WO2012147633A1 - 光学フィルム用粘着剤層およびその製造方法、粘着型光学フィルムおよびその製造方法、画像表示装置ならびに塗布液供給装置 - Google Patents
光学フィルム用粘着剤層およびその製造方法、粘着型光学フィルムおよびその製造方法、画像表示装置ならびに塗布液供給装置 Download PDFInfo
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- WO2012147633A1 WO2012147633A1 PCT/JP2012/060666 JP2012060666W WO2012147633A1 WO 2012147633 A1 WO2012147633 A1 WO 2012147633A1 JP 2012060666 W JP2012060666 W JP 2012060666W WO 2012147633 A1 WO2012147633 A1 WO 2012147633A1
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- Prior art keywords
- pressure
- sensitive adhesive
- optical film
- adhesive layer
- meth
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Classifications
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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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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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
- C09J201/00—Adhesives based on unspecified macromolecular 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
-
- 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
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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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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
-
- 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
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249982—With component specified as adhesive or bonding agent
- Y10T428/249983—As outermost component
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T428/2848—Three or more layers
Definitions
- the present invention relates to an optical film pressure-sensitive adhesive layer in which appearance defects due to bubbles and / or foreign matters are reduced, a method for producing the same, and an adhesive optical film in which an adhesive layer is laminated on at least one side of the optical film.
- the present invention also relates to a pressure-sensitive adhesive optical film having reduced appearance defects in the pressure-sensitive adhesive layer and a method for producing the same.
- an adhesive type optical film a polarizing plate, a phase difference plate, an optical compensation film, a brightness enhancement film, a surface treatment film such as an antireflection film, etc., and these layers are laminated on at least one side. are listed.
- the present invention provides an image display device using at least one of the pressure-sensitive adhesive optical film, and a coating liquid supply device for supplying a pressure-sensitive adhesive coating liquid that is a raw material of the pressure-sensitive adhesive layer constituting the pressure-sensitive adhesive optical film.
- a coating liquid supply device for supplying a pressure-sensitive adhesive coating liquid that is a raw material of the pressure-sensitive adhesive layer constituting the pressure-sensitive adhesive optical film.
- liquid crystal display devices and organic EL display devices for example, in liquid crystal display devices, it is indispensable to dispose polarizing elements on both sides of the liquid crystal cell, and in general, polarizing plates are attached.
- polarizing plates various optical elements have been used for display panels such as liquid crystal panels and organic EL panels in order to improve the display quality of displays.
- a front plate is used to protect an image display device such as a liquid crystal display device, an organic EL display device, a CRT, or a PDP, to give a high-class feeling, or to differentiate a design.
- a viewing angle widening film For members used together with image display devices such as liquid crystal display devices and organic EL display devices, and image display devices such as front plates, for example, retardation plates for preventing coloring, and for improving the viewing angle of liquid crystal displays
- a viewing angle widening film a brightness enhancement film for increasing the contrast of a display, a hard coat film used for imparting scratch resistance to the surface, an anti-glare treatment film for preventing reflection on an image display device,
- Surface treatment films such as antireflection films such as reflective films and low reflective films are used. These films are collectively called optical films.
- an adhesive is usually used.
- the adhesion between the optical film and the display panel such as the liquid crystal cell and the organic EL panel, or the front plate, or the optical film is usually made by adhering each material using an adhesive to reduce light loss. Yes.
- an adhesive optical film in which an adhesive layer is laminated on at least one side of the optical film is generally used because it has a merit that a drying process is not required to fix the optical film. Used.
- Adhesive optical films are used in image display devices that are directly viewed, and therefore, the adhesive layer is subjected to extremely strict quality control against appearance defects (streak defects, point defects) caused by foreign matters or bubbles.
- the pressure-sensitive adhesive coating solution that is the raw material of the pressure-sensitive adhesive layer is generally applied onto the optical film through vacuum defoaming treatment, centrifugal separation treatment, and filtration treatment as necessary.
- vacuum defoaming treatment centrifugal separation treatment
- filtration treatment as necessary.
- the viscosity of the coating solution is high or if bubbles having a minute bubble diameter are removed, a great deal of time and effort is required.
- the removal of bubbles is insufficient.
- Patent Document 1 a coating solution containing a solvent and a monomer component curable by actinic radiation (so-called “solvent” for the purpose of removing a component that generates a small amount of repellency defects such as polydimethylsiloxane.
- System coating solution at least including a step of filtering with a depth type filter having a polyolefin filter material, and a coating step of coating the filtered coating solution on a film substrate to form a coating layer,
- Such a method described in the patent document is useful as a means for removing foreign matters and bubbles that cause a defect of 100 ⁇ m or more in the case of a solvent-based coating solution having a generally low viscosity.
- a water-dispersed adhesive such as an emulsion solution in which foam biting is likely to occur, or an adhesive having a higher viscosity than a solvent-based coating liquid.
- agent coating solution it was found that the removal efficiency of bubbles and / or foreign matters was inferior.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to effectively remove bubbles and / or foreign matters in the pressure-sensitive adhesive coating liquid that is a raw material of the pressure-sensitive adhesive layer.
- Pressure-sensitive adhesive layer for optical film with reduced defects and method for producing the same, pressure-sensitive adhesive optical film on which the pressure-sensitive adhesive layer for optical film is laminated, method for producing the same, image display device, and pressure-sensitive adhesive for forming the pressure-sensitive adhesive layer The object is to provide a coating liquid supply apparatus.
- a pressure-sensitive adhesive coating liquid containing a water-dispersed pressure-sensitive adhesive as a main component is liable to cause foam biting, and has minute bubbles, specifically Has a special problem that is not easily seen in the solvent-based coating solution, and (ii) the adhesive coating solution having a higher viscosity than the solvent-based coating solution is filtered.
- the differential pressure is high, bubbles and / or foreign matters tend to easily pass through the filter while being deformed.
- the present invention has been made as a result of the above-described studies, and achieves the above-described object with the following configuration.
- the method for producing the pressure-sensitive adhesive layer for optical films according to the present invention uses a depth type filter having a filtration accuracy of 1 to 20 ⁇ m, and a pressure-sensitive adhesive coating solution containing a water-dispersed pressure-sensitive adhesive has a differential pressure. It is characterized by including the filtration process filtered in the state of 150 kPa or less, and the application
- the depth type filter has a gradient in filtration accuracy.
- the pressure-sensitive adhesive layer for an optical film according to the present invention is produced by any one of the production methods described above, and particularly does not contain bubbles and / or foreign matter having a maximum length exceeding 100 ⁇ m, and In the surface of the pressure-sensitive adhesive layer, the number of bubbles and / or foreign matters having a maximum length of 20 ⁇ m or more is preferably 10 / m 2 or less.
- the cause of the appearance defect of the pressure-sensitive adhesive layer may be only bubbles present in the pressure-sensitive adhesive coating liquid, or may be only foreign matter, or bubbles present in the pressure-sensitive adhesive coating liquid and It can be both foreign matter.
- the method for producing an adhesive optical film according to the present invention is a method for producing an adhesive optical film in which an adhesive layer is laminated on at least one side of the optical film, and the step of producing the adhesive layer comprises And a filtration step of using a depth type filter to filter the pressure-sensitive adhesive coating liquid as a raw material of the pressure-sensitive adhesive layer in a state where the differential pressure exceeds 0 kPa and 150 kPa or less, and the pressure-sensitive adhesive coating liquid is And a water-dispersed pressure-sensitive adhesive, wherein the depth-type filter has a filtration accuracy of 1 to 20 ⁇ m.
- the depth type filter preferably has a gradient in filtration accuracy.
- the said adhesive coating liquid is apply
- the method further includes a coating / drying step of drying after applying the pressure-sensitive adhesive coating solution on the optical film after the filtration step.
- the pressure-sensitive adhesive optical film according to the present invention is manufactured by any one of the manufacturing methods described above.
- an image display device according to the present invention is characterized by using at least one adhesive optical film described above.
- a coating liquid supply apparatus is a coating liquid supply apparatus for supplying an adhesive coating liquid that is a raw material for an adhesive layer constituting an adhesive optical film, and at least feeds the adhesive coating liquid.
- a filtration unit for removing air bubbles and / or foreign matters contained in the adhesive coating solution, and a liquid feeding unit for transferring the adhesive coating solution.
- the method for producing an optical film pressure-sensitive adhesive layer according to the present invention includes a step of filtering a pressure-sensitive adhesive coating solution containing a water-dispersed pressure-sensitive adhesive.
- a water-dispersed pressure-sensitive adhesive generally tends to cause foam biting as compared with a solvent-based coating solution having a low viscosity, and has a relatively high viscosity, and therefore tends to contain fine bubbles, specifically bubbles of less than 100 ⁇ m.
- a depth type filter is used, and the pressure-sensitive adhesive coating liquid that is the raw material of the pressure-sensitive adhesive layer is in a state where the differential pressure exceeds 0 kPa and 150 kPa or less
- the filtration accuracy of the depth type filter is 1 to 20 ⁇ m, and it is reliable and efficient even for minute bubbles and / or foreign matters, especially bubbles and / or foreign matters less than 100 ⁇ m. Can be removed well.
- a depth-type filter that has a gradient in filtration accuracy and a high filtration accuracy toward the downstream side, large bubbles and / or foreign matter are collected on the upstream side, and the flow proceeds toward the downstream side.
- the method for producing an adhesive layer for an optical film according to the present invention has such a viscosity because the efficiency of removing bubbles and / or foreign matter is high with respect to an adhesive coating solution having a viscosity of 5 to 50000 mPa ⁇ s. This is particularly useful when an adhesive coating solution is used as a raw material.
- a depth type filter can be installed in the manufacturing process, especially the application process of an adhesive coating liquid, and there is little influence on an adhesive coating liquid. Therefore, it is convenient even when compared with other defoaming methods (for example, vacuum defoaming or centrifugation).
- the pressure-sensitive adhesive layer for an optical film in which appearance defects are extremely reduced, in particular, does not contain bubbles and / or foreign matters having a maximum length exceeding 100 ⁇ m, and
- a pressure-sensitive adhesive layer for an optical film having a maximum length of 20 ⁇ m or more and / or the number of foreign matters within 10 / m 2 can be produced.
- Such an adhesive layer is useful as a member for an optical film.
- the method for producing an adhesive optical film according to the present invention includes a step of filtering an adhesive coating solution containing a water-dispersed adhesive.
- a water-dispersed pressure-sensitive adhesive generally tends to cause foam biting as compared with a solvent-based coating solution having a low viscosity, and has a relatively high viscosity, and therefore tends to contain fine bubbles, specifically bubbles of less than 100 ⁇ m.
- a depth type filter is used, and the adhesive coating liquid as a raw material for the adhesive layer is filtered in a state where the differential pressure exceeds 0 kPa and is 150 kPa or less.
- the filtration process of the depth type filter is 1 to 20 ⁇ m, it is possible to reliably and efficiently remove even fine bubbles and / or foreign materials, especially bubbles and / or foreign materials of less than 100 ⁇ m. can do.
- a depth-type filter that has a gradient in filtration accuracy and a high filtration accuracy toward the downstream side, large bubbles and / or foreign matter are collected on the upstream side, and the flow proceeds toward the downstream side. Small air bubbles and / or foreign matter can be collected. For this reason, the removal efficiency of bubbles and / or foreign matters can be enhanced while extending the filter life.
- the method for producing an adhesive optical film according to the present invention has a high efficiency of removing bubbles and / or foreign matter with respect to an adhesive coating liquid having a viscosity of 5 to 50000 mPa ⁇ s. This is particularly useful when the coating solution is used as a raw material.
- a depth type filter can be installed during the production process, particularly during the application process of the adhesive coating liquid, and has little influence on the adhesive coating liquid. It is also convenient compared with other defoaming methods (for example, vacuum defoaming or centrifugation).
- the pressure-sensitive adhesive optical film on which the pressure-sensitive adhesive layer is laminated may be manufactured by further including a coating / drying step in which the pressure-sensitive adhesive coating solution is coated on the optical film and then dried. . Moreover, after the said filtration process, the said adhesive coating liquid is apply
- the pressure-sensitive adhesive layer was laminated by further including a drying step and a transfer step of transferring the pressure-sensitive adhesive layer onto the optical film from the flexible support (web) provided with the pressure-sensitive adhesive layer.
- An adhesive optical film may be manufactured. In the latter case, since the optical film can be prevented from being heated in the drying step by heating, an adhesive optical film can be produced while maintaining the optical properties of the optical film.
- an adhesive optical film with reduced appearance defects in the adhesive layer can be produced.
- the image display apparatus using at least one such adhesive optical film has reduced appearance defects as well.
- the coating liquid supply apparatus can reliably and efficiently remove bubbles and / or foreign matters that cause appearance defects from the coating liquid. For this reason, it is useful as an apparatus for producing an adhesive optical film.
- the method for producing a pressure-sensitive adhesive layer for an optical film uses a depth-type filter having a filtration accuracy of 1 to 20 ⁇ m, and applies a pressure-sensitive adhesive coating solution containing a water-dispersed pressure-sensitive adhesive to a differential pressure of 0 kPa. And a filtration step of filtration in a state of 150 kPa or less, and a coating / drying step of drying after applying the pressure-sensitive adhesive coating solution after the filtration treatment.
- the adhesive coating solution contains a water-dispersed adhesive.
- adhesive coating liquids include various viscosity modifiers, release modifiers, tackifiers, plasticizers, softeners, glass fibers, glass beads, metal powders, and other inorganic substances. It can contain a filler made of powder or the like, a pigment, a colorant (pigment, dye, etc.), a pH adjuster (acid or base), an antioxidant, an ultraviolet absorber, a silane coupling agent and the like.
- the water-dispersed pressure-sensitive adhesive is an aqueous dispersion in which at least a base polymer is dispersed and contained in water.
- a dispersion in which a base polymer is dispersed in the presence of a surfactant is usually used. If the base polymer is dispersed and contained in water, a self-dispersing base polymer is used. A water dispersion can be used by self-dispersion.
- Examples of the base polymer in the aqueous dispersion include those obtained by polymerizing a monomer by emulsion polymerization in the presence of an emulsifier or by dispersion polymerization in the presence of a surfactant.
- the aqueous dispersion can be produced by emulsifying and dispersing a separately produced base polymer in water in the presence of an emulsifier.
- an emulsification method a polymer and an emulsifier are heated and melted in advance, or without being heated and melted, and they and water are subjected to high shear using a mixer such as a pressure kneader, a colloid mill, and a high-speed stirring shaft. And then uniformly emulsify and disperse, then cool the dispersed particles so that they do not melt and aggregate (high pressure emulsification method), or polymer in advance in an organic solvent such as benzene, toluene or ethyl acetate.
- an organic solvent such as benzene, toluene or ethyl acetate.
- the emulsifier and water are added, and the mixture is uniformly emulsified and dispersed by applying high shear using, for example, a high-speed emulsifier, and then the organic solvent is removed by reduced pressure-heating treatment or the like to obtain a desired aqueous dispersion. (Solvent dissolution method) and the like.
- Various adhesives can be used as the water-dispersed adhesive, such as rubber adhesives, acrylic adhesives, silicone adhesives, polyurethane adhesives, vinyl alkyl ether adhesives, polyvinyl alcohol adhesives. Examples thereof include a pressure-sensitive adhesive, a polyvinyl pyrrolidone pressure-sensitive adhesive, a polyacrylamide-based pressure-sensitive adhesive, a cellulose-based pressure-sensitive adhesive, a polyester-based pressure-sensitive adhesive, and a fluorine-based pressure-sensitive adhesive.
- An adhesive base polymer and a dispersing means are selected according to the type of the adhesive.
- the present invention is excellent in optical transparency, exhibits appropriate wettability, cohesiveness, and adhesive pressure-sensitive adhesive properties, and is excellent in weather resistance, heat resistance, and the like.
- a system adhesive is preferably used.
- the (meth) acrylic polymer which is the base polymer for water-dispersed acrylic pressure-sensitive adhesives, is, for example, emulsion polymerization of a monomer component mainly composed of (meth) acrylic acid alkyl ester in the presence of an emulsifier and a radical polymerization initiator. To obtain a copolymer emulsion.
- the (meth) acrylic acid alkyl ester refers to an acrylic acid alkyl ester and / or a methacrylic acid alkyl ester, and (meth) in the present invention has the same meaning.
- the alkyl group includes a methyl group, an ethyl group, a propyl group, an isopropyl group, an n-butyl group, an isobutyl group, a sec-butyl group, a t-butyl group, a pentyl group, a neopentyl group, an isoamyl group, a hexyl group, Heptyl, 2-ethylhexyl, isooctyl, nonyl, isononyl, decyl, isodecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl
- alkyl groups preferably have an average carbon number of 3 to 9.
- a monomer having a boiling point higher than that of water such as butyl acrylate, is particularly preferably used as the (meth) acrylic acid alkyl ester.
- the adhesive layer is improved in adhesion to a support substrate such as an optical film.
- a support substrate such as an optical film
- copolymerization monomers having a polymerizable functional group related to an unsaturated double bond such as a (meth) acryloyl group or a vinyl group are introduced by copolymerization. be able to.
- the copolymerization monomer examples include carboxyl group-containing monomers such as (meth) acrylic acid, itaconic acid, maleic acid, fumaric acid, crotonic acid, carboxyethyl acrylate, and carboxypentyl acrylate; , Maleic anhydride, itaconic anhydride and other acid anhydride group-containing monomers; for example, (meth) acrylic alicyclic carbonization such as cyclohexyl (meth) acrylate, bornyl (meth) acrylate, isobornyl (meth) acrylate Hydrogen esters; for example, (meth) acrylic acid aryl esters such as phenyl (meth) acrylate, for example, vinyl esters such as vinyl acetate and vinyl propionate; for example, styrene monomers such as styrene and ⁇ -methylstyrene; , (Meth) acrylic acid Epoxy group-containing monomers such as (meth) acrylic acid
- copolymerizable monomers include maleimide monomers such as N-cyclohexylmaleimide, N-isopropylmaleimide, N-laurylmaleimide, and N-phenylmaleimide; for example, N-methylitaconimide, N-ethylitaconimide, N Itaconimide monomers such as butyl itaconimide, N-octyl itaconimide, N-2-ethylhexylitaconimide, N-cyclohexyl itaconimide, N-lauryl itaconimide; N- (meth) acryloyloxymethylene succinimide, N- Succinimide monomers such as (meth) acryloyl-6-oxyhexamethylene succinimide and N- (meth) acryloyl-8-oxyoctamethylene succinimide; for example, styrene sulfonic acid Examples include sulfonic acid group
- Examples of the copolymerizable monomer include a phosphate group-containing monomer.
- Examples of the phosphate group-containing monomer include the following general formula (1): (In the general formula (1), R 1 represents a hydrogen atom or a methyl group, R 2 represents an alkylene group having 1 to 4 carbon atoms, m represents an integer of 2 or more, and M 1 and M 2 are each independently Represents a hydrogen atom or a cation).
- the phosphoric acid group containing monomer represented by this is mentioned.
- m is 2 or more, preferably 4 or more and usually 40 or less, and m represents the degree of polymerization of the oxyalkylene group.
- the polyoxyalkylene group include a polyoxyethylene group and a polyoxypropylene group, and these polyoxyalkylene groups may be random, block or graft units.
- the cation according to the salt of the phosphate group is not particularly limited, for example, an alkali metal such as sodium or potassium, for example, an inorganic cation such as an alkaline earth metal such as calcium or magnesium, for example, a quaternary amine And organic cations.
- glycol-based acrylic ester monomers such as polyethylene glycol (meth) acrylate, polypropylene glycol (meth) acrylate, methoxyethylene glycol (meth) acrylate, and methoxypolypropylene glycol (meth) acrylate
- examples include, for example, tetrahydrofurfuryl (meth) acrylate, a heterocyclic ring such as fluorine (meth) acrylate, and an acrylate monomer containing a halogen atom.
- examples of the copolymerizable monomer include silicone unsaturated monomers.
- Silicone unsaturated monomers include silicone (meth) acrylate monomers and silicone vinyl monomers.
- silicone-based (meth) acrylate monomers include (meth) acryloyloxymethyl-trimethoxysilane, (meth) acryloyloxymethyl-triethoxysilane, 2- (meth) acryloyloxyethyl-trimethoxysilane, 2- ( (Meth) acryloyloxyethyl-triethoxysilane, 3- (meth) acryloyloxypropyl-trimethoxysilane, 3- (meth) acryloyloxypropyl-triethoxysilane, 3- (meth) acryloyloxypropyl-tripropoxysilane, 3 -(Meth) acryloyloxyalkyl-trialkoxysilanes such as (meth) acryloyloxy
- silicone-based vinyl monomer examples include vinyltrialkoxysilanes such as vinyltrimethoxysilane, vinyltriethoxysilane, vinyltripropoxysilane, vinyltriisopropoxysilane, vinyltributoxysilane, and vinyl corresponding to these.
- Alkyldialkoxysilanes and vinyldialkylalkoxysilanes such as vinylmethyltrimethoxysilane, vinylmethyltriethoxysilane, ⁇ -vinylethyltrimethoxysilane, ⁇ -vinylethyltriethoxysilane, ⁇ -vinylpropyltrimethoxysilane, ⁇ -Vinylalkyl such as vinylpropyltriethoxysilane, ⁇ -vinylpropyltripropoxysilane, ⁇ -vinylpropyltriisopropoxysilane, ⁇ -vinylpropyltributoxysilane Another trialkoxysilane, these correspond and (vinyl) alkyl dialkoxy silanes, and the like (vinyl alkyl) dialkyl (mono) alkoxysilanes.
- a polyfunctional monomer can be used as the copolymerizable monomer for adjusting the gel fraction of the water-dispersed pressure-sensitive adhesive.
- the polyfunctional monomer include compounds having two or more unsaturated double bonds such as a (meth) acryloyl group and a vinyl group.
- alkylene glycol di (meth) acrylates such as ethylene glycol di (meth) acrylate and (mono or poly) propylene glycol di (meth) acrylate such as propylene glycol di (meth) acrylate, neopentyl glycol Di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, pentaerythritol di (meth) acrylate, trimethylolpropane tri (meth) acrylate , Esterified product of (meth) acrylic acid and polyhydric alcohol such as pentaerythritol tri (meth) acrylate and dipentaerythritol hexa (meth) acrylate; polyfunctional vinyl compound such as divinylbenzene; allyl (meth) acrylate, ( Examples thereof include compounds having a reactive unsaturated double bond such as (meth) vinyl acrylate
- polyester (meta) having two or more unsaturated double bonds such as (meth) acryloyl group and vinyl group as functional groups similar to the monomer component is added to a skeleton such as polyester, epoxy, and urethane.
- a skeleton such as polyester, epoxy, and urethane.
- Acrylate, epoxy (meth) acrylate, urethane (meth) acrylate, and the like can also be used.
- acrylics are used from the viewpoint of stabilizing aqueous dispersions (emulsions, etc.) and ensuring adhesion to glass panels that are adherends of adhesive layers formed from the aqueous dispersions.
- a carboxyl group-containing monomer such as an acid, a phosphate group-containing monomer, or a silicone-based unsaturated monomer is preferably used.
- the (meth) acrylic polymer is mainly composed of (meth) acrylic acid alkyl ester, and the blending ratio thereof is 50% by weight or more, preferably 60% by weight or more, more preferably, based on the total amount of the monomer components. Is 70% by weight or more.
- the upper limit in particular is not restrict
- pressure-sensitive adhesive properties such as adhesive strength of the pressure-sensitive adhesive layer may be lowered.
- the blending ratio of the copolymerizable monomer is, for example, less than 50% by weight, preferably less than 40% by weight, and more preferably less than 30% by weight with respect to the total amount of the monomer components.
- the blending ratio of the copolymerizable monomer can be appropriately selected according to the type of each copolymerizable monomer.
- the proportion is preferably 0.1 to 6% by weight based on the total amount of the monomer components, and when the copolymerizable monomer is a phosphate group-containing monomer, the proportion is 0.5%.
- the ratio is preferably 0.005 to 0.2% by weight.
- Emulsion polymerization of the monomer component is performed by emulsion polymerization after emulsifying the monomer component in water by a conventional method. Thereby, a (meth) acrylic polymer aqueous dispersion is prepared.
- emulsion polymerization for example, an emulsifier, a radical polymerization initiator, and, if necessary, a chain transfer agent are appropriately blended in water together with the monomer components described above. More specifically, for example, known emulsion polymerization methods such as a batch charging method (batch polymerization method), a monomer dropping method, and a monomer emulsion dropping method can be employed. In the monomer dropping method and the monomer emulsion dropping method, continuous dropping or divided dropping is appropriately selected. These methods can be appropriately combined. The reaction conditions and the like are appropriately selected.
- the polymerization temperature is, for example, about 0 to 150 ° C., and the polymerization time is about 2 to 15 hours.
- the emulsifier is not particularly limited, and various emulsifiers usually used for emulsion polymerization are used.
- various emulsifiers usually used for emulsion polymerization are used.
- sodium lauryl sulfate, ammonium lauryl sulfate, sodium dodecylbenzene sulfonate sodium polyoxyethylene lauryl sulfate, sodium polyoxyethylene alkyl ether sulfate, ammonium polyoxyethylene alkyl phenyl ether sulfate, sodium polyoxyethylene alkyl phenyl ether sulfate, polyoxyethylene Anionic emulsifiers such as sodium alkylsulfosuccinate; for example, nonionic emulsifiers such as polyoxyethylene alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene fatty acid ester, polyoxyethylene polyoxypropylene block polymer, and the like.
- radically polymerizable emulsifiers in which radically polymerizable functional groups (radical reactive groups) such as propenyl groups and allyl ether groups are introduced into these anionic and nonionic emulsifiers are listed. These emulsifiers are used alone or in combination as appropriate. Among these emulsifiers, a radical polymerizable emulsifier having a radical polymerizable functional group is preferably used from the viewpoint of the stability of the aqueous dispersion (emulsion) and the durability of the pressure-sensitive adhesive layer.
- the blending ratio of the emulsifier is, for example, about 0.1 to 5 parts by weight, preferably 0.4 to 3 parts by weight with respect to 100 parts by weight of the monomer component mainly composed of the (meth) acrylic acid alkyl ester. is there.
- the blending ratio of the emulsifier is within this range, it is possible to improve water resistance, adhesive properties, polymerization stability, mechanical stability, and the like.
- the radical polymerization initiator is not particularly limited, and a known radical polymerization initiator usually used for emulsion polymerization is used.
- a known radical polymerization initiator usually used for emulsion polymerization is used.
- 2,2′-azobisisobutyronitrile, 2,2′-azobis (2-methylpropionamidine) disulfate, 2,2′-azobis (2-methylpropionamidine) dihydrochloride, 2, Azo initiators such as 2′-azobis (2-amidinopropane) dihydrochloride, 2,2′-azobis [2- (2-imidazolin-2-yl) propane] dihydrochloride; for example, potassium persulfate, Persulfate initiators such as ammonium persulfate; peroxide initiators such as benzoyl peroxide, t-butyl hydroperoxide, hydrogen peroxide; substituted ethane initiators such as phenyl substituted ethane; And carbonyl-
- an azo radical polymerization disclosure agent is preferable because it can improve the transparency of the pressure-sensitive adhesive layer formed in the present invention.
- These polymerization initiators are suitably used alone or in combination.
- the blending ratio of the radical polymerization initiator is appropriately selected. For example, about 0.02 to 0.5 parts by weight, preferably 0.08 to 0.3 parts by weight with respect to 100 parts by weight of the monomer component. Part. When the amount is less than 0.02 part by weight, the effect as a radical polymerization initiator may be reduced. When the amount exceeds 0.5 part by weight, the molecular weight of the water-dispersed (meth) acrylic polymer decreases, The adhesiveness of the dispersion-type pressure-sensitive adhesive composition may decrease.
- the chain transfer agent adjusts the molecular weight of the water-dispersed (meth) acrylic polymer as necessary, and a chain transfer agent usually used for emulsion polymerization is used.
- a chain transfer agent usually used for emulsion polymerization examples thereof include mercaptans such as 1-dodecanethiol, mercaptoacetic acid, 2-mercaptoethanol, 2-ethylhexyl thioglycolate, 2,3-dimethylcapto-1-propanol, and mercaptopropionic acid esters.
- These chain transfer agents are appropriately used alone or in combination.
- the blending ratio of the chain transfer agent is, for example, 0.001 to 0.3 parts by weight with respect to 100 parts by weight of the monomer component.
- a water-dispersed (meth) acrylic polymer can be prepared as an aqueous dispersion (emulsion).
- the average particle diameter of such a water-dispersed (meth) acrylic polymer is adjusted to, for example, 0.05 to 3 ⁇ m, preferably 0.05 to 1 ⁇ m. If the average particle size is less than 0.05 ⁇ m, the viscosity of the water-dispersed pressure-sensitive adhesive may increase. If it is greater than 1 ⁇ m, the adhesion between particles may decrease and the cohesive force may decrease.
- the (meth) acrylic polymer according to the aqueous dispersion contains a carboxyl group-containing monomer as a copolymerizable monomer. It is preferable to neutralize monomers and the like. Neutralization can be performed, for example, with ammonia, alkali metal hydroxide, or the like.
- the water-dispersed (meth) acrylic polymer of the present invention preferably has a weight average molecular weight of 1 million or more.
- those having a weight average molecular weight of 1,000,000 to 4,000,000 are preferred in terms of heat resistance and moisture resistance.
- heat resistance and moisture resistance are lowered, which is not preferable.
- the pressure-sensitive adhesive obtained by emulsion polymerization is preferable because its molecular weight becomes very high due to its polymerization mechanism.
- the pressure-sensitive adhesive obtained by emulsion polymerization generally has a large gel content and cannot be measured by GPC (gel permeation chromatography), it is often difficult to support the actual measurement regarding molecular weight.
- the water-dispersed pressure-sensitive adhesive used in the present invention can contain a crosslinking agent in addition to the above base polymer.
- a crosslinking agent used when the water-dispersed pressure-sensitive adhesive is a water-dispersed acrylic pressure-sensitive adhesive include isocyanate-based crosslinking agents, epoxy-based crosslinking agents, oxazoline-based crosslinking agents, aziridine-based crosslinking agents, carbodiimide-based crosslinking agents, and metal chelates. Commonly used materials such as a system cross-linking agent can be used. These crosslinking agents have the effect of reacting with a functional group introduced into the polymer and crosslinking by using a functional group-containing monomer.
- the blending ratio of the base polymer and the crosslinking agent is not particularly limited, but is usually blended at a ratio of about 10 parts by weight or less of the crosslinking agent (solid content) with respect to 100 parts by weight of the base polymer (solid content).
- the blending ratio of the crosslinking agent is preferably 0.001 to 10 parts by weight, more preferably about 0.01 to 5 parts by weight.
- the pressure-sensitive adhesive coating liquid containing a water-dispersed pressure-sensitive adhesive as a main component has a viscosity of 5 to 50000 mPa ⁇ s. It is preferable to use a certain pressure-sensitive adhesive coating liquid, more preferably a pressure-sensitive adhesive coating liquid having a pressure of 50 to 20000 mPa ⁇ s, and particularly preferably a pressure-sensitive adhesive coating liquid having a pressure of 200 to 10,000 mPa ⁇ s.
- the depth type filter used in the filtration step of the adhesive coating solution that is the raw material of the adhesive layer is a polyolefin-based filter.
- a void is formed by using a composite fiber, a heat-adhesive polyester fiber, or the like and thermally bonding the entanglement points of the fiber.
- a pleated type filter that filters on the surface of the filter medium is small when the filter medium is crushed when it is repeatedly used in the filtration process, or when the differential pressure during filtration is large, bubbles and / or foreign matters are easily deformed by the pressure.
- a depth type filter can be used conveniently in the filtration process of the adhesive coating liquid which concerns on this invention.
- the depth type filter is usually marketed as a cartridge type filter, and a commercially available depth type filter can also be suitably used.
- a depth type filter having a filtration accuracy of 1 to 20 ⁇ m is used.
- the filtration pore diameter is too large, and bubbles and / or foreign matters are likely to pass through the filter. In particular, the efficiency of removing bubbles and / or foreign matters less than 100 ⁇ m is lowered.
- the filtration accuracy of the depth type filter should be 1 to 10 ⁇ m Is preferably 5 to 10 ⁇ m.
- the pressure difference of the depth type filter is set to exceed 0 kPa and to 150 kPa or less.
- the differential pressure exceeds 150 kPa, bubbles and / or foreign matters are deformed by the pressure and easily pass through the filter, and in particular, the efficiency of removing bubbles and / or foreign matters less than 100 ⁇ m is deteriorated.
- the lower limit of the differential pressure is not particularly limited, but if it is too low, the time required for the filtration process becomes longer, so it is preferable to set it to exceed 0 kPa.
- the differential pressure of the depth type filter is preferably more than 0 kPa and not more than 130 kPa, more preferably more than 0 kPa and not more than 100 kPa. .
- the depth type filter having a gradient in filtration accuracy and having high filtration accuracy toward the downstream side, large bubbles and / or foreign matters are collected on the upstream side and proceed to the downstream side. As a result, small bubbles and / or foreign substances can be collected. For this reason, the removal efficiency of bubbles and / or foreign matters can be enhanced while extending the filter life.
- a liquid feeding part, and the filtration part is provided with a depth type filter having a filtration accuracy of 1 to 20 ⁇ m, and has a function of performing a filtration treatment in a state where the differential pressure exceeds 0 kPa and is 150 kPa or less.
- the apparatus can be preferably used.
- a depth type filter a filter having a gradient in filtration accuracy can be suitably used.
- the method for producing a pressure-sensitive adhesive optical film according to the present invention includes a step of forming a pressure-sensitive adhesive layer using a pressure-sensitive adhesive coating solution that has undergone filtration, and laminating the pressure-sensitive adhesive layer on at least one side of the optical film.
- the adhesive layer lamination surface side of an optical film May have a step of performing corona treatment or plasma treatment, and may further have a step of forming an anchor layer between the optical film and the pressure-sensitive adhesive layer.
- the step of laminating the pressure-sensitive adhesive layer on the optical film is not particularly limited, and the step of applying and drying the pressure-sensitive adhesive solution on the optical film (or the anchor layer, corona-treated surface or plasma-treated surface formed on the optical film). And a step of transferring with a flexible support (web) provided with an adhesive layer.
- a coating method a roll coating method such as reverse coating or gravure coating, a spin coating method, a screen coating method, a fountain coating method, a dipping method, or a spray method can be adopted.
- a drying step by heating at 80 ° C.
- a transfer system in which a pressure-sensitive adhesive coating solution is applied to a flexible support (web) and transferred by a flexible support (web) provided with a pressure-sensitive adhesive layer after the drying step is preferable.
- the thickness of the pressure-sensitive adhesive layer to be laminated is preferably 1 to 100 ⁇ m, more preferably 5 to 70 ⁇ m, and particularly preferably 10 to 50 ⁇ m. If the thickness of the pressure-sensitive adhesive layer is too thin, problems such as insufficient adhesion to the optical film and peeling from the glass interface are likely to occur, and if it is too thick, problems such as foaming of the pressure-sensitive adhesive may occur. .
- Constituent materials of the flexible support (web) include synthetic resin films such as paper, polyethylene, polypropylene, and polyethylene terephthalate, rubber sheets, paper, cloth, nonwoven fabric, nets, foam sheets, metal foils, and laminates thereof. Suitable thin leaf bodies and the like.
- the surface of the flexible support (web) is subjected to low-adhesion release treatment such as silicone treatment, long-chain alkyl treatment, and fluorine treatment as necessary to enhance the peelability from the pressure-sensitive adhesive layer. May be.
- Examples of the optical film used in the method for producing an adhesive optical film according to the present invention include a polarizing plate.
- a polarizing plate one having a transparent protective film on one side or both sides of a polarizer is usually used.
- 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. Examples thereof include those obtained by adsorbing a substance and uniaxially stretched, and polyene-based oriented films such as dehydrated polyvinyl alcohol and dehydrochlorinated polyvinyl chloride. Among these, a polarizer composed of a polyvinyl alcohol film and a dichroic material such as iodine is preferable.
- the thickness of these polarizers is not particularly limited, but is generally about 3 to 80 ⁇ m.
- a polarizer in which a polyvinyl alcohol film is dyed with iodine and uniaxially stretched can be prepared, for example, by dyeing polyvinyl alcohol in an aqueous solution of iodine and stretching it 3 to 7 times the original length. 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.
- 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.
- a transparent protective film is bonded to one side of the polarizer by an adhesive layer.
- thermosetting resin such as a system or an ultraviolet curable resin
- a thermosetting resin such as a system or an ultraviolet curable resin
- the additive 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.
- the transparent protective film examples include a polymer film described in JP-A-2001-343529 (WO01 / 37007), for example, (A) a thermoplastic resin having a substituted and / or unsubstituted imide group in the side chain, B) Resin compositions containing a thermoplastic resin having substituted and / or unsubstituted phenyl and nitrile groups in the side chain.
- Specific examples include a film of a resin composition containing an alternating copolymer composed of isobutylene and N-methylmaleimide and an acrylonitrile / styrene copolymer.
- As the film a film made of a mixed extruded product of the resin composition or the like can be used. Since these films have a small phase difference and a small photoelastic coefficient, problems such as unevenness due to the distortion of the polarizing plate can be eliminated, and since the moisture permeability is small, the humidification durability is excellent.
- the thickness of the transparent protective film can be appropriately determined, but is generally about 1 to 500 ⁇ m from the viewpoints of workability such as strength and handleability, and thin layer properties. 1 to 300 ⁇ m is particularly preferable, and 5 to 200 ⁇ m is more preferable. The transparent protective film is particularly suitable when the thickness is from 5 to 150 ⁇ m.
- the protective film which consists of the same polymer material may be used for the front and back, and the protective film which consists of a different polymer material etc. may be used.
- the transparent protective film of the present invention it is preferable to use at least one selected from cellulose resin, polycarbonate resin, cyclic polyolefin resin and (meth) acrylic resin.
- Cellulose resin is an ester of cellulose and fatty acid.
- cellulose ester resins include triacetyl cellulose, diacetyl cellulose, tripropionyl cellulose, dipropionyl cellulose, and the like.
- triacetyl cellulose is particularly preferable.
- Many products of triacetylcellulose are commercially available, which is advantageous in terms of availability and cost. Examples of commercially available products of triacetylcellulose include the product names “UV-50”, “UV-80”, “SH-80”, “TD-80U”, “TD-TAC”, “UZ” manufactured by Fujifilm Corporation.
- -TAC "and” KC series manufactured by Konica. In general, these triacetyl celluloses have an in-plane retardation (Re) of almost zero, but a thickness direction retardation (Rth) of about 60 nm.
- a cellulose resin film having a small thickness direction retardation can be obtained, for example, by treating the cellulose resin.
- a base film such as polyethylene terephthalate, polypropylene or stainless steel coated with a solvent such as cyclopentanone or methyl ethyl ketone is bonded to a general cellulose film and dried by heating (for example, at 80 to 150 ° C.
- a fatty acid cellulose resin film with a controlled degree of fat substitution can be used as the cellulose resin film having a small thickness direction retardation.
- triacetyl cellulose has an acetic acid substitution degree of about 2.8.
- the Rth can be reduced by controlling the acetic acid substitution degree to 1.8 to 2.7.
- Rth can be controlled to be small.
- the addition amount of the plasticizer is preferably 40 parts by weight or less, more preferably 1 to 20 parts by weight, and further preferably 1 to 15 parts by weight with respect to 100 parts by weight of the fatty acid cellulose resin.
- a specific example of the cyclic polyolefin resin is preferably a norbornene resin.
- the cyclic olefin-based resin is a general term for resins that are polymerized using a cyclic olefin as a polymerization unit. Resin. Specific examples include cyclic olefin ring-opening (co) polymers, cyclic olefin addition polymers, cyclic olefins and ⁇ -olefins such as ethylene and propylene (typically random copolymers), And graft polymers obtained by modifying them with an unsaturated carboxylic acid or a derivative thereof, and hydrides thereof. Specific examples of the cyclic olefin include norbornene monomers.
- Various products are commercially available as cyclic polyolefin resins.
- trade names “ZEONEX” and “ZEONOR” manufactured by ZEON CORPORATION product names “ARTON” manufactured by JSR Corporation, “TOPAS” manufactured by TICONA, and product names manufactured by Mitsui Chemicals, Inc. “APEL” may be mentioned.
- Tg glass transition temperature
- the upper limit of Tg of the (meth) acrylic resin is not particularly limited, but is preferably 170 ° C. or less from the viewpoint of moldability. From the (meth) acrylic resin, a film having in-plane retardation (Re) and thickness direction retardation (Rth) of almost zero can be obtained.
- any appropriate (meth) acrylic resin can be adopted as long as the effects of the present invention are not impaired.
- poly (meth) acrylic acid ester such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymer, methyl methacrylate- (meth) acrylic acid ester copolymer, methyl methacrylate-acrylic acid ester- (Meth) acrylic acid copolymer, (meth) methyl acrylate-styrene copolymer (MS resin, etc.), a polymer having an alicyclic hydrocarbon group (for example, methyl methacrylate-cyclohexyl methacrylate copolymer, Methyl methacrylate- (meth) acrylate norbornyl copolymer, etc.).
- Preferable examples include C1-6 alkyl poly (meth) acrylates such as poly (meth) acrylate methyl. More preferred is a methyl methacrylate resin containing methyl methacrylate as a main component (50 to 100% by weight, preferably 70 to 100% by weight).
- the (meth) acrylic resin examples include, for example, (Meth) acrylic resin having a ring structure in the molecule described in Acrypet VH and Acrypet VRL20A manufactured by Mitsubishi Rayon Co., Ltd., and JP-A-2004-70296. And a high Tg (meth) acrylic resin system obtained by intramolecular crosslinking or intramolecular cyclization reaction.
- (Meth) acrylic resin having a lactone ring structure can also be used as the (meth) acrylic resin. It is because it has high mechanical strength by high heat resistance, high transparency, and biaxial stretching.
- Examples of the (meth) acrylic resin having a lactone ring structure include JP 2000-230016, JP 2001-151814, JP 2002-120326, JP 2002-254544, and JP 2005. Examples thereof include (meth) acrylic resins having a lactone ring structure described in Japanese Patent No. 146084.
- the (meth) acrylic resin having a lactone ring structure preferably has a ring pseudo structure represented by the following general formula (Formula 2).
- R 1 , R 2 and R 3 each independently represent a hydrogen atom or an organic residue having 1 to 20 carbon atoms.
- the organic residue may contain an oxygen atom.
- the content of the lactone ring structure represented by the general formula (Formula 2) in the structure of the (meth) acrylic resin having a lactone ring structure is preferably 5 to 90% by weight, more preferably 10 to 70% by weight, More preferably, it is 10 to 60% by weight, and particularly preferably 10 to 50% by weight.
- the content of the lactone ring structure represented by the general formula (Chemical Formula 2) in the structure of the (meth) acrylic resin having a lactone ring structure is less than 5% by weight, heat resistance, solvent resistance, and surface hardness are reduced. May be insufficient. If the content of the lactone ring structure represented by the general formula (Chemical Formula 2) in the structure of the (meth) acrylic resin having a lactone ring structure is more than 90% by weight, molding processability may be poor.
- the (meth) acrylic resin having a lactone ring structure has a mass average molecular weight (sometimes referred to as a weight average molecular weight) of preferably 1,000 to 2,000,000, more preferably 5,000 to 1,000,000, still more preferably 10,000 to 500,000, and particularly preferably. Is from 50,000 to 500,000. If the mass average molecular weight is out of the above range, it is not preferable from the viewpoint of molding processability.
- the (meth) acrylic resin having a lactone ring structure preferably has a Tg of 115 ° C. or higher, more preferably 120 ° C. or higher, still more preferably 125 ° C. or higher, and particularly preferably 130 ° C. or higher. Since Tg is 115 ° C. or higher, for example, when incorporated into a polarizing plate as a transparent protective film, it has excellent durability.
- the upper limit of Tg of the (meth) acrylic resin having the lactone ring structure is not particularly limited, but is preferably 170 ° C. or less from the viewpoint of moldability and the like.
- the (meth) acrylic resin having a lactone ring structure is more preferable as the total light transmittance of a molded product obtained by injection molding measured by a method according to ASTM-D-1003 is higher, preferably 85 % Or more, more preferably 88% or more, and still more preferably 90% or more.
- the total light transmittance is a measure of transparency. If the total light transmittance is less than 85%, the transparency may be lowered.
- the transparent protective film those having a front retardation of less than 40 nm and a thickness direction retardation of less than 80 nm are usually used.
- the slow axis direction is the direction that maximizes the refractive index in the film plane. ].
- a transparent protective film has as little color as possible.
- a protective film having a retardation value in the thickness direction of ⁇ 90 nm to +75 nm is preferably used.
- the thickness direction retardation value (Rth) is more preferably ⁇ 80 nm to +60 nm, and particularly preferably ⁇ 70 nm to +45 nm.
- a retardation plate having a retardation with a front retardation of 40 nm or more and / or a thickness direction retardation of 80 nm or more can be used as the transparent protective film.
- the front phase difference is usually controlled in the range of 40 to 200 nm
- the thickness direction phase difference is usually controlled in the range of 80 to 300 nm.
- the retardation plate functions also as a transparent protective film, so that the thickness can be reduced.
- the retardation plate examples include a birefringent film obtained by uniaxially or biaxially stretching a polymer material, a liquid crystal polymer alignment film, and a liquid crystal polymer alignment layer supported by a film.
- the thickness of the retardation plate is not particularly limited, but is generally about 20 to 150 ⁇ m.
- polymer material examples include polyvinyl alcohol, polyvinyl butyral, polymethyl vinyl ether, polyhydroxyethyl acrylate, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, polycarbonate, polyarylate, polysulfone, polyethylene terephthalate, polyethylene naphthalate, polyether sulfone, Polyphenylene sulfide, polyphenylene oxide, polyallylsulfone, polyamide, polyimide, polyolefin, polyvinyl chloride, cellulose resin, cyclic polyolefin resin (norbornene resin), or any of these binary, ternary copolymers, graft copolymers Examples thereof include polymers and blends. These polymer materials become oriented products (stretched films) by stretching or the like.
- liquid crystal polymer examples include various main chain types and side chain types in which a conjugated linear atomic group (mesogen) imparting liquid crystal orientation is introduced into the main chain or side chain of the polymer.
- main chain type liquid crystal polymer examples include a nematic alignment polyester liquid crystal polymer, a discotic polymer, and a cholesteric polymer having a structure in which a mesogen group is bonded at a spacer portion that imparts flexibility.
- the side chain type liquid crystal polymer include polysiloxane, polyacrylate, polymethacrylate or polymalonate as a main chain skeleton, and a nematic alignment-providing para-substitution via a spacer portion composed of a conjugated atomic group as a side chain.
- examples thereof include those having a mesogenic part composed of a cyclic compound unit.
- These liquid crystal polymers are prepared by, for example, applying a solution of a liquid crystalline polymer on an alignment surface such as a surface of a thin film such as polyimide or polyvinyl alcohol formed on a glass plate, or a silicon oxide is obliquely deposited. This is done by developing and heat treatment.
- the retardation plate may have an appropriate retardation according to the purpose of use, such as for the purpose of compensating for coloring or viewing angle due to birefringence of various wave plates and liquid crystal layers, and may be two or more types. It may be one in which retardation plates are stacked and optical characteristics such as retardation are controlled.
- a retardation plate that satisfies nx> ny> nz use a plate that satisfies a front phase difference of 40 to 100 nm, a thickness direction retardation of 100 to 320 nm, and an Nz coefficient of 1.8 to 4.5. Is preferred.
- a retardation plate that satisfies a front phase difference of 100 to 200 nm.
- a retardation plate satisfying nx> nz> ny it is preferable to use a retardation plate having a front phase difference of 150 to 300 nm and an Nz coefficient exceeding 0 to 0.7.
- the transparent protective film can be appropriately selected according to the applied liquid crystal display device.
- VA including Vertical Alignment, MVA, and PVA
- at least one of the polarizing plates (cell side) has a retardation.
- nx> ny nz
- nx> ny> nz nx> nz> ny
- both the upper and lower sides of the liquid crystal cell may have a phase difference, or any one of the upper and lower transparent protective films may have a phase difference.
- both cases where the transparent protective film on one side of the polarizing plate has a phase difference or not can be used.
- the liquid crystal cell does not have a phase difference both above and below (cell side).
- the liquid crystal cell has a phase difference
- the liquid crystal cell has a phase difference in the upper and lower sides, or the upper and lower sides have a phase difference (for example, nx> nz> ny on the upper side).
- Biaxial film satisfying the relationship, when there is no retardation on the lower side, positive A plate on the upper side, and positive C plate on the lower side).
- nx> ny nz
- nx> nz> ny ny
- nz> nx> ny positive A plate, biaxial, positive C plate
- the film having the retardation can be separately attached to a transparent protective film having no retardation to give the function.
- the transparent protective film may be subjected to surface modification treatment in order to improve adhesiveness with a polarizer before applying an adhesive.
- Specific examples of the treatment include corona treatment, plasma treatment, flame treatment, ozone treatment, primer treatment, glow treatment, saponification treatment, and treatment with a coupling agent.
- an antistatic layer can be appropriately formed.
- the surface of the transparent protective film to which the polarizer is not adhered may be subjected to a treatment for the purpose of hard coat layer, antireflection treatment, antisticking, diffusion or antiglare.
- the hard coat treatment is applied for the purpose of preventing scratches on the surface of the polarizing plate.
- a transparent protective film with a cured film excellent in hardness, sliding properties, etc. by an appropriate ultraviolet curable resin such as acrylic or silicone is used. It can be formed by a method of adding to the surface of the film.
- the antireflection treatment is performed for the purpose of preventing reflection of external light on the surface of the polarizing plate, and can be achieved by forming an antireflection film or the like according to the conventional art.
- the sticking prevention treatment is performed for the purpose of preventing adhesion with an adjacent layer (for example, a backlight-side diffusion plate).
- Anti-glare treatment is applied for the purpose of preventing the outside light from being reflected on the surface of the polarizing plate and obstructing the visibility of the light transmitted through the polarizing plate.
- the surface is roughened by a sandblasting method or an embossing method. It can be formed by imparting a fine concavo-convex structure to the surface of the transparent protective film by an appropriate method such as a blending method of transparent fine particles.
- the fine particles to be included in the formation of the fine surface uneven structure include conductive materials made of silica, alumina, titania, zirconia, tin oxide, indium oxide, cadmium oxide, antimony oxide, and the like having an average particle diameter of 0.5 to 20 ⁇ m.
- transparent fine particles such as inorganic fine particles and organic fine particles composed of a crosslinked or uncrosslinked polymer are used.
- the amount of fine particles used is generally about 2 to 70 parts by weight, preferably 5 to 50 parts by weight, based on 100 parts by weight of the transparent resin forming the surface fine uneven structure.
- the antiglare layer may also serve as a diffusion layer (viewing angle expanding function or the like) for diffusing the light transmitted through the polarizing plate to expand the viewing angle.
- the antireflection layer, anti-sticking layer, diffusion layer, antiglare layer and the like can be provided on the transparent protective film itself, or can be provided separately from the transparent protective film as an optical layer.
- 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 plate adhesive exhibits suitable adhesion to the various transparent protective films.
- the adhesive used in the present invention can contain a metal compound filler.
- optical film examples include liquid crystal display devices such as a reflection plate, an anti-transmission plate, a retardation plate (including wavelength plates such as 1/2 and 1/4), a visual compensation film, a brightness enhancement film, and a surface treatment film.
- liquid crystal display devices such as a reflection plate, an anti-transmission plate, a retardation plate (including wavelength plates such as 1/2 and 1/4), a visual compensation film, a brightness enhancement film, and a surface treatment film.
- the surface treatment film is also provided by bonding to the front plate.
- Anti-reflective films such as hard coat films used to impart surface scratch resistance, anti-glare treated films to prevent reflection on image display devices, anti-reflective films, low-reflective films, etc. Is mentioned.
- the front plate is attached to the surface of the image display device in order to protect the image display device such as a liquid crystal display device, an organic EL display device, a CRT, or a PDP, to give a high-class feeling, or to differentiate by design. It is provided together.
- the front plate is used as a support for a ⁇ / 4 plate in 3D-TV. For example, in a liquid crystal display device, it is provided above the polarizing plate on the viewing side.
- the same effect as that of the glass substrate is exhibited not only on the glass substrate but also on a plastic substrate such as a polycarbonate substrate and a polymethyl methacrylate substrate as the front plate. .
- An optical film in which the optical layer is laminated on a polarizing plate can be formed by a method of sequentially laminating separately in the manufacturing process of a liquid crystal display device or the like. It is excellent in stability and assembly work, and has the advantage of improving the manufacturing process of a liquid crystal display device and the like.
- Appropriate bonding means such as an adhesive layer can be used for lamination. When adhering the polarizing plate and the other optical layer, their optical axes can be set at an appropriate arrangement angle in accordance with the target phase difference characteristic.
- the pressure-sensitive adhesive optical film of the present invention can be preferably used for forming various image display devices such as liquid crystal display devices.
- 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, an adhesive optical film, and an illumination system as required, and incorporating a drive circuit. There is no particular limitation except that the pressure-sensitive adhesive optical film according to the present invention is used.
- the liquid crystal cell any type such as a TN type, STN type, ⁇ type, VA type, IPS type, or the like can be used.
- liquid crystal display devices such as a liquid crystal display device in which an adhesive optical film is disposed on one side or both sides of a display panel such as a liquid crystal cell, or a backlight or reflector used in an illumination system can be formed.
- the optical film according to the present invention can be installed on one side or both sides of a display panel such as a liquid crystal cell.
- optical films When optical films are provided on both sides, they may be the same or different.
- a single layer or a suitable layer such as a diffusion plate, an antiglare layer, an antireflection film, a protective plate, a prism array, a lens array sheet, a light diffusion plate, a backlight, Two or more layers can be arranged.
- organic electroluminescence device organic EL display device: OLED
- a transparent electrode, an organic light emitting layer, and a metal electrode are sequentially laminated on a transparent substrate to form a light emitter (organic electroluminescent light emitter).
- the organic light emitting layer is a laminate of various organic thin films, for example, a laminate of a hole injection layer made of a triphenylamine derivative and a light emitting layer made of a fluorescent organic solid such as anthracene, Alternatively, a structure having various combinations such as a laminate of such a light-emitting layer and an electron injection layer composed of a perylene derivative, or a stack of these hole injection layer, light-emitting layer, and electron injection layer is known. It has been.
- holes and electrons are injected into the organic light-emitting layer by applying a voltage to the transparent electrode and the metal electrode, and the energy generated by recombination of these holes and electrons excites the phosphor material. Then, light is emitted on the principle that the excited fluorescent material emits light when returning to the ground state.
- the mechanism of recombination in the middle is the same as that of a general diode, and as can be predicted from this, the current and the emission intensity show strong nonlinearity with rectification with respect to the applied voltage.
- an organic EL display device in order to extract light emitted from the organic light emitting layer, at least one of the electrodes must be transparent, and a transparent electrode usually formed of a transparent conductor such as indium tin oxide (ITO) is used as an anode. It is used as On the other hand, in order to facilitate electron injection and increase luminous efficiency, it is important to use a material having a small work function for the cathode, and usually metal electrodes such as Mg—Ag and Al—Li are used.
- ITO indium tin oxide
- the organic light emitting layer is formed of a very thin film having a thickness of about 10 nm. For this reason, the organic light emitting layer transmits light almost completely like the transparent electrode. As a result, light that is incident from the surface of the transparent substrate at the time of non-light emission, passes through the transparent electrode and the organic light emitting layer, and is reflected by the metal electrode is again emitted to the surface side of the transparent substrate.
- the display surface of the organic EL display device looks like a mirror surface.
- an organic EL display device comprising an organic electroluminescent light emitting device comprising a transparent electrode on the surface side of an organic light emitting layer that emits light upon application of a voltage and a metal electrode on the back side of the organic light emitting layer, the surface of the transparent electrode While providing a polarizing plate on the side, a retardation plate can be provided between the transparent electrode and the polarizing plate.
- the retardation plate and the polarizing plate have a function of polarizing light incident from the outside and reflected by the metal electrode, there is an effect that the mirror surface of the metal electrode is not visually recognized by the polarization action.
- the mirror surface of the metal electrode can be completely shielded by configuring the retardation plate with a quarter-wave plate and adjusting the angle formed by the polarization direction of the polarizing plate and the retardation plate to ⁇ / 4. .
- linearly polarized light becomes generally elliptically polarized light by the phase difference plate, but becomes circularly polarized light particularly when the phase difference plate is a quarter wavelength plate and the angle formed by the polarization direction of the polarizing plate and the phase difference plate is ⁇ / 4. .
- This circularly polarized light is transmitted through the transparent substrate, the transparent electrode, and the organic thin film, reflected by the metal electrode, is again transmitted through the organic thin film, the transparent electrode, and the transparent substrate, and becomes linearly polarized light again on the retardation plate. And since this linearly polarized light is orthogonal to the polarization direction of a polarizing plate, it cannot permeate
- Example 1 In Example 1, a water-dispersed acrylic pressure-sensitive adhesive was used as the pressure-sensitive adhesive coating solution.
- 55554 parts of butyl acrylate, 2776 parts of acrylic acid, mono [poly (propylene oxide) methacrylate] phosphate ester (average degree of polymerization of propylene oxide is 5.0) ) 1665 parts and 5-methacryloyloxypropyl-triethoxysilane (Shin-Etsu Chemical Co., Ltd., KBM-503) 5 parts were added and mixed to obtain a monomer mixture.
- a coating liquid supply apparatus including a filter (30 inch size ⁇ 6), a filtration section having an initial differential pressure set to 40 kPa, and a liquid feeding section for transferring the coating liquid, the water
- the pressure-sensitive adhesive coating solution containing the dispersion type acrylic pressure-sensitive adhesive was subjected to filtration treatment (filtration step).
- the number of bubbles and the number of foreign substances in the adhesive coating solution were evaluated with a particle counter.
- the particle counter used is based on the principle that laser light is attenuated when bubbles and / or foreign objects are present when laser light is applied to the adhesive coating liquid that passes through a certain area. By detecting the amount of attenuation with a photodetector, the bubble diameter and foreign substance diameter, the number of bubbles and the number of foreign substances in the adhesive coating solution are measured. Details of the evaluation method are shown below.
- Example 2 Application of adhesive containing the water-dispersed acrylic adhesive in the same manner as in Example 1 except that the filtration accuracy, the presence or absence of a gradient of filtration accuracy, and the differential pressure were changed to those shown in Table 1.
- the liquid was subjected to filtration treatment (filtration step).
- Comparative Example 1 using a pleated type filter, Comparative Example 2 having a large differential pressure, and Comparative Example 3 having a high filtration accuracy, the efficiency of removing bubbles and foreign matters deteriorates.
- Comparative Example 4 where the filtration accuracy is small, the initial bubble and foreign matter removal efficiency is good, but it can be seen that the differential pressure increases with time, and the bubble and foreign matter removal efficiency also deteriorates with time. Therefore, when removing bubbles and foreign substances by filtering a pressure-sensitive adhesive coating solution containing a water-dispersed acrylic pressure-sensitive adhesive using a depth type filter, the optimum range (1 to 20 ⁇ m) for filtration accuracy is obtained. You can see that it exists.
- the pressure-sensitive adhesive layer obtained using the pressure-sensitive adhesive coating solution obtained after the filtration step of Comparative Examples 1 to 3 has a large number of bubbles and foreign matter detected as foreign matters, and therefore the finally obtained pressure-sensitive adhesive type It can be seen that also in the optical film, appearance defects due to bubbles and foreign matters increase.
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- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Adhesive Tapes (AREA)
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Abstract
Description
(一般式(1)中、R1は、水素原子またはメチル基を示し、R2は炭素数1~4のアルキレン基、mは2以上の整数を示し、M1およびM2は、それぞれ独立に、水素原子またはカチオンを示す。)で表されるリン酸基またはその塩を示す。)で表されるリン酸基含有モノマーが挙げられる。
式中、R1、R2およびR3は、それぞれ独立に、水素原子または炭素原子数1~20の有機残基を示す。なお、有機残基は酸素原子を含んでいてもよい。
実施例1では、粘着剤塗布液として水分散型アクリル系粘着剤を用いた。この水分散型アクリル系粘着剤の調製に際しては、容器に、原料としてブチルアクリレート55554部、アクリル酸2776部、モノ[ポリ(プロピレンオキシド)メタクリレート]リン酸エステル(プロピレンオキシドの平均重合度5.0)1665部、および3-メタクリロイルオキシプロピル-トリエトキシシラン(信越化学工業(株)製,KBM-503)5部を加えて混合し、モノマー混合物を得た。次いで、調製したモノマー混合物60000部に、反応性乳化剤としてアクアロンHS-10(第一工業製薬社製)1300部、イオン交換水38700部を加え、ホモジナイザー(特殊機化工業(株)製)を用い、10分間、7000rpmで攪拌し、モノマーエマルションを調製した。次に、冷却管、窒素導入管、温度計、滴下ロートおよび攪拌羽根を備えた反応容器に、上記のようにして調製したモノマーエマルションのうちの20000部およびイオン交換水35000部を仕込み、次いで、反応容器を十分窒素置換した後、過硫酸アンモニウム10部を添加して、60℃で1時間重合した。次いで、残りのモノマーエマルションのうち80000部を、反応容器に3時間かけて滴下し、その後、3時間重合した。さらにその後、窒素置換しながら、65℃で5時間重合し、固形分濃度45%の水分散型粘着剤水溶液を得た。次いで、上記エマルション溶液を室温まで冷却した後、濃度10%のアンモニア水を30部添加し、さらに蒸留水で固形分を調製して39%とした。この液を、B型粘度計(東機産業製)を用いて、23℃、ローター回転数20rpmにて測定した結果、2000mPa・sであった。
塗布液中の気泡数および異物数評価として、Particle Measuring Systems社製の光遮蔽式のパーティクルカウンターを使用して、5~100umのサイズの気泡および異物を計測した。塗布液は、ろ過前、ろ過後の液をサンプリングして評価した。また、フィルターのライフ(寿命)を評価するために、フィルターを10時間連続使用した後のろ過後の液もサンプリングしてパーティクルカウンターで計測した。測定結果は、単位重量当たりの気泡数および異物数(個/g)で表わされる。計測された5~100umの気泡数および異物数を合計して、ろ過前後で計測された気泡数および異物数から(1)式の除去効率を算出して評価した。各実施例および比較例の評価結果を表1に示す。
[除去効率]=([ろ過後の気泡数および異物数]/[ろ過前の気泡数および異物数])×100 (1)
ろ過精度、ろ過精度の勾配の有無、および差圧を表1に記載のものに変更したこと以外は、実施例1と同様の方法により、前記水分散型アクリル系粘着剤を含有する粘着剤塗布液をろ過処理した(ろ過工程)。
デプスタイプ・フィルターに代えて、プリーツタイプ・フィルターを使用したこと以外は、実施例1と同様の方法により、前記水分散型アクリル系粘着剤を含有する粘着剤塗布液をろ過処理した(ろ過工程)。
ろ過精度、ろ過精度の勾配の有無、および差圧を表1に記載のものに変更したこと以外は、実施例1と同様の方法により、前記水分散型アクリル系粘着剤を含有する粘着剤塗布液をろ過処理した(ろ過工程)。
実施例1~9および比較例1~4のろ過工程後に得られた粘着剤塗布液を、剥離処理したポリエチレンテレフタレート(厚さ38μm)からなるセパレータの表面に、乾燥厚みが25μmになるようにダイコーターにより塗布した後、100℃で150秒間乾燥して、粘着剤層を形成した。
得られた粘着剤層(面積1m2)の面に含まれる気泡および/または異物を、目視、および光学顕微鏡にて、その個数と大きさを測定した。最大長さが20μm以上の気泡および/または異物の個数(個/m2)を表2に示す。なお、表2中、「20μm以上の気泡および/または異物の個数(個/m2);10時間後」は、フィルターのライフ(寿命)を評価するために、フィルターを10時間連続使用した後のろ過後の粘着剤塗布液を用いて形成した粘着剤層の面において測定された、20μm以上の気泡および/または異物の個数(個/m2)を意味する。
Claims (12)
- ろ過精度が1~20μmであるデプスタイプ・フィルターを使用し、水分散型粘着剤を含有する粘着剤塗布液を、差圧が0kPaを超え、かつ150kPa以下の状態でろ過処理するろ過工程と、ろ過処理後の前記粘着剤塗布液を塗布した後、乾燥する塗布・乾燥工程と、を含むことを特徴とする光学フィルム用粘着剤層の製造方法。
- 前記デプスタイプ・フィルターが、ろ過精度に勾配を有する請求項1に記載の光学フィルム用粘着剤層の製造方法。
- 請求項1または2に記載の製造方法により製造された光学フィルム用粘着剤層。
- 最大長さが100μmを超える気泡および/または異物を含んでおらず、かつ、前記粘着剤層の面において、最大長さが20μm以上の気泡および/または異物の個数が、10個/m2以内である請求項3に記載の光学フィルム用粘着剤層。
- 光学フィルムの少なくとも片側に、粘着剤層が積層されている粘着型光学フィルムの製造方法であって、
前記粘着剤層を製造する工程が、デプスタイプ・フィルターを使用し、前記粘着剤層の原料となる粘着剤塗布液を、差圧が0kPaを超え、かつ150kPa以下の状態でろ過処理するろ過工程を含み、
前記粘着剤塗布液が、水分散型粘着剤を含有するものであり、
前記デプスタイプ・フィルターのろ過精度が1~20μmであることを特徴とする粘着型光学フィルムの製造方法。 - 前記デプスタイプ・フィルターが、ろ過精度に勾配を有する請求項5に記載の粘着型光学フィルムの製造方法。
- 前記ろ過工程の後、前記粘着剤塗布液を可撓性支持体(ウェブ)に塗布し、乾燥することにより、粘着剤層を設けた可撓性支持体(ウェブ)を製造する塗布・乾燥工程と、前記粘着剤層を設けた可撓性支持体(ウェブ)から、前記粘着剤層を前記光学フィルム上に転写する転写工程と、をさらに含む請求項5または6に記載の粘着型光学フィルムの製造方法。
- 前記ろ過工程の後、前記粘着剤塗布液を前記光学フィルム上に塗布した後、乾燥する塗布・乾燥工程をさらに含む請求項5~7のいずれかに記載の粘着型光学フィルムの製造方法。
- 請求項5~8のいずれかに記載の製造方法により製造された粘着型光学フィルム。
- 請求項9に記載の粘着型光学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。
- 粘着型光学フィルムを構成する粘着剤層の原料となる粘着剤塗布液を供給するための塗布液供給装置であって、
少なくとも前記粘着剤塗布液を送液するためのポンプと、前記粘着剤塗布液中に含まれる気泡を除去するためのろ過部と、前記粘着剤塗布液を移送するための送液部と、を備え、
前記ろ過部が、ろ過精度が1~20μmであるデプスタイプ・フィルターを備え、差圧が0kPaを超え、かつ150kPa以下の状態でろ過処理する機能を有することを特徴とする塗布液供給装置。 - 前記デプスタイプ・フィルターが、ろ過精度に勾配を有する請求項11に記載の塗布液供給装置。
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KR1020137027322A KR101918791B1 (ko) | 2011-04-25 | 2012-04-20 | 광학 필름용 점착제층 및 그 제조 방법, 점착형 광학 필름 및 그 제조 방법, 화상 표시 장치 그리고 도포액 공급 장치 |
US14/112,099 US20140044953A1 (en) | 2011-04-25 | 2012-04-20 | Adhesive layer for optical film and method for producing same, adhesive optical film and method for producing same, image display device, and coating liquid supply device |
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WO2015156254A1 (ja) * | 2014-04-07 | 2015-10-15 | 日本ゼオン株式会社 | 熱伝導性感圧接着性積層シートの製造方法、熱伝導性感圧接着性積層シート、及び、電子機器 |
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10297093A (ja) * | 1997-04-25 | 1998-11-10 | Tdk Corp | 熱転写記録媒体の製造方法 |
JPH11195324A (ja) * | 1998-01-05 | 1999-07-21 | Murata Mfg Co Ltd | 厚膜形成用ペーストの製造方法 |
JP2001213974A (ja) * | 2000-01-31 | 2001-08-07 | Konica Corp | 光学フィルム及びその製造方法 |
JP2007297475A (ja) * | 2006-04-28 | 2007-11-15 | Asahi Glass Co Ltd | ポリエーテル、ポリウレタン、イソシアネート基末端プレポリマーおよびポリウレタンフォームの製造方法 |
JP4542920B2 (ja) * | 2004-11-04 | 2010-09-15 | 富士フイルム株式会社 | 光学フィルム、偏光板、ディスプレイ装置、及び光学フィルムの製造方法 |
JP2010280856A (ja) * | 2009-06-05 | 2010-12-16 | Nitto Denko Corp | 粘着剤層、粘着部材、その製造方法および画像表示装置 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10128211A (ja) * | 1996-10-29 | 1998-05-19 | Teijin Ltd | 塗布方法及びその装置 |
JP2002188063A (ja) * | 2000-12-21 | 2002-07-05 | Nitto Denko Corp | 粘着シートの製造方法およびその装置 |
JP2011241324A (ja) * | 2010-05-19 | 2011-12-01 | Sumitomo Chemical Co Ltd | 水性エマルションの製造方法 |
-
2011
- 2011-04-25 JP JP2011097249A patent/JP5847429B2/ja active Active
-
2012
- 2012-04-20 WO PCT/JP2012/060666 patent/WO2012147633A1/ja active Application Filing
- 2012-04-20 CN CN201280019993.6A patent/CN103492512B/zh active Active
- 2012-04-20 KR KR1020137027322A patent/KR101918791B1/ko active IP Right Grant
- 2012-04-20 US US14/112,099 patent/US20140044953A1/en not_active Abandoned
- 2012-04-24 TW TW101114518A patent/TWI531635B/zh active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10297093A (ja) * | 1997-04-25 | 1998-11-10 | Tdk Corp | 熱転写記録媒体の製造方法 |
JPH11195324A (ja) * | 1998-01-05 | 1999-07-21 | Murata Mfg Co Ltd | 厚膜形成用ペーストの製造方法 |
JP2001213974A (ja) * | 2000-01-31 | 2001-08-07 | Konica Corp | 光学フィルム及びその製造方法 |
JP4542920B2 (ja) * | 2004-11-04 | 2010-09-15 | 富士フイルム株式会社 | 光学フィルム、偏光板、ディスプレイ装置、及び光学フィルムの製造方法 |
JP2007297475A (ja) * | 2006-04-28 | 2007-11-15 | Asahi Glass Co Ltd | ポリエーテル、ポリウレタン、イソシアネート基末端プレポリマーおよびポリウレタンフォームの製造方法 |
JP2010280856A (ja) * | 2009-06-05 | 2010-12-16 | Nitto Denko Corp | 粘着剤層、粘着部材、その製造方法および画像表示装置 |
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WO2019012968A1 (ja) * | 2017-07-10 | 2019-01-17 | 日東電工株式会社 | 積層体および偏光膜の製造方法 |
JPWO2019012968A1 (ja) * | 2017-07-10 | 2020-04-02 | 日東電工株式会社 | 積層体および偏光膜の製造方法 |
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US20140044953A1 (en) | 2014-02-13 |
KR20140061308A (ko) | 2014-05-21 |
KR101918791B1 (ko) | 2018-11-14 |
TWI531635B (zh) | 2016-05-01 |
TW201247837A (en) | 2012-12-01 |
CN103492512B (zh) | 2016-05-25 |
JP5847429B2 (ja) | 2016-01-20 |
CN103492512A (zh) | 2014-01-01 |
JP2012229305A (ja) | 2012-11-22 |
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