WO2016072437A1 - 易接着組成物、及びこれを用いた光学フィルムとその製造方法 - Google Patents
易接着組成物、及びこれを用いた光学フィルムとその製造方法 Download PDFInfo
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- WO2016072437A1 WO2016072437A1 PCT/JP2015/081116 JP2015081116W WO2016072437A1 WO 2016072437 A1 WO2016072437 A1 WO 2016072437A1 JP 2015081116 W JP2015081116 W JP 2015081116W WO 2016072437 A1 WO2016072437 A1 WO 2016072437A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
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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
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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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
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
Definitions
- the present invention relates to an easy-adhesion composition and an optical film having an easy-adhesion layer composed of the easy-adhesion composition. Furthermore, this invention relates to the manufacturing method of this optical film, a polarizing plate provided with this optical film, and an image display apparatus.
- Acrylic resin films formed from (meth) acrylic polymers typified by polymethyl methacrylate are known to have excellent optical properties such as light transmittance, as well as excellent balance between mechanical strength and moldability. ing. For this reason, the acrylic resin film is applied to an optical film incorporated in an image display device such as a liquid crystal display device (LCD), a plasma display panel (PDP), or an organic EL display device (OLED).
- LCD liquid crystal display device
- PDP plasma display panel
- OLED organic EL display device
- the optical film is usually used in a state where it is laminated with another functional film.
- an optical film is used as a polarizer protective film, it is laminated on at least one surface of the polarizer via a hydrophilic adhesive layer.
- the obtained polarizing plate is used for an image display device or the like. In this case, it is important that the adhesion between the optical film and the polarizer is good.
- the acrylic resin film is inferior in adhesiveness with a hydrophilic adhesive and has a problem that adhesiveness with a polarizer is not sufficient.
- a method has been proposed in which an easy-adhesion layer mainly composed of a co-adhesive resin such as polyester, acrylic, or polyurethane is provided on the surface of the acrylic resin film to impart easy adhesion to the acrylic resin film.
- portable devices using an image display device such as an LCD are recently used in various environments, indoors or outdoors, and may require moisture and heat resistance that can withstand high-temperature and high-humidity environments.
- a polarizing plate used for such an application is required to have high adhesion that does not cause delamination even under high temperature and high humidity.
- Japanese Patent Application Laid-Open No. 2009-193061 discloses an easy-adhesion layer in which a polymer having an oxazoline group as a crosslinking agent is blended on the surface of a (meth) acrylic resin film as a polarizing plate having excellent adhesion under high temperature and high humidity. It is described to form.
- Japanese Patent Application Laid-Open No. 2014-35411 discloses an easy-adhesion layer in which a polyester resin, a polyvinyl alcohol resin, and a crosslinking agent composed of an isocyanate compound or a melamine compound are blended in order to improve the adhesion between an acrylic film and a polarizer. It is described to provide.
- the optical film having an easy-adhesion layer disclosed in the above document initially exhibits good adhesion, a decrease in adhesion with a polarizer is inevitable when used for a long time under high temperature and high humidity. It was a thing. Due to such a decrease in adhesion, there is a problem that initial performance (initial adhesion) is not maintained for a long time. Further, the optical film having an easy-contact layer disclosed in the above document satisfies the moisture and heat resistance in an environment of about 40 to 60 ° C. and about 60 to 90% RH, but under a more severe environment (for example, 80 ° C., The heat and humidity resistance at 90% RH) was not satisfactory.
- the present invention has been made in view of such problems, and is an easy-adhesive composition that can suppress deterioration in initial performance in long-term use under high temperature and high humidity, and can also satisfy moisture and heat resistance in a harsh environment. And an optical film in which an easy-adhesion layer comprising the easy-adhesion composition is provided on at least one surface of a thermoplastic resin film.
- An easily adhesive composition containing 100 parts by weight of a water-dispersible urethane resin having a carboxyl group, 1 to 25 parts by weight of a water-soluble carbodiimide compound, and 1 to 25 parts by weight of a water-dispersible carbodiimide compound is provided.
- the present invention also provides (2) The easy-adhesion composition according to (1), wherein the weight ratio of the water-soluble carbodiimide compound and the water-dispersible carbodiimide compound is in the range of 30:70 to 95: 5; (3) The easy-adhesive composition according to (1) or (2), further containing 0.1 to 15 parts by weight of fine particles with respect to 100 parts by weight of the water-dispersible urethane resin; (4) A thermoplastic resin film and an easy-adhesion layer provided on at least one surface of the thermoplastic resin film and formed from the easy-adhesion composition according to any one of (1) to (3) Optical film; (5) The thermoplastic resin film is made of a (meth) acrylic resin, the optical film according to (4); and (6) a polarizer and the surface of the polarizer is covered and protected (4) or ( 5) A polarizing plate comprising the optical film described above.
- the present invention further includes (7) Easily containing 100 parts by weight of a water-dispersible urethane resin diluted with an aqueous solvent and having a carboxyl group, 1 to 25 parts by weight of a water-soluble carbodiimide compound, and 1 to 25 parts by weight of a water-dispersible carbodiimide compound
- a method for producing an optical film comprising a step of applying an adhesive composition to at least one surface of a thermoplastic resin film to form a coating film, and a step of drying the coating film to form an easy-adhesion layer.
- the easy-adhesion composition of the present invention having the above-described configuration can suppress a decrease in initial performance when used for a long time under high temperature and high humidity, and can maintain high adhesion even in a harsh environment. Therefore, the polarizing plate using the optical film which has the easily bonding layer which consists of an easily bonding composition of this invention is excellent in the adhesiveness of the optical film and polarizer under high temperature and high humidity.
- the term “(meth) acryl” is used as a general term for methacryl, acryl, or both. The same applies to the term “(meth) acrylonitrile”.
- the easy-adhesion composition of the present invention comprises a water-dispersible urethane resin having a carboxyl group (hereinafter sometimes simply referred to as U resin), a water-soluble carbodiimide compound (hereinafter sometimes simply referred to as S compound) as a crosslinking agent, and A water-dispersible carbodiimide compound (hereinafter sometimes simply referred to as a D compound).
- U resin a water-dispersible urethane resin having a carboxyl group
- S compound water-soluble carbodiimide compound
- a water-dispersible carbodiimide compound hereinafter sometimes simply referred to as a D compound.
- the easy-adhesion layer that has been known for this purpose is unavoidably deteriorated in adhesion when used for a long time under high temperature and high humidity.
- the fall of the initial performance in long-time use under high temperature and high humidity is suppressed, and it is excellent in adhesiveness under high temperature and high humidity. The reason for this is not clear, but it is presumed that the S compound and the D compound form a crosslinked structure at different times and function as follows.
- the S compound since the S compound has good compatibility with other hydrophilic resins and has a high crosslinking reaction rate, it forms a crosslinked structure with the carboxyl group of the U resin at the time of forming the easy adhesion layer or at an early stage after the formation.
- the D compound since the D compound has a slower crosslinking reaction rate than the S compound, the unreacted D compound remains in the easy-adhesion layer when the easy-adhesion layer is formed. Under high temperature and high humidity, when the U resin in the easy-adhesion layer is a polyester, the polyester undergoes hydrolysis, the ester bond is cleaved, and a carboxylic acid group is generated.
- the unreacted D compound reacts with the generated carboxylic acid group to form a cross-linked structure, and self-healing degradation of the easy-adhesion layer due to hydrolysis reduces the strength degradation of the easy-adhesion layer under high temperature and high humidity. It is thought that it is suppressing.
- a functional group such as a carboxyl group is present in the functional layer or the thermoplastic resin film laminated on the easy adhesion layer. Under high temperature and high humidity, these functional layers or thermoplastic resin films react with carboxyl groups and unreacted D compounds to form a cross-linked structure, thereby suppressing the strength deterioration of the easily adhesive layer. It is done.
- the U resin is not particularly limited as long as it is a water dispersible urethane resin having a carboxyl group in the molecule.
- U resin can be manufactured by the following method, for example. First, an isocyanate group-terminated prepolymer is formed by reacting a polyisocyanate and a polyol in an organic solvent which is inert to isocyanate and compatible with water. This is then reacted with a chain extender having a free carboxyl group to obtain a linear urethane prepolymer. Thereafter, the linear urethane prepolymer is chain-extended in water in the presence of a neutralizing agent, and at the same time is made aqueous, thereby obtaining a U resin.
- water-based as used herein means that the resin is stably dispersed or emulsified in water.
- polyisocyanates examples include tetramethylene diisocyanate, dodecamethylene diisocyanate, 1,4-butane diisocyanate, hexamethylene diisocyanate, 2,2,4-trimethylhexamethylene diisocyanate, 2,4,4-trimethylhexamethylene diisocyanate, and lysine diisocyanate.
- Aliphatic diisocyanates such as 2-methylpentane-1,5-diisocyanate, 3-methylpentane-1,5-diisocyanate; isophorone diisocyanate, hydrogenated xylylene diisocyanate, 4,4'-cyclohexylmethane diisocyanate, 1,4- Cycloaliphatic diisocyanate, methylcyclohexylene diisocyanate, 1,3-bis (isocyanatomethyl) cyclohexane Socyanate; tolylene diisocyanate, 2,2'-diphenylmethane diisocyanate, 2,4'-diphenylmethane diisocyanate, 4,4'-diphenylmethane diisocyanate, 4,4'-diphenyldimethylmethane diisocyanate, 4,4'-dibenzyl diisocyanate, 1 , 5-naphthylene diisocyanate, xylylene
- the polyol is not particularly limited as long as it has two or more hydroxyl groups in the molecule, and any appropriate polyol can be adopted.
- polyacryl polyol, polyester polyol, polyether polyol, polycarbonate polyol and the like can be mentioned. These can be used alone or in combination of two or more.
- Examples of the chain extender having a free carboxyl group include dihydroxycarboxylic acid and dihydroxysuccinic acid.
- Examples of the dihydroxycarboxylic acid include dialkyrol alkanoic acids such as dimethylol alkanoic acid (for example, dimethylol acetic acid, dimethylol butanoic acid, dimethylol propionic acid, dimethylol butyric acid, dimethylol pentanoic acid). These can be used alone or in combination of two or more.
- neutralizing agent examples include ammonia, N-methylmorpholine, triethylamine, dimethylethanolamine, methyldiethanolamine, triethanolamine, morpholine, tripropylamine, ethanolamine, triisopropanolamine, 2-amino-2-methyl-1 -Propanol and the like. These can be used alone or in combination of two or more.
- chain extenders include low molecular weight diol compounds such as ethylene glycol, propylene glycol, 1,4-butanediol, neopentyl glycol, furan methanol, diethylene glycol, triethylene glycol, tetraethylene glycol, and the like.
- Polyether diol compounds obtained by addition polymerization of ethylene oxide, propylene oxide, tetrahydrofuran, etc .; obtained from the above low molecular weight diol compounds and dicarboxylic acids such as (anhydrous) succinic acid, adipic acid, (anhydrous) phthalic acid, and their anhydrides Polyester diols having a hydroxyl group at the terminal; polyhydric alcohols such as trimethylolethane and trimethylolpropane; amino alcohols such as monoethanolamine, diethanolamine and triethanolamine Lumpur ethylenediamine, propylene diamine, butylene diamine, hexamethylene diamine, phenylene diamine, toluene diamine, xylene diamine, diamine compounds such as isophoronediamine; water, ammonia, hydrazine, may be mentioned dibasic acid hydrazide and the like. These can be used alone or in combination of two or more.
- the U resin preferably has a number average molecular weight of 5,000 to 600,000, more preferably 10,000 to 400,000, and an acid value of preferably 10 or more, more preferably 10 to 50, and particularly preferably 20 to 45.
- an acid value preferably 10 or more, more preferably 10 to 50, and particularly preferably 20 to 45.
- preferable U resins include “Superflex (registered trademark)” series manufactured by Daiichi Kogyo Seiyaku Co., Ltd., “Adekabon titer (registered trademark) HUX” series manufactured by ADEKA, and “Takelac ( Commercially available U resins such as “Registered Trademarks” W, WPB, WS ”series and“ Hydran (registered trademark) ”series manufactured by DIC.
- the easy-adhesion composition may be diluted with an aqueous solvent from the viewpoint of workability when forming the easy-adhesion layer.
- aqueous solvent include water or water and hydrophilic organic solvents (for example, alcohol solvents such as methanol, ethanol, isopropyl alcohol, ethylene glycol, and propylene glycol; ester solvents such as ethyl acetate, butyl acetate, and ⁇ -butyrolactone; A mixed solvent with a ketone solvent such as acetone; an ether solvent such as tetrahydrofuran or dioxane; an aprotic polar solvent such as N-methylpyrrolidone) can be used, but water is particularly preferable.
- alcohol solvents such as methanol, ethanol, isopropyl alcohol, ethylene glycol, and propylene glycol
- ester solvents such as ethyl acetate, butyl acetate, and ⁇ -butyrolactone
- the content of the U resin in the easy-adhesion composition is not particularly limited, and may be appropriately set in consideration of coating workability and the like.
- the content is preferably 1 to 25% by weight, more preferably 3 to 20% by weight. More preferably, it is 5 to 15% by weight. If the U resin in the easy-adhesive composition is in the above range, it is preferable because workability during formation of the easy-adhesive layer is excellent.
- the solid content of the easy-adhesive composition may be appropriately set in consideration of application workability and the like, but is preferably 1 to 30% by weight, more preferably 2 to 25% by weight, and further preferably 3 to 20% by weight. %.
- the S compound is not particularly limited as long as it is a water-soluble compound having two or more carbodiimide groups in the molecule.
- an isocyanate-terminated polycarbodiimide was synthesized by a condensation reaction involving decarbonization of an organic diisocyanate compound. Thereafter, a polycarbodiimide resin obtained by reacting an isocyanate group with a hydrophilic organic compound having a reactive functional group and sealing the terminal isocyanate with a hydrophilic segment, which is soluble in water. It is done.
- S compound examples include “Carbodilite (registered trademark) SV-02”, “Carbodilite (registered trademark) V-02”, “Carbodilite (registered trademark) V-04”, “Carbodilite (registered trademark) V-” manufactured by Nisshinbo Chemical Co., Ltd.
- Commercially available products such as “10”, “Carbodilite (registered trademark) V-02-L2” can be used.
- the amount of S compound used is preferably 1 to 25 parts by weight, more preferably 3 to 20 parts by weight, still more preferably 5 to 15 parts by weight, based on 100 parts by weight of the U resin, in terms of solid content. is there.
- the D compound is not particularly limited as long as it is a water-dispersible compound having two or more carbodiimide groups in the molecule.
- an isocyanate-terminated polycarbodiimide is synthesized by a condensation reaction involving decarbonization of an organic diisocyanate compound. After that, a polycarbodiimide resin obtained by reacting an isocyanate group with a hydrophilic organic compound having a reactive functional group and sealing the terminal isocyanate with a hydrophilic segment, which is finely dissolved in water. What disperses (emulsifies).
- the amount of D compound used is preferably 1 to 25 parts by weight, more preferably 1 to 20 parts by weight, still more preferably 1 to 10 parts by weight, based on 100 parts by weight of U resin, in terms of solid content. is there.
- the weight ratio (S / D) between the S compound and the D compound in the easy-adhesion composition is usually in the range of 30:70 to 95: 5, preferably 40:60 to 90:10, and more preferably 50:50 to 80:20.
- the easy-adhesion composition can contain any appropriate fine particles, preferably water-dispersible fine particles, in accordance with a desired function.
- the fine particles either inorganic fine particles or organic fine particles can be used.
- the inorganic fine particles include inorganic oxides such as silica, titania, alumina, zirconia, calcium carbonate, talc, clay, calcined kaolin, calcined calcium silicate, hydrated calcium silicate, aluminum silicate, magnesium silicate, calcium phosphate, and the like.
- the organic fine particles include silicone resins, fluorine resins, (meth) acrylic resins, (meth) acrylonitrile resins, and the like.
- (meth) acrylonitrile resin is preferable. Fine particles made of a (meth) acrylonitrile-based resin are further excellent in blocking inhibition ability, are excellent in transparency, do not cause haze, and are not colored. Therefore, the influence of the easy-contact layer on the optical characteristics is small. In addition, the strength and adhesion of the easy-adhesion layer are reduced by adding fine particles, but the easy-adhesion layer containing fine particles made of (meth) acrylonitrile resin is the strength and adhesion of the easy-adhesion layer. It is preferable because it is possible to suppress the decrease in the thickness.
- the average particle diameter of the fine particles is not particularly limited, but is preferably 1 to 500 nm, more preferably 50 to 350 nm, and still more preferably 100 to 300 nm from the viewpoint of maintaining the transparency of the easy-contact layer.
- the above average particle diameter means a median diameter (d50) measured by laser diffraction / scattering particle size distribution measurement.
- the content of fine particles is preferably 0.1 to 15 parts by weight in terms of solid content with respect to 100 parts by weight of U resin. More preferred is 0.3 to 5 parts by weight, still more preferred is 0.5 to 3 parts by weight.
- the easy-adhesion composition may contain a crosslinking agent different from the above-described S and D compounds or a resin having a crosslinking group in order to improve the coating film strength.
- a crosslinking agent include urea, epoxy, melamine, isocyanate, oxazoline, silanol and the like.
- the easy-adhesion composition can further contain any appropriate additive.
- the additive include a dispersion stabilizer, a thixotropic agent, an antioxidant, an ultraviolet absorber, an antifoaming agent, a thickener, a dispersant, a surfactant, a catalyst, a lubricant, and an antistatic agent.
- FIG. 1 shows an example of the optical film of the present invention.
- An optical film 1 shown in FIG. 1 has an easy adhesion layer 3 formed from the above-mentioned easy adhesion composition on one surface of a thermoplastic resin film 2.
- an easy adhesion layer may be formed on both surfaces of the thermoplastic resin film.
- thermoplastic resin constituting the thermoplastic resin film examples include cellulose resins such as triacetyl cellulose, polyester resins, polyether sulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, Examples include cyclic polyolefin resins, (meth) acrylic resins, polyarylate resins, polystyrene resins, and polyvinyl alcohol resins. These can be used alone or in combination of two or more. Among these, the (meth) acrylic resin (hereinafter sometimes abbreviated as “ACR”) is inferior in adhesiveness with a hydrophilic adhesive, and thus the effect of the present invention is particularly remarkable when ACR is used.
- ACR the (meth) acrylic resin
- the glass transition temperature (hereinafter referred to as Tg) of ACR is preferably 115 ° C. or higher, more preferably 120 ° C. or higher, and further preferably 125 ° C. or higher.
- the thermoplastic resin film can be excellent in durability by containing ACR having a Tg of 115 ° C. or higher as a main component.
- the upper limit of Tg is not particularly limited, but is usually 170 ° C. or lower from the viewpoint of moldability and the like.
- ACR examples include poly (meth) acrylic acid esters such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymers, methyl methacrylate- (meth) acrylic acid ester copolymers, and methyl methacrylate.
- polymer having an alicyclic hydrocarbon group for example, methyl methacrylate-methacrylic acid
- Acid cyclohexyl copolymer resistance methyl methacrylate- (meth) acrylate norbornyl copolymer, etc.
- poly (meth) acrylate C1-6 alkyl such as poly (meth) acrylate is preferable, and methacrylic acid having methyl methacrylate as a main component (50 to 100% by weight, preferably 70 to 100% by weight) is preferable.
- An acid methyl resin is more preferable.
- ACR include, for example, “Acrypet (registered trademark) VH”, “Acrypet (registered trademark) VRL20A” manufactured by Mitsubishi Rayon Co., Ltd., high Tg (meta) obtained by intramolecular crosslinking and intramolecular cyclization reaction.
- An acrylic resin is mentioned.
- the ACR preferably has a ring structure in the main chain in that it has high heat resistance, high transparency, and high mechanical strength.
- the ACR having a ring structure in the main chain include a resin having a glutaric anhydride structure or a glutarimide structure (WO2007 / 26659, WO2005 / 108438), a maleic anhydride structure or an N-substituted maleimide structure. Resins (Japanese Patent Laid-Open Nos. 57-153008 and 2007-31537) and resins having a lactone ring structure (Japanese Patent Laid-Open Nos. 2006-96960, 2006-171464, and 2007-63541) JP, 2008-191426, A).
- the thermoplastic resin film may contain an additive.
- additives include hindered phenol-based, phosphorus-based and sulfur-based antioxidants; light-resistant stabilizers, weather-resistant stabilizers, heat stabilizers and other stabilizers; reinforcing materials such as glass fibers and carbon fibers; ultraviolet rays Absorbers; Near infrared absorbers; Flame retardants; Antistatic agents such as anionic, cationic and nonionic surfactants; Colorants such as inorganic pigments, organic pigments and dyes; Organic fillers and inorganic fillers; Resin modification Agents; organic fillers and inorganic fillers; plasticizers; lubricants; flame retardants; retardation reducing agents and the like.
- thermoplastic resin film is not particularly limited.
- the thermoplastic resin and other polymers and additives are sufficiently mixed by any appropriate mixing method and heated in advance. From the plastic resin composition, it can be formed into a film.
- the thermoplastic resin and other polymers, additives, and the like may be made into separate solutions and mixed to form a uniform mixed solution, and then formed into a film.
- the film raw material is pre-blended with any appropriate mixer such as an omni mixer, and then the obtained mixture is extruded and kneaded.
- the kneader used for extrusion kneading is not particularly limited.
- any suitable mixer such as an extruder such as a single screw extruder or a twin screw extruder or a pressure kneader may be used. Can do.
- the film forming method examples include any appropriate film forming method such as a solution casting method (solution casting method), a melt extrusion method, a calendar method, and a compression molding method. Of these film forming methods, the melt extrusion method is preferred.
- melt extrusion method examples include a T-die method and an inflation method.
- the molding temperature is preferably 150 to 350 ° C, more preferably 200 to 300 ° C.
- a T-die When forming a film by the T-die method, a T-die is attached to the tip of a known single-screw extruder or twin-screw extruder, a film is formed by the T die, and then the film is wound to form a roll. A film can be obtained.
- the thermoplastic resin film may be an unstretched film or a stretched film.
- a stretched film either a uniaxially stretched film or a biaxially stretched film may be used.
- a biaxially stretched film either a simultaneous biaxially stretched film or a sequential biaxially stretched film may be used.
- biaxial stretching the mechanical strength is improved and the film performance is improved.
- the stretching temperature is preferably in the vicinity of the glass transition temperature of the thermoplastic resin composition as the film raw material, and specifically, preferably (glass transition temperature ⁇ 30 ° C.) to (glass transition temperature + 100 ° C.), more preferably Is in the range of (glass transition temperature ⁇ 20 ° C.) to (glass transition temperature + 80 ° C.). If the stretching temperature is less than (glass transition temperature-30 ° C.), a sufficient stretching ratio may not be obtained. On the other hand, if the stretching temperature exceeds (glass transition temperature + 100 ° C.), the resin composition may flow, and stable stretching may not be performed.
- the draw ratio defined by the area ratio is preferably 1.1 to 25 times, more preferably 1.3 to 10 times. There exists a possibility that it may not lead to the improvement of the toughness accompanying extending
- the stretching speed is unidirectional, preferably 10 to 20,000% / min, more preferably 100 to 10,000% / min. When the stretching speed is less than 10% / min, it takes time to obtain a sufficient stretching ratio, and the production cost may increase. If the stretching speed exceeds 20,000% / min, the stretched film may be broken.
- thermoplastic resin film can be subjected to a heat treatment (annealing) or the like after the stretching treatment in order to stabilize its optical isotropy and mechanical properties.
- Arbitrary appropriate conditions can be employ
- the thickness of the thermoplastic resin film is preferably 5 to 200 ⁇ m, more preferably 10 to 100 ⁇ m. If the thickness is less than 5 ⁇ m, sufficient strength as an optical film may not be obtained. When the thickness exceeds 200 ⁇ m, the transparency is lowered and there is a possibility that it is not suitable for use as an optical film.
- the thickness of the easy-adhesion layer can be set to any appropriate value.
- the thickness is preferably 0.1 to 10 ⁇ m, more preferably 0.1 to 5 ⁇ m, and particularly preferably 0.2 to 1.0 ⁇ m. By setting to such a range, it is excellent in adhesiveness with another functional film, and it can suppress that a phase difference expresses in an easily bonding layer.
- the functional layer is, for example, an antistatic layer, an adhesive layer, an adhesive layer, an easy adhesion layer, an antiglare layer (non-glare) layer, an antifouling layer such as a photocatalyst layer, an antireflection layer, a hard coat layer, an ultraviolet shielding layer, A heat ray shielding layer, an electromagnetic wave shielding layer, a gas barrier layer, etc. are mentioned.
- the optical film can be used as, for example, a polarizer protective film, a retardation film, a viewing angle compensation film, a light diffusion film, a reflection film, an antireflection film, an antiglare film, a brightness enhancement film, and a conductive film for a touch panel.
- a polarizer protective film is particularly preferable.
- a polarizing plate 10 shown in FIG. 2 has an adhesive 5 on the surface of the optical film 1 having the easy adhesion layer 3 formed from the above-mentioned easy adhesion composition on one surface of the thermoplastic resin film 2.
- the polarizer 6 has a stacked structure.
- the polarizing plate 10 may have a protective film laminated via an adhesive layer on the opposite side of the polarizer 6 from the optical film 1.
- any appropriate polarizer can be adopted depending on the purpose.
- dichroic substances such as iodine and dichroic dyes are adsorbed on hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene-vinyl acetate copolymer partially saponified films.
- polyene-based oriented films such as a uniaxially stretched product, a polyvinyl alcohol dehydrated product and a polyvinyl chloride dehydrochlorinated product.
- a polarizer obtained by adsorbing a dichroic substance such as iodine on a polyvinyl alcohol film and uniaxially stretching is particularly preferable because of its high polarization dichroic ratio.
- the thickness of these polarizers is not particularly limited, but is generally about 1 to 80 ⁇ m.
- the adhesive layer is formed from an adhesive composition containing a polyvinyl alcohol-based resin.
- Arbitrary appropriate protective films can be employ
- the image display apparatus of the present invention includes the polarizing plate described above.
- Specific examples of the image display device include a self-luminous display device such as an electroluminescence (EL) display, a plasma display (PD), a field emission display (FED), and a liquid crystal display (LCD). .
- EL electroluminescence
- PD plasma display
- FED field emission display
- LCD liquid crystal display
- an easy-adhesive composition comprising a water-dispersible urethane resin diluted with an aqueous solvent and having a carboxyl group, a water-soluble carbodiimide compound, and a water-dispersible carbodiimide compound, It coats on at least one surface of a thermoplastic resin film, forms a coat (application process), and then dries the coat and forms an easy-adhesion layer (dry process).
- any appropriate method can be adopted as a method of applying the easy-adhesion composition in the application step.
- Examples thereof include a bar coating method, a roll coating method, a gravure coating method, a rod coating method, a slot orifice coating method, a curtain coating method, and a fountain coating method.
- the thickness of the coating film formed in the coating process can be appropriately adjusted according to the thickness required when the coating film becomes an easy-adhesion layer.
- the surface of the thermoplastic resin film to which the easy-adhesion composition is applied is preferably subjected to a surface treatment.
- the surface treatment is preferably corona discharge treatment or plasma treatment. By performing the corona discharge treatment, the adhesion between the thermoplastic resin film and the easy adhesion layer can be improved.
- the drying process is not particularly limited, and a conventionally known method can be used.
- the drying temperature is typically 50 ° C. or higher, preferably 90 ° C. or higher, more preferably 110 ° C. or higher. By setting the drying temperature in such a range, an optical film excellent in color resistance (particularly under high temperature and high humidity) can be obtained.
- the upper limit of the drying temperature is preferably 200 ° C. or lower, more preferably 180 ° C. or lower.
- thermoplastic resin film When producing an optical film that is a stretched film from an unstretched thermoplastic resin film, and an optical film that is a biaxially stretched film from a uniaxially stretched thermoplastic resin film by the method for producing an optical film of the present invention. In some cases, it is necessary to stretch these thermoplastic resin films at any point.
- the stretching of the thermoplastic resin film may be performed before the formation of the easy adhesion layer or after the formation of the easy adhesion layer. Moreover, you may perform formation of an easily bonding layer and extending
- the thermoplastic resin film on which the coating film of the easy-adhesive composition is formed may be stretched in a heated atmosphere. Due to the heat applied to the film for stretching, the coating film of the easy-adhesive composition formed on the surface of the thermoplastic resin film is dried to form an easy-adhesive layer. If it does in this way, the extending
- Examples 1 to 5 and Comparative Examples 1 to 10 Manufacture of an easily bonding composition Each component shown in Table 1 and 2 was mixed so that it might become the solid content amount (unit is a weight part) shown in Table 1 and 2, and the easily bonding composition was manufactured. In addition, ion-exchange water was used as an aqueous solvent for the easy-adhesion composition, and the solid content was adjusted to 8% by weight.
- the polyvinyl alcohol-type adhesive composition was apply
- peel adhesion strength was evaluated according to the following criteria. ⁇ : Peeling adhesive strength is superior or equivalent to that of the reference polarizing plate. ⁇ : Peeling adhesive strength is inferior to that of the reference polarizing plate. X: Not closely adhered and cannot be measured.
- the measurement sample obtained in the same manner as described above was put in a constant temperature and humidity chamber at a temperature of 60 ° C. and a humidity of 90% RH, and was subjected to a heat treatment that was allowed to stand for 250 hours and 500 hours. The peel adhesion strength was measured. From the measurement results, the peel adhesion strength was evaluated according to the following criteria.
- an easily adhesive composition containing a water-dispersible urethane resin (U resin) having a carboxyl group, a water-soluble carbodiimide compound (S compound), and a water-dispersible carbodiimide compound (D compound) is used.
- U resin water-dispersible urethane resin
- S compound water-soluble carbodiimide compound
- D compound water-dispersible carbodiimide compound
- the optical films of Comparative Examples 1 to 7 containing no cross-linking agent or containing only the S compound showed the result that the adhesiveness with the polarizer decreased under high temperature and high humidity.
- the optical films of Comparative Examples 8 to 10 containing only the D compound showed excellent results in inferior initial adhesiveness, although they were excellent in adhesiveness when used for a long time under high temperature and high humidity.
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Abstract
Description
(1)カルボキシル基を有する水分散性ウレタン樹脂100重量部と、水溶性カルボジイミド化合物1~25重量部と、水分散性カルボジイミド化合物1~25重量部と、を含有する易接着組成物が提供される。
(2)前記水溶性カルボジイミド化合物と前記水分散性カルボジイミド化合物との重量比が30:70~95:5の範囲である、(1)記載の易接着組成物;
(3)前記水分散性ウレタン樹脂100重量部に対し、さらに、微粒子を0.1~15重量部含有する、(1)又は(2)記載の易接着組成物;
(4)熱可塑性樹脂フィルムと、該熱可塑性樹脂フィルムの少なくとも一方の表面に設けられ、且つ(1)~(3)のいずれか記載の易接着組成物から形成される易接着層とを備える光学フィルム;
(5)前記熱可塑性樹脂フィルムは、(メタ)アクリル系樹脂からなる(4)記載の光学フィルム;及び
(6)偏光子と、該偏光子の表面を被覆して保護する(4)又は(5)記載の光学フィルムとを備える偏光板;を提供する。
(7)水系溶媒で希釈され、カルボキシル基を有する水分散性ウレタン樹脂100重量部と、水溶性カルボジイミド化合物1~25重量部と、水分散性カルボジイミド化合物1~25重量部と、を含有する易接着組成物を、熱可塑性樹脂フィルムの少なくとも一方の表面に塗布して塗膜を形成する工程と、前記塗膜を乾燥して易接着層を形成する工程からなる光学フィルムの製造方法を提供する。
本発明の易接着組成物は、カルボキシル基を有する水分散性ウレタン樹脂(以下単にU樹脂と呼ぶことがある)と、架橋剤として水溶性カルボジイミド化合物(以下単にS化合物と呼ぶことがある)及び水分散性カルボジイミド化合物(以下単にD化合物と呼ぶことがある)と、を含有する。このように構成された易接着組成物は、高温高湿下での長時間使用における初期性能の低下を抑制するとともに、より過酷な環境下においても密着性に優れる。
好ましいU樹脂の具体例としては、第一工業製薬社製の「スーパーフレックス(登録商標)」シリーズ、ADEKA社製の「アデカボンタイター(登録商標)HUX」シリーズ、三井化学社製の「タケラック(登録商標)W、WPB、WS」シリーズ、DIC社製の「ハイドラン(登録商標)」シリーズ等の市販のU樹脂が挙げられる。
図1に本発明の光学フィルムの一例を示す。図1に示す光学フィルム1は、熱可塑性樹脂フィルム2の一方の表面に上述した易接着組成物から形成される易接着層3を有する。なお、本発明の光学フィルムは、熱可塑性樹脂フィルムの双方の表面に易接着層が形成されていても良い。
次に、本発明の偏光板の一例を説明する。図2に示す偏光板10は、熱可塑性樹脂フィルム2の一方の表面に上述した易接着組成物から形成される易接着層3を有する光学フィルム1の易接着層側の表面に接着剤5を介し、偏光子6が積層された構造を有する。なお、図示しないが、偏光板10は、偏光子6の光学フィルム1と反対側に、接着剤層を介して積層された保護フィルムを有していても良い。
本発明の画像表示装置は、上述した偏光板を備える。画像表示装置の具体例としては、エレクトロルミネッセンス(EL)ディスプレイ、プラズマディスプレイ(PD)、電界放出ディスプレイ(FED:Field Emission Display)のような自発光型表示装置、液晶表示装置(LCD)が挙げられる。
本発明の光学フィルムの好ましい製造方法においては、水系溶媒で希釈され、カルボキシル基を有する水分散性ウレタン樹脂と、水溶性カルボジイミド化合物と、水分散性カルボジイミド化合物と、を含む易接着組成物を、熱可塑性樹脂フィルムの少なくとも一方の表面に塗布して塗膜を形成(塗布工程)し、次いで塗膜を乾燥して易接着層を形成(乾燥工程)する。
<U樹脂>
カルボキシル基を有する水分散性ウレタン樹脂のエマルジョン[第一工業製薬社製、スーパーフレックス(登録商標)210、固形分量35重量%]
<S化合物(1)>
水溶性カルボジイミド化合物を含む水溶液[日清紡ケミカル社製、カルボジライト(登録商標)V-02-L2、固形分量40重量%]
<S化合物(2)>
水溶性カルボジイミド化合物を含む水溶液[日清紡ケミカル社製、カルボジライト(登録商標)V-10、固形分量40重量%]
<D化合物>
水分散性カルボジイミド化合物のエマルジョン[日清紡ケミカル社製、カルボジライト(登録商標)E-02、固形分量40重量%]
<微粒子>
アクリロニトリル系微粒子(PAN微粒子)を含むエマルジョン[積水化学工業社製、ADVANCELL NS K-001、平均粒子径150nm、固形分量20重量%]
1.易接着組成物の製造
表1及び2に示す各成分を、表1及び2に示す固形分量(単位は重量部)となるよう混合し、易接着組成物を製造した。なお、易接着組成物の水系溶媒としてはイオン交換水を使用し、固形分量は8重量%となるよう調製した。
アクリル系樹脂組成物[Tg:135℃、溶融粘度:700Pa・s(温度270℃、せん断速度100(1/sec))]のペレットを、単軸押出機(φ=20.0mm、L/D=25)及びコートハンガータイプTダイ(幅150mm)を用いて280℃で溶融押出し、110℃に保持した冷却ロールに溶融状態の上記樹脂組成物を吐出して、厚さ100μmのアクリル系樹脂フィルムを形成した。次に、アクリル系樹脂フィルムの一方の表面に、上記で得られた易接着組成物を、バーコーターを用いて塗布した後、熱風乾燥機に投入して100℃で90秒間乾燥した。そして、テーブル延伸機を用いて当該フィルムを一軸延伸(延伸倍率:2.5倍)し、厚さ40μmのアクリル系樹脂フィルムの表面に、厚さ0.3μmの易接着層を有する光学フィルムを製造した。
上記で得られた光学フィルムの易接着層側に、ポリビニルアルコール系接着剤組成物を塗布した。また、ケン化処理を施した厚さ40μmのトリアセチルセルロースフィルム(保護フィルム)の片側にポリビニルアルコール系接着剤組成物を塗布した。次に、厚さ30μmの偏光子の両側それぞれに光学フィルム及び保護フィルムをポリビニルアルコール系接着剤塗布層を介して積層し、得られた積層体を熱風乾燥機(70℃)に投入して5分乾燥させて、偏光板を製造した。また、偏光子の両側にトリアセチルセルロースからなる保護フィルムを設けた評価用の基準偏光板を同様に作成した。
(1)初期密着性
上記で得られた偏光板から25mm×250mmの寸法の試験片を切り出し、試験片の光学フィルムの表面に粘着加工を施した後、ガラス板に貼り付け測定用サンプルを得た。その後、サンプルのの偏光子と光学フィルムとの間に切込みを入れ、偏光子と保護フィルムとを掴み、日本接着剤工業規格 JAI 13-1996の浮動ローラー法に準じて、90度での剥離接着強さを測定した。なお、基準偏光板においても同様の条件で剥離接着強さを測定した。測定結果から、剥離接着強さを次の基準により評価した。
○:基準偏光板よりも剥離接着強さが優れるあるいは同等
△:基準偏光板よりも剥離接着強さが劣る
×:密着しておらず測定不可
(2)耐湿熱性(60℃、90%RH)
上記と同様にして得た測定用サンプルを温度60℃、湿度90%RHの恒温恒湿機に入れ、250時間及び500時間放置する熱処理を施した以外は、初期密着性の評価と同様にして、剥離接着強さを測定した。測定結果から剥離接着強さを次の基準により評価した。
◎:基準偏光板よりも剥離接着強さが優れる
○:基準偏光板と剥離接着強さが同等
△:基準偏光板よりも剥離接着強さが劣る
×:密着しておらず測定不可
(3)耐湿熱性(80℃、90%RH)
上記と同様にして得た測定用サンプルを温度80℃、湿度90%RHの恒温恒湿機に入れ、100時間放置する熱処理を施した以外は、初期密着性の評価と同様にして、剥離接着強さを測定した。測定結果から剥離接着強さを次の基準により評価した。
◎:基準偏光板よりも剥離接着強さが優れる
○:基準偏光板と剥離接着強さが同等
△:基準偏光板よりも剥離接着強さが劣る
×:密着しておらず測定不可
Claims (7)
- カルボキシル基を有する水分散性ウレタン樹脂100重量部と、水溶性カルボジイミド化合物1~25重量部と、水分散性カルボジイミド化合物1~25重量部と、を含有する易接着組成物。
- 前記水溶性カルボジイミド化合物と前記水分散性カルボジイミド化合物との重量比が30:70~95:5の範囲である請求項1記載の易接着組成物。
- 前記水分散性ウレタン樹脂100重量部に対し、さらに、微粒子を0.1~15重量部含有する請求項1又は2記載の易接着組成物。
- 熱可塑性樹脂フィルムと、該熱可塑性樹脂フィルムの少なくとも一方の表面に設けられ、且つ請求項1乃至3のいずれか記載の易接着組成物から形成される易接着層とを備える光学フィルム。
- 前記熱可塑性樹脂フィルムは、(メタ)アクリル系樹脂からなる請求項4記載の光学フィルム。
- 偏光子と、該偏光子の表面を被覆して保護する請求項4又は5記載の光学フィルムとを備える偏光板。
- 水系溶媒で希釈され、カルボキシル基を有する水分散性ウレタン樹脂100重量部と、水溶性カルボジイミド化合物1~25重量部と、水分散性カルボジイミド化合物1~25重量部と、を含有する易接着組成物を、熱可塑性樹脂フィルムの少なくとも一方の表面に塗布して塗膜を形成する工程と、前記塗膜を乾燥して易接着層を形成する工程からなる光学フィルムの製造方法。
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JP2019105819A (ja) * | 2017-02-06 | 2019-06-27 | 株式会社日本触媒 | 光学フィルムの製造方法および光学フィルム |
JP7122830B2 (ja) | 2017-02-06 | 2022-08-22 | 株式会社日本触媒 | 光学フィルムの製造方法および光学フィルム |
WO2019155791A1 (ja) * | 2018-02-07 | 2019-08-15 | 日東電工株式会社 | 偏光板および画像表示装置 |
JP2019139204A (ja) * | 2018-02-07 | 2019-08-22 | 日東電工株式会社 | 偏光板および画像表示装置 |
WO2021090903A1 (ja) * | 2019-11-06 | 2021-05-14 | 日東電工株式会社 | 偏光板、画像表示装置、偏光板の設計方法、偏光板の製造方法、画像表示装置の製造方法 |
JP2021076656A (ja) * | 2019-11-06 | 2021-05-20 | 日東電工株式会社 | 偏光板、画像表示装置、偏光板の設計方法、偏光板の製造方法、画像表示装置の製造方法 |
WO2022239648A1 (ja) * | 2021-05-08 | 2022-11-17 | 大倉工業株式会社 | 光学フィルム、偏光板、画像表示装置及び光学フィルムの製造方法 |
Also Published As
Publication number | Publication date |
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CN107075298A (zh) | 2017-08-18 |
TWI661021B (zh) | 2019-06-01 |
KR20170084060A (ko) | 2017-07-19 |
CN107075298B (zh) | 2019-09-10 |
KR102394207B1 (ko) | 2022-05-03 |
JP6527878B2 (ja) | 2019-06-05 |
TW201623537A (zh) | 2016-07-01 |
JPWO2016072437A1 (ja) | 2017-08-24 |
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