was 5.0 micrometers. No wrinkles were observed in the stretched film, the thickness difference in the film width direction was 2 ⁇ m, and the stretching was performed uniformly.
  • the pasting step and the peeling step proceeded without any problem, and a polarizing plate on which a protective film was laminated could be obtained.
  • Example 3 A polarizing plate was produced in the same manner as in Example 1 except that the stretching ratios in the first and second stretching processes were 2.80 times and 2.07 times (total stretching ratio 5.80 times), respectively. did.
  • the thickness of the polyvinyl alcohol-type resin layer in a stretched film one side was 5.2 micrometers and the other was 5.4 micrometers. No wrinkles were observed in the stretched film, the thickness difference in the film width direction was 2 ⁇ m, and the stretching was performed uniformly. The pasting step and the peeling step proceeded without any problem, and a polarizing plate on which a protective film was laminated could be obtained.
  • Example 4 A polarizing plate was produced in the same manner as in Example 1 except that the stretching ratios in the first and second stretching processes were 3.40 times and 1.70 times (total stretching ratio 5.78 times), respectively. did.
  • the thickness of the polyvinyl alcohol-type resin layer in a stretched film one side was 5.1 micrometers and the other was 5.3 micrometers. No wrinkles were observed in the stretched film, the thickness difference in the film width direction was 2 ⁇ m, and the stretching was performed uniformly. The pasting step and the peeling step proceeded without any problem, and a polarizing plate on which a protective film was laminated could be obtained.
  • ⁇ Comparative Example 1> A stretched film was produced in the same manner as in Example 1 except that the stretching ratio in the first-stage stretching treatment was 5.80 times and the second-stage stretching treatment was not performed. In the obtained stretched film, strong wrinkles were generated in the stretching direction.
  • ⁇ Comparative Example 2> A stretched film is produced in the same manner as in Example 1 except that the stretching ratio in the first and second stretching processes is 1.54 times and 3.80 times (total stretching ratio 5.85 times), respectively. did.
  • the thickness of the polyvinyl alcohol-type resin layer in a stretched film one side was 4.7 micrometers and the other was 5.2 micrometers.
  • Stretch ratio in the first and second stage stretching processes stretch ratio (ratio of stretch ratio in the first stage stretching process to stretch ratio in the second stage stretching process), total stretch ratio, and stretching Table 1 summarizes the measurement results of wrinkles and thickness differences in the film width direction.
  • the occurrence of wrinkles and stretching unevenness in the film width direction during the stretching of the laminated film can be effectively suppressed.
  • a good polarizing laminate film or polarizing plate can be produced with good yield.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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