WO2020100870A1 - 画像表示装置 - Google Patents
画像表示装置 Download PDFInfo
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- WO2020100870A1 WO2020100870A1 PCT/JP2019/044277 JP2019044277W WO2020100870A1 WO 2020100870 A1 WO2020100870 A1 WO 2020100870A1 JP 2019044277 W JP2019044277 W JP 2019044277W WO 2020100870 A1 WO2020100870 A1 WO 2020100870A1
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- WIPO (PCT)
- Prior art keywords
- polarizing film
- adhesive layer
- group
- weight
- film
- Prior art date
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/50—OLEDs integrated with light modulating elements, e.g. with electrochromic elements, photochromic elements or liquid crystal elements
Definitions
- the present invention relates to an image display device.
- a polarizing film used for various image display devices such as liquid crystal display devices and organic EL display devices
- dyed such as iodine and dichroic dyes
- Polyvinyl alcohol-based films (containing dichroic substances) have been used.
- the polarizing film is produced by subjecting a polyvinyl alcohol-based film to various treatments such as swelling, dyeing, crosslinking and stretching in a bath, followed by washing treatment and drying.
- the polarizing film is usually used as a polarizing film (polarizing plate) in which a protective film such as triacetyl cellulose is attached to one surface or both surfaces thereof with an adhesive.
- the polarizing film is used as a laminated polarizing film (optical laminated body) by laminating other optical layers as necessary, and the polarizing film or the laminated polarizing film (optical laminated body) is a liquid crystal cell or an organic EL element. And the like, and the front side transparent member (window layer) on the viewing side and the front side transparent member such as a touch panel, which are bonded together via an adhesive layer or an adhesive layer to provide the above various image display devices. Used.
- a dye-based polarizing film using a dichroic dye such as an azo-based compound generally has a higher temperature and a higher temperature than an iodine-based polarizing film (a polarizing film formed by adsorbing and orienting iodine on a polyvinyl alcohol-based film). It is known that light resistance under high humidity conditions is excellent (Patent Document 2), and in order to improve color loss in a light resistance test of a polarizing plate having the dye-based polarizing film, the polarizing plate is used. It is disclosed that the hindered amine compound is contained in the adhesive used (Patent Document 3).
- a water-insoluble HALS Hindered Amine Light Stabilizer
- an adhesive containing an epoxy compound Patent Document 4
- the polarizing film is colored and the single transmittance thereof is lowered.
- an image display device configured by laminating the above polarizing film or laminated polarizing film with an adhesive layer or an adhesive layer between the image display cell and the front transparent member has a coloring film of a polarizing film.
- the single substance transmittance is significantly reduced.
- an object of the present invention to provide an image display device having an excellent effect of suppressing a decrease in single-piece transmittance due to coloring of a polarizing film in a high temperature environment.
- the present invention is an image display device in which a front transparent member, a polarizing film, and an image display cell are provided in this order via an adhesive layer or an adhesive layer, wherein the polarizing film is a polyvinyl alcohol film.
- the polarizing film is a polyvinyl alcohol film.
- At least one of the polarizing film, the pressure-sensitive adhesive layer, and the adhesive layer contains a hindered amine-based compound, and the hindered amine-based compound has a temperature of 25 ° C.
- Is a water-soluble hindered amine compound that can be dissolved in 1 part by weight or more with respect to 100 parts by weight of water, and the polarizing film has the following general formula (1): X (wt%)> 0.01 (in the general formula (1)).
- X is a laminated body in which a glass plate is bonded to both surfaces of a polarizing film having the transparent protective film bonded to at least one surface of the polarizing film via the adhesive layer via the pressure-sensitive adhesive layer.
- the content of the hindered amine compound in the polarizing film in the laminate left under the condition of 24 ° C. for 24 hours is shown).
- the front transparent member, the polarizing film, and the image display cell are provided in this order via a pressure-sensitive adhesive layer or an adhesive layer, and the polarizing film, the pressure-sensitive adhesive layer, and the adhesive layer.
- At least one of the agent layers contains a water-soluble hindered amine-based compound which is soluble in 1 part by weight or more in 100 parts by weight of water at 25 ° C.
- the polarizing film has an iodine-based polarizing film formed by adsorbing and orienting iodine on a polyvinyl alcohol-based film.
- the iodine-based polarizing film is inferior in durability such as heat resistance to the dye-based polarizing film, and the reason is included in the polarizing film. It is presumed that the iodine generated promotes the deterioration phenomenon called polyene formation that occurs in the dehydration reaction of polyvinyl alcohol in a high temperature environment.
- the hindered amine-based compound contained in at least one of the polarizing film, the pressure-sensitive adhesive layer, and the adhesive layer of the present invention when exposed to a high temperature environment, contains moisture (adhesion) present in the image display device. It is presumed that a part of the water-soluble hindered amine-based compound permeates into the iodine-based polarizing film because it moves (stays) inside the image display device together with the water present in the agent layer, the adhesive layer, etc.). As a result, it is estimated that the water-soluble hindered amine-based compound in the polarizing film can efficiently capture the radicals generated in the above-mentioned polyene conversion reaction under a high temperature environment. It is possible to suppress a decrease in single-body transmittance due to.
- FIG. 1 is a schematic cross-sectional view showing one form of the image display device of the present invention.
- the front transparent member 80 and the polarizing film 10 are attached to each other via the adhesive layer or the adhesive layer 20, and the image display cell 90 and the polarizing film 10 are attached to the adhesive layer or the adhesive layer. It is bonded via the agent layer 30.
- FIG. 2 is a schematic cross-sectional view showing one mode of the single-sided protective polarizing film of the present invention.
- the single-sided protective polarizing film 101 of FIG. 2 shows one embodiment of the polarizing film 10 in which the polarizing film 11 and the transparent protective film 13 are bonded together via the pressure-sensitive adhesive layer or the adhesive layer 50.
- FIG. 3 is a schematic cross-sectional view showing one mode of the double-sided protective polarizing film of the present invention.
- the polarizing film 11 and the transparent protective film 13 are exposed to each other via the adhesive layer or the adhesive layer 50, and the polarizing film 11 and the transparent protective film 12 are adhesive.
- One mode of the polarizing film 10 bonded together via a layer or an adhesive layer 40 is shown.
- the front transparent member, the polarizing film, and the image display cell are provided in this order via a pressure-sensitive adhesive layer or an adhesive layer, and the polarizing film, the pressure-sensitive adhesive layer, and the adhesive layer.
- At least one of the agent layers contains a hindered amine-based compound, and the hindered amine-based compound is a water-soluble hindered amine-based compound that can be dissolved in 1 part by weight or more in 100 parts by weight of water at 25 ° C.
- the hindered amine compounds may be used alone or in combination of two or more.
- the hindered amine-based compound moves (stays) inside the image display device together with the water present inside the image display device (water present in the pressure-sensitive adhesive layer or adhesive layer), thereby coloring the polarizing film in a high temperature environment.
- the hindered amine compound has a molecular weight of preferably 1,000 or less, more preferably 500 or less, and further preferably 300 or less, from the viewpoint of efficiently trapping radicals generated in the polyene reaction. preferable.
- the hindered amine compound of the present invention is a secondary amine or tertiary amine in which an alkyl group is substituted on a carbon adjacent to an amino group to sterically protect the amino group, and for example, an organic group having the following structure: And the like.
- the exemplified compound may include a structure that cannot be dissolved in 1 part by weight or more with respect to 100 parts by weight of water at 25 ° C., but those skilled in the art will consider common general knowledge and the exemplified compound However, it can be immediately confirmed whether 1 part by weight or more can be dissolved in 100 parts by weight of water at 25 ° C.
- R 1 is oxy radical, a hydrogen atom, a hydroxyl group or an alkyl group having 1 to 30 carbon atoms, a hydroxyalkyl group, hydroxyalkoxy group or an alkoxy group, a R 2, R 5 independently represents a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, and n represents 0 or 1.
- R 1 is oxy radical, a hydrogen atom, a hydroxyl group or an alkyl group having 1 to 30 carbon atoms, a hydroxyalkyl group, hydroxyalkoxy group or an alkoxy group, a R 2, R 5 independently represents a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, and n represents 0 or 1.
- the left side of the dotted line part is arbitrary. Represents an organic group of.
- the hindered amine compounds are known compounds and are described, for example, in US Pat. No. 4,619,956, columns 5 to 11 and US Pat. No. 4,839,405, columns 3 to 5. 2,2,6,6-tetraalkylpiperidine compounds, or their acid addition salts or their complexes with metal compounds, as described above.
- Examples of the compound having an organic group include compounds represented by the following general formulas (2) to (5).
- R 1 is oxy radical, a hydrogen atom, a hydroxyl group or an alkyl group having 1 to 30 carbon atoms, a hydroxyalkyl group, hydroxyalkoxy group or an alkoxy group, a R 2, R 5 independently represents a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, and R 6 represents a hydrogen atom or an alkyl group, an acyl group, or an aryl group having 1 to 10 carbon atoms.
- R 1 to R 5 and n are the same as above, and R 7 and R 8 are independently a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, Represents an acyl group or an aryl group.
- R 9 to R 11 are independently a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, Represents an acyl group, an amino group, an alkoxy group, a hydroxy group, or an aryl group.
- R 12 is a hydrogen atom, or an alkyl group having 1 to 10 carbon atoms, an amino group, an alkoxy group, a hydroxy group. Represents a group or an aryl group.
- R 1 is preferably an oxy radical, a hydrogen atom, a hydroxy group, or an alkyl group, from the viewpoint of effectively suppressing accelerated deterioration of polyvinyl alcohol, and an oxy radical group. Is more preferable.
- R 2 to R 5 are preferably alkyl groups having 1 to 6 carbon atoms, from the viewpoint of easy availability and water solubility. Is more preferably an alkyl group of 1 to 3.
- R 6 is preferably a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, and more preferably a hydrogen atom, from the viewpoint of easy availability and water solubility. preferable.
- R 7 and R 8 each independently represent a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, from the viewpoints of availability and water solubility. More preferably, it is an atom.
- R 9 to R 11 are preferably hydrogen atoms or alkyl groups having 1 to 10 carbon atoms from the viewpoints of easy availability and water solubility.
- R 12 is preferably a hydroxy group, an amino group, or an alkoxy group, from the viewpoint of easy availability and water solubility.
- n is preferably 1 from the viewpoint of easy availability.
- the polarizing film of the present invention has a polarizing film formed by adsorbing and orienting iodine on a polyvinyl alcohol film.
- the polyvinyl alcohol (PVA) film a film having a light-transmitting property in a visible light region and capable of dispersing and adsorbing iodine can be used without particular limitation.
- the PVA-based film which is usually used as a raw fabric, preferably has a thickness of about 1 to 100 ⁇ m, more preferably about 1 to 50 ⁇ m, and a width of about 100 to 5000 mm.
- polyvinyl alcohol or its derivative can be mentioned.
- the polyvinyl alcohol derivative include polyvinyl formal, polyvinyl acetal, olefins such as ethylene and propylene, unsaturated carboxylic acids such as acrylic acid, methacrylic acid, and crotonic acid, and their modified alkyl esters, acrylamides, and the like. Is mentioned.
- the polyvinyl alcohol preferably has an average degree of polymerization of about 100 to 10,000, more preferably about 1,000 to 10,000, and even more preferably about 1,500 to 4,500. ..
- the saponification degree of the polyvinyl alcohol is preferably about 80 to 100 mol%, more preferably about 95 mol% to 99.95 mol.
- the average degree of polymerization and the degree of saponification can be determined according to JIS K 6726.
- the polyvinyl alcohol film may contain additives such as a plasticizer and a surfactant.
- the plasticizer include polyols such as glycerin, diglycerin, triglycerin, ethylene glycol, propylene glycol, and polyethylene glycol, and condensates thereof.
- the amount of the additive used is not particularly limited, but is preferably about 20% by weight or less in the polyvinyl alcohol film.
- the content of iodine in the polarizing film is preferably 1% by weight or more and 15% by weight or less.
- the content of the iodine in the polarizing film is preferably 1.5% by weight or more, more preferably 2% by weight or more, from the viewpoint of suppressing color loss during a durability test, and From the viewpoint of preventing polyene formation, it is preferably 12% by weight or less, and more preferably 10% by weight or less.
- the content of the hindered amine compound is preferably 20% by weight or less.
- the content of the hindered amine-based compound in the polarizing film is preferably 0.005% by weight or more, and 0.01% by weight, from the viewpoint of suppressing a decrease in single transmittance due to coloring of the polarizing film in a high temperature environment. % Or more, more preferably 0.1% by weight or more, further preferably 15% by weight or less, more preferably 12% by weight or less, and 10% by weight or less. It is more preferable that there is.
- the method for producing the polarizing film can be obtained by subjecting the polyvinyl alcohol-based film to an arbitrary swelling step and a washing step, and at least a dyeing step, a crosslinking step, and a stretching step.
- the treatment bath in any one or more treatment steps of the swelling step, the washing step, the dyeing step, the crosslinking step, and the stretching step is the hindered amine. It suffices to include a system compound.
- the content of the hindered amine compound contained in the polarizing film and the content of iodine are the hindered amine compound contained in any of the treatment baths in the swelling step, the dyeing step, the crosslinking step, the stretching step and the washing step. And the concentration of iodine and potassium iodide, and the treatment temperature and treatment time of each treatment bath described above.
- the washing step is performed after the dyeing step, the crosslinking step, and the stretching step, the washing step is performed after considering the treatment conditions in the dyeing step, the crosslinking step, the stretching step, and the like.
- the content of the hindered amine-based compound and the content of iodine can be easily adjusted to a desired range.
- each treatment bath in the swelling step, the dyeing step, the crosslinking step, the stretching step and the washing step contains an additive such as a zinc salt, a pH adjusting agent, a pH buffering agent and other salts.
- a zinc salt include zinc halides such as zinc chloride and zinc iodide; inorganic zinc salts such as zinc sulfate and zinc acetate.
- the pH adjuster include strong acids such as hydrochloric acid, sulfuric acid and nitric acid, and strong bases such as sodium hydroxide and potassium hydroxide.
- Examples of the pH buffer include carboxylic acids such as acetic acid, oxalic acid and citric acid and salts thereof, and weak inorganic acids such as phosphoric acid and carbonic acid and salts thereof.
- Examples of the other salts include chlorides such as sodium chloride, potassium chloride and barium chloride, nitrates such as sodium nitrate and potassium nitrate, sulfates such as sodium sulfate and potassium sulfate, and alkali metals and alkaline earth metals. Salt etc. are mentioned.
- the concentration of the hindered amine compound contained in any of the treatment baths cannot be unconditionally determined because it is affected by the number of treatments, the treatment time, and the treatment temperature of each treatment, but the content of the hindered amine compound in the polarizing film is not included. From the viewpoint of efficiently controlling the amount, it is usually preferably 0.01% by weight or more, more preferably 0.05% by weight or more, further preferably 0.1% by weight or more, and , 30 wt% or less, preferably 20 wt% or less, more preferably 10 wt% or less.
- the swelling step is a treatment step of immersing the polyvinyl alcohol-based film in a swelling bath, which can remove stains and blocking agents on the surface of the polyvinyl alcohol-based film, and can also be dyed by swelling the polyvinyl alcohol-based film. Unevenness can be suppressed.
- a medium containing water as a main component such as water, distilled water, or pure water, is usually used.
- a surfactant, alcohol, etc. may be appropriately added according to a conventional method.
- the temperature of the swelling bath is preferably about 10 to 60 ° C., more preferably about 15 to 45 ° C., and further preferably about 18 to 35 ° C.
- the dipping time in the swelling bath cannot be unconditionally determined because the degree of swelling of the polyvinyl alcohol film is affected by the temperature of the swelling bath, but is preferably about 5 to 300 seconds, and preferably 10 to 200 seconds. It is more preferably about 10 to 100 seconds, still more preferably about 20 to 100 seconds.
- the swelling step may be performed only once, or may be performed multiple times as necessary.
- the dyeing step is a step of immersing the polyvinyl alcohol film in a dyeing bath (iodine solution), and iodine can be adsorbed and oriented on the polyvinyl alcohol film.
- the iodine solution is preferably an aqueous iodine solution and contains iodine and iodide as a dissolution aid.
- the iodide include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and iodide.
- examples include titanium.
- potassium iodide is preferable from the viewpoint of controlling the content of potassium in the polarizing film.
- the iodine concentration in the dyeing bath is preferably about 0.01 to 1% by weight, more preferably about 0.02 to 0.5% by weight.
- the iodide concentration is preferably about 0.01 to 20% by weight, more preferably about 0.05 to 10% by weight, and about 0.1 to 5% by weight. It is more preferable that there is.
- the temperature of the dyeing bath is preferably about 10 to 50 ° C., more preferably about 15 to 45 ° C., and further preferably about 18 to 30 ° C.
- the immersion time in the dyeing bath cannot be unconditionally determined because the degree of dyeing of the polyvinyl alcohol film is affected by the temperature of the dyeing bath, but it is preferably about 10 to 300 seconds, and 20 to 240 seconds. It is more preferable that the degree is approximately.
- the dyeing step may be performed only once, or may be performed multiple times as necessary.
- the cross-linking step is a step of immersing the polyvinyl alcohol-based film in a treatment bath containing a boron compound (cross-linking bath), and the polyvinyl alcohol-based film is cross-linked by the boron compound, and the iodine molecule or the dye molecule is cross-linked. Can be adsorbed on the structure.
- the boron compound include boric acid, borate, and borax.
- the cross-linking bath is generally an aqueous solution, but may be, for example, a mixed solution of an organic solvent miscible with water and water. Further, the crosslinking bath may contain potassium iodide from the viewpoint of controlling the content of potassium in the polarizing film.
- the concentration of the boron compound in the crosslinking bath is preferably about 1 to 15% by weight, more preferably about 1.5 to 10% by weight, and even more preferably about 2 to 5% by weight. preferable.
- concentration of potassium iodide in the crosslinking bath is preferably about 1 to 15% by weight, more preferably about 1.5 to 10% by weight. More preferably, it is more preferably about 2 to 5% by weight.
- the temperature of the crosslinking bath is preferably about 20 to 70 ° C, more preferably about 30 to 60 ° C.
- the immersion time in the crosslinking bath cannot be unconditionally determined because the degree of crosslinking of the polyvinyl alcohol film is affected by the temperature of the crosslinking bath, but it is preferably about 5 to 300 seconds, preferably 10 to 200 seconds. It is more preferable that the degree is approximately.
- the cross-linking step may be performed only once, or may be performed multiple times as necessary.
- the stretching step is a treatment step of stretching the polyvinyl alcohol film in at least one direction at a predetermined ratio.
- a polyvinyl alcohol film is uniaxially stretched in the transport direction (longitudinal direction).
- the stretching method is not particularly limited, and either a wet stretching method or a dry stretching method can be adopted.
- the stretching step may be performed only once, or may be performed multiple times as necessary.
- the stretching process may be performed at any stage in manufacturing the polarizing film.
- the stretching bath may contain potassium iodide from the viewpoint of controlling the content of the potassium in the polarizing film.
- the concentration of potassium iodide in the stretching bath is preferably about 1 to 15% by weight, more preferably about 2 to 10% by weight, and 3 It is more preferably about 6 to 6% by weight.
- the treatment bath (stretching bath) may contain the boron compound from the viewpoint of suppressing film breakage during stretching, and in this case, the concentration of the boron compound in the stretching bath is 1 to 15. It is preferably about wt%, more preferably about 1.5 to 10 wt%, and even more preferably about 2 to 5 wt%.
- the temperature of the stretching bath is preferably about 25 to 80 ° C, more preferably about 40 to 75 ° C, and further preferably about 50 to 70 ° C.
- the dipping time in the stretching bath cannot be unconditionally determined because the extent of stretching of the polyvinyl alcohol film is affected by the temperature of the stretching bath, but is preferably about 10 to 800 seconds, and preferably 30 to 500 seconds. It is more preferable that the degree is approximately.
- the stretching treatment in the wet stretching method may be performed together with one or more treatment steps of the swelling step, the dyeing step, the crosslinking step, and the washing step.
- Examples of the dry stretching method include a roll stretching method, a heated roll stretching method, and a compression stretching method.
- the dry stretching method may be performed together with the drying step.
- the total draw ratio (cumulative draw ratio) applied to the polyvinyl alcohol film can be appropriately set according to the purpose, but it is preferably about 2 to 7 times, and preferably about 3 to 6.8 times. More preferably, it is more preferably about 3.5 to 6.5 times.
- the cleaning step is a treatment step of immersing the polyvinyl alcohol-based film in a cleaning bath, and foreign substances remaining on the surface of the polyvinyl alcohol-based film can be removed.
- a medium containing water as a main component such as water, distilled water, or pure water, is usually used.
- the cleaning bath may contain potassium iodide.
- the concentration of potassium iodide in the cleaning bath is 1 to 10% by weight. %, Preferably about 1.5 to 4% by weight, more preferably about 1.8 to 3.8% by weight.
- the temperature of the washing bath is preferably about 5 to 50 ° C, more preferably about 10 to 40 ° C, and further preferably about 15 to 30 ° C.
- the dipping time in the washing bath cannot be unconditionally determined because the washing degree of the polyvinyl alcohol film is affected by the temperature of the washing bath, but it is preferably about 1 to 100 seconds, and preferably 2 to 50 seconds. It is more preferably about 3 to 20 seconds.
- the swelling step may be performed only once, or may be performed multiple times as necessary.
- the method for manufacturing the polarizing film may include a drying step.
- the drying step is a step of drying the polyvinyl alcohol film washed in the washing step to obtain a polarizing film, and by drying, a polarizing film having a desired moisture content is obtained.
- the drying is performed by any appropriate method, and examples thereof include natural drying, blast drying, and heat drying.
- the drying temperature is preferably about 20 to 150 ° C, more preferably about 25 to 100 ° C.
- the drying time cannot be unconditionally determined because the drying degree of the polarizing film is affected by the drying temperature, but is preferably about 30 to 600 seconds, more preferably about 60 to 300 seconds. preferable.
- the drying step may be performed only once, or may be performed multiple times as necessary.
- the thickness of the polarizing film is preferably about 1 to 50 ⁇ m, more preferably about 1 to 25 ⁇ m.
- the following thin type using a laminate including a polyvinyl alcohol-based resin layer formed on a resin substrate such as a thermoplastic resin as the polyvinyl alcohol-based film The manufacturing method of the polarizing film can be applied.
- the method for producing a polarizing film (thin polarizing film) includes a step of forming a polyvinyl alcohol-based resin layer containing a polyvinyl alcohol-based resin on one side of a long thermoplastic resin substrate, and preparing a laminate, While transporting the obtained laminate in the longitudinal direction, an insolubilization treatment step, a crosslinking treatment step, and a washing treatment step are performed on the laminate, and at least an in-air auxiliary stretching treatment step, a dyeing treatment step, and an underwater stretching treatment step. It is obtained by applying.
- the polarizing film contains the hindered amine-based compound
- the treatment bath contains the hindered amine compound.
- the washing treatment step is a dyeing treatment step, and in consideration of the treatment conditions such as an underwater stretching treatment step, components such as a hindered amine compound and iodine are eluted from the polyvinyl alcohol film, Alternatively, it is easy to adjust the content of the hindered amine compound and the content of iodine to a desired range from the viewpoint that they can be adsorbed on a polyvinyl alcohol film.
- the concentration of the hindered amine compound contained in any one of the treatment baths cannot be unconditionally determined because it is affected by the number of treatments, the treatment time, the treatment temperature of each treatment, etc., but the content of the hindered amine compound in the polarizing film From the viewpoint of efficiently controlling the amount, it is generally preferably 0.01% by weight or more, more preferably 0.05% by weight or more, and further preferably 0.1% by weight or more, and , 30 wt% or less, preferably 25 wt% or less, more preferably 20 wt% or less.
- thermoplastic resin substrate is preferably about 20 to 300 ⁇ m, more preferably about 50 to 200 ⁇ m.
- the thickness of the PVA-based resin layer is preferably about 3 to 40 ⁇ m, more preferably about 3 to 20 ⁇ m.
- the thermoplastic resin base material preferably has a water absorption rate of about 0.2% or more, from the viewpoint of absorbing water to significantly reduce the stretching stress and allowing stretching to a high ratio, and 0.3. % Or more is more preferable.
- the thermoplastic resin base material has a water absorption of 3 from the viewpoint that the dimensional stability of the thermoplastic resin base material is remarkably reduced and the appearance of the obtained polarizing film is deteriorated. % Or less, more preferably about 1% or less.
- the water absorption can be adjusted, for example, by introducing a modifying group into the constituent material of the thermoplastic resin substrate.
- the water absorption rate is a value obtained according to JIS K7209.
- the thermoplastic resin base material has a glass transition temperature (Tg) of about 120 ° C. or lower from the viewpoint of being able to sufficiently secure the stretchability of the laminate while suppressing the crystallization of the PVA-based resin layer. Is preferred. Further, in consideration of the plasticization of the thermoplastic resin substrate with water and the favorable underwater drawing, the glass transition temperature (Tg) is more preferably about 100 ° C. or lower, and about 90 ° C. or lower. Is more preferable. On the other hand, the glass transition temperature of the thermoplastic resin substrate is such that when the coating liquid is applied and dried, problems such as deformation of the thermoplastic resin substrate can be prevented and a good laminate can be produced. Therefore, the temperature is preferably about 60 ° C. or higher. The glass transition temperature can be adjusted, for example, by introducing a modifying group into the constituent material of the thermoplastic resin substrate or by heating with a crystallization material. The glass transition temperature (Tg) is a value determined according to JIS K7121.
- thermoplastic resin can be adopted as the constituent material of the thermoplastic resin base material.
- the thermoplastic resin include ester resins such as polyethylene terephthalate resins, cycloolefin resins such as norbornene resins, olefin resins such as polypropylene, polyamide resins, polycarbonate resins, and copolymer resins thereof. Etc. Among these, norbornene-based resins and amorphous (amorphous) polyethylene terephthalate-based resins are preferable. Further, the thermoplastic resin base material has extremely excellent stretchability, and from the viewpoint that crystallization during stretching can be suppressed. Amorphous (non-crystalline) polyethylene terephthalate resin is preferably used.
- amorphous (amorphous) polyethylene terephthalate-based resin examples include a copolymer containing isophthalic acid and / or cyclohexanedicarboxylic acid as a dicarboxylic acid, and a copolymer containing cyclohexanedimethanol or diethylene glycol as a glycol.
- the thermoplastic resin substrate may be subjected to a surface treatment (for example, corona treatment) before forming the PVA-based resin layer, or an easy adhesion layer may be formed on the thermoplastic resin substrate. . By performing such a treatment, it is possible to improve the adhesion between the thermoplastic resin substrate and the PVA-based resin layer.
- the thermoplastic resin substrate may be stretched before forming the PVA-based resin layer.
- the above coating solution is a solution of PVA resin dissolved in a solvent.
- the solvent include water, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, N-methylpyrrolidone, various glycols, polyhydric alcohols such as trimethylolpropane, amines such as ethylenediamine and diethylenetriamine, and water. preferable. These can be used alone or in combination of two or more.
- the concentration of the PVA-based resin in the coating liquid is preferably about 3 to 20 parts by weight based on 100 parts by weight of the solvent, from the viewpoint of forming a uniform coating film in close contact with the thermoplastic resin substrate. ..
- the coating liquid contains a halide.
- Any appropriate halide can be adopted as the halide, and examples thereof include iodide and sodium chloride.
- the iodide include potassium iodide, sodium iodide, lithium iodide and the like, and potassium iodide is preferable.
- the concentration of the halide in the coating liquid is preferably about 5 to 20 parts by weight, more preferably about 10 to 15 parts by weight, based on 100 parts by weight of the PVA-based resin.
- additives may be added to the coating liquid.
- the additives include plasticizers such as ethylene glycol and glycerin; surfactants such as nonionic surfactants.
- any appropriate method can be adopted as a method for applying the coating solution, and examples thereof include a roll coating method, a spin coating method, a wire bar coating method, a dip coating method, a die coating method, a curtain coating method, and a spray coating method. , Knife coating method (comma coating method, etc.) and the like.
- the drying temperature of the coating liquid is preferably about 50 ° C or higher.
- the stretching method of the in-air auxiliary stretching treatment step may be fixed-end stretching (for example, a method of stretching using a tenter stretching machine) or free-end stretching (for example, uniaxial stretching through a laminate between rolls having different peripheral speeds). Method), but free end drawing is preferable from the viewpoint of obtaining high optical characteristics.
- the draw ratio in the above-mentioned in-air auxiliary drawing process is preferably about 2 to 3.5 times.
- the in-air auxiliary stretching treatment may be performed in one stage or in multiple stages. When performing in multiple stages, the draw ratio is the product of the draw ratios of the respective stages.
- the stretching temperature in the in-air auxiliary stretching treatment step can be set to any appropriate value depending on the forming material of the thermoplastic resin substrate, the stretching method, and the like.
- the glass transition temperature of the thermoplastic resin substrate It is preferably (Tg) or higher, more preferably the glass transition temperature (Tg) + 10 ° C. or higher, and further preferably the glass transition temperature (Tg) + 15 ° C. or higher.
- the upper limit of the stretching temperature is from the viewpoint that the crystallization of the PVA-based resin can be prevented from rapidly progressing and defects due to crystallization (for example, hindering the orientation of the PVA-based resin layer due to the stretching) can be suppressed. It is preferably about 170 ° C.
- an insolubilization treatment step may be performed after the in-air auxiliary stretching treatment step and before the dyeing treatment step or the underwater stretching treatment step.
- the insolubilization treatment step is typically performed by immersing the PVA-based resin layer in an aqueous boric acid solution. By performing the insolubilization treatment step, it is possible to impart water resistance to the PVA-based resin layer and prevent the orientation of PVA from being lowered when immersed in water.
- the concentration of the boric acid aqueous solution is preferably about 1 to 5 parts by weight with respect to 100 parts by weight of water.
- the liquid temperature of the insolubilization bath is preferably about 20 to 50 ° C.
- the dyeing treatment step is performed by dyeing the PVA-based resin layer with iodine.
- the adsorption method include a method of immersing the PVA-based resin layer (laminate) in a dyeing solution containing iodine, a method of applying the dyeing solution to the PVA-based resin layer, and a method of applying the dyeing solution to the PVA-based resin layer. Examples thereof include a method of spraying, and a method of immersing the PVA-based resin layer (laminate) in a dyeing solution containing iodine is preferable.
- the blending amount of iodine in the dyeing bath is preferably about 0.05 to 0.5 parts by weight with respect to 100 parts by weight of water.
- the iodide content is preferably about 0.1 to 10 parts by weight, and more preferably about 0.3 to 5 parts by weight, based on 100 parts by weight of water.
- the liquid temperature of the dyeing bath is preferably about 20 to 50 ° C. in order to suppress dissolution of the PVA-based resin.
- the immersion time is preferably about 5 seconds to 5 minutes, and more preferably about 30 seconds to 90 seconds, from the viewpoint of ensuring the transmittance of the PVA-based resin layer.
- the ratio of the iodine and iodide contents in the iodine aqueous solution is preferably about 1: 5 to 1:20, and about 1: 5 to 1:10. More preferably.
- a crosslinking treatment step may be performed after the dyeing treatment step and before the underwater stretching treatment step.
- the cross-linking treatment step is typically performed by immersing the PVA-based resin layer in an aqueous boric acid solution.
- the boric acid concentration of the aqueous boric acid solution is preferably about 1 to 5 parts by weight with respect to 100 parts by weight of water.
- the crosslinking bath further contains the iodide.
- the iodide content is preferably about 1 to 5 parts by weight with respect to 100 parts by weight of water.
- the liquid temperature of the crosslinking bath is preferably about 20 to 50 ° C.
- the underwater stretching treatment step is performed by immersing the laminate in a stretching bath. According to the underwater stretching treatment step, it is possible to stretch at a temperature lower than the glass transition temperature (typically about 80 ° C.) of the thermoplastic resin base material or the PVA type resin layer, and the PVA type resin layer is crystallized. It is possible to stretch at a high magnification while suppressing the above.
- the stretching method in the underwater stretching treatment step may be fixed-end stretching (for example, a stretching method using a tenter stretching machine) or free-end stretching (for example, a uniaxial stretching method in which a laminate is passed between rolls having different peripheral speeds). ) May be used, but free-end stretching is preferable from the viewpoint of obtaining high optical characteristics.
- the above-mentioned underwater stretching treatment step is preferably performed by immersing the laminate in a boric acid aqueous solution (boric acid underwater stretching).
- a boric acid aqueous solution boric acid underwater stretching
- the boric acid concentration of the boric acid aqueous solution is preferably 1 to 10 parts by weight, and more preferably 2.5 to 6 parts by weight with respect to 100 parts by weight of water.
- the liquid temperature of the stretching bath is preferably about 40 to 85 ° C, more preferably about 60 to 75 ° C.
- the immersion time of the laminate in the stretching bath is preferably about 15 seconds to 5 minutes.
- the draw ratio in the underwater stretching process is preferably about 1.5 times or more, more preferably about 3 times or more.
- the total draw ratio of the laminate is preferably about 5 times or more, more preferably about 5.5 times or more of the original length of the laminate.
- the cleaning treatment step is typically performed by immersing the PVA-based resin layer in an aqueous potassium iodide solution.
- each treatment bath in the dyeing treatment step, the underwater stretching treatment step, the insolubilization treatment step, the cross-linking treatment step, and the washing treatment step contains zinc salt, a pH adjusting agent, a pH buffering agent, and other salts. It may contain various additives.
- the zinc salt include zinc halides such as zinc chloride and zinc iodide; inorganic zinc salts such as zinc sulfate and zinc acetate.
- the pH adjuster include strong acids such as hydrochloric acid, sulfuric acid and nitric acid, and strong bases such as sodium hydroxide and potassium hydroxide.
- Examples of the pH buffer include carboxylic acids such as acetic acid, oxalic acid and citric acid and salts thereof, and weak inorganic acids such as phosphoric acid and carbonic acid and salts thereof.
- Examples of the other salts include chlorides such as sodium chloride, potassium chloride and barium chloride, nitrates such as sodium nitrate and potassium nitrate, sulfates such as sodium sulfate and potassium sulfate, and alkali metals and alkaline earth metals. Salt etc. are mentioned.
- ⁇ Adhesive layer> As the pressure-sensitive adhesive forming the pressure-sensitive adhesive layer of the present invention, various pressure-sensitive adhesives used in polarizing films can be applied, and examples thereof include a rubber-based pressure-sensitive adhesive, an acrylic pressure-sensitive adhesive, a silicone-based pressure-sensitive adhesive, and a urethane-based pressure-sensitive adhesive. , Vinyl alkyl ether-based adhesives, polyvinyl alcohol-based adhesives, polyvinyl porolidone-based adhesives, polyacrylamide-based adhesives, and cellulose-based adhesives. Among these, acrylic adhesives are suitable.
- the acrylic pressure-sensitive adhesive contains an acrylic polymer as a base polymer, and examples thereof include the acrylic pressure-sensitive adhesives described in JP-A-2017-75998.
- the acrylic polymer in the acrylic pressure-sensitive adhesive has a monomer unit of (meth) acrylic acid alkyl ester as a main skeleton.
- a (meth) acrylic acid alkyl ester having an alkyl group having 1 to 20 carbon atoms is preferably used, and the content of the (meth) acrylic acid alkyl ester is the same as that of the base polymer. It is preferably 40% by weight or more, more preferably 60% by weight or more, based on the total amount of the constituent monomer components.
- it may contain a monomer unit such as a nitrogen-containing monomer unit or a hydroxy group-containing monomer.
- a crosslinking agent may be used, and examples of the crosslinking agent include an isocyanate crosslinking agent, an epoxy crosslinking agent, an oxazoline crosslinking agent, an aziridine crosslinking agent, and a carbodiimide crosslinking agent. Commonly used crosslinking agents, metal chelate crosslinking agents, etc. can be used.
- the amount of the crosslinking agent used is usually 10 parts by weight or less, preferably 5 parts by weight or less, based on 100 parts by weight of the base polymer.
- the adhesive includes silane coupling agents; terpene-based tackifiers, styrene-based tackifiers, phenol-based tackifiers, rosin-based tackifiers, epoxy-based tackifiers, etc.
- a tackifier may be added.
- an ultraviolet absorber may be added.
- the pressure-sensitive adhesive may include additives such as a plasticizer, a softening agent, a deterioration inhibitor, a filler, a colorant, an antioxidant, a surfactant, and an antistatic agent. Can be used within a range that does not impair
- a method of forming the pressure-sensitive adhesive layer for example, a method of applying the pressure-sensitive adhesive to a release-treated separator or the like, forming a pressure-sensitive adhesive layer by drying, and then transferring to a polarizing film, or the pressure-sensitive adhesive is polarized. Examples thereof include a method of forming a pressure-sensitive adhesive layer by applying it on a film or the like and drying it.
- the thickness of the pressure-sensitive adhesive layer is not particularly limited and is, for example, about 1 to 100 ⁇ m, preferably about 2 to 50 ⁇ m.
- Adhesive layer As the adhesive forming the adhesive layer of the present invention, various adhesives used in polarizing films can be applied, and examples thereof include isocyanate adhesives, polyvinyl alcohol adhesives, gelatin adhesives, vinyl latex. Examples thereof include water-based polyester and water-based polyester. These adhesives are usually used as an adhesive composed of an aqueous solution (water-based adhesive) and contain a solid content of 0.5 to 60% by weight. Among these, polyvinyl alcohol adhesives are preferable, and acetoacetyl group-containing polyvinyl alcohol adhesives are more preferable.
- the water-based adhesive may contain a crosslinking agent.
- a crosslinking agent a compound having at least two functional groups reactive with a component such as a polymer constituting an adhesive in one molecule is usually used, and examples thereof include alkylenediamines; isocyanates; epoxies; Aldehydes; amino-formaldehyde and the like such as methylol urea and methylol melamine.
- the compounding amount of the crosslinking agent in the adhesive is usually about 10 to 60 parts by weight with respect to 100 parts by weight of the components such as the polymer constituting the adhesive.
- examples of the adhesive include active energy ray curable adhesives such as ultraviolet curable adhesives and electron beam curable adhesives.
- active energy ray-curable adhesive include (meth) acrylate adhesives.
- examples of the curable component in the (meth) acrylate-based adhesive include compounds having a (meth) acryloyl group and compounds having a vinyl group.
- examples of the compound having a (meth) acryloyl group include alkyl (meth) acrylates such as a chain alkyl (meth) acrylate having 1 to 20 carbon atoms, an alicyclic alkyl (meth) acrylate, and a polycyclic alkyl (meth) acrylate.
- (Meth) acrylate adhesives include hydroxyethyl (meth) acrylamide, N-methylol (meth) acrylamide, N-methoxymethyl (meth) acrylamide, N-ethoxymethyl (meth) acrylamide, (meth) acrylamide, (meth) It may contain a nitrogen-containing monomer such as acryloylmorpholine.
- the (meth) acrylate-based adhesive includes tripropylene glycol diacrylate, 1,9-nonanediol diacrylate, tricyclodecane dimethanol diacrylate, cyclic trimethylolpropane formal acrylate, dioxane glycol diacrylate, and EO as cross-linking components. It may contain a polyfunctional monomer such as modified diglycerin tetraacrylate. Further, a compound having an epoxy group or an oxetanyl group can also be used as the cationic polymerization curable adhesive.
- the compound having an epoxy group is not particularly limited as long as it has at least two epoxy groups in the molecule, and various commonly known curable epoxy compounds can be used.
- the adhesive may contain an appropriate additive as needed.
- the additives include silane coupling agents, coupling agents such as titanium coupling agents, adhesion promoters such as ethylene oxide, ultraviolet absorbers, deterioration inhibitors, dyes, processing aids, ion trap agents, and antioxidants.
- the application of the adhesive may be performed on either the transparent protective film side (or the functional layer side described later) described later, the polarizing film side, or both.
- a drying process is performed to form an adhesive layer composed of a coating and drying layer.
- ultraviolet rays or an electron beam can be irradiated if necessary.
- the thickness of the adhesive layer is not particularly limited, and when an aqueous adhesive or the like is used, it is preferably about 30 to 5000 nm, more preferably about 100 to 1000 nm, and an ultraviolet curable adhesive. When using an electron beam curable adhesive or the like, the thickness is preferably about 0.1 to 100 ⁇ m, more preferably about 0.5 to 10 ⁇ m.
- the content of the hindered amine-based compound is a pressure-sensitive adhesive from the viewpoint of suppressing a decrease in single transmittance due to coloring of the polarizing film under a high temperature environment.
- the layer or the adhesive layer it is preferably 1% by weight or more, more preferably 5% by weight or more, further preferably 10% by weight or more, and preferably 70% by weight or less. More preferably 50% by weight or less.
- the single-sided protective polarizing film of the present invention has a transparent protective film attached to at least one surface of the polarizing film via the pressure-sensitive adhesive layer or the adhesive layer.
- a transparent protective film is attached to both sides of the polarizing film via the pressure-sensitive adhesive layer or the adhesive layer.
- the transparent protective film is not particularly limited, and various transparent protective films used for polarizing films can be used.
- a material forming the transparent protective film for example, a thermoplastic resin having excellent transparency, mechanical strength, thermal stability, moisture barrier property, isotropic property, etc. is used.
- the thermoplastic resin include cellulose ester resins such as triacetyl cellulose, polyester resins such as polyethylene terephthalate and polyethylene naphthalate, polyether sulfone resins, polysulfone resins, polycarbonate resins, nylon and aroma.
- Polyamide resins such as group polyamides, polyimide resins, polyolefin resins such as polyethylene, polypropylene and ethylene-propylene copolymers, (meth) acrylic resins, cyclo polyolefin resins having a norbornene structure (norbornene resins) ), Polyarylate-based resins, polystyrene-based resins, polyvinyl alcohol-based resins, and mixtures thereof.
- the transparent protective film may use a cured layer formed of a thermosetting resin such as a (meth) acrylic resin, a urethane resin, an acryl urethane resin, an epoxy resin, a silicone resin or an ultraviolet curable resin.
- a cellulose ester resin, a polycarbonate resin, a (meth) acrylic resin, a cyclic polyolefin resin, and a polyester resin are preferable.
- the thickness of the transparent protective film can be appropriately determined, but generally, from the viewpoint of workability such as strength and handleability, thin layer property, etc., it is preferably about 1 to 500 ⁇ m, and about 1 to 300 ⁇ m. More preferably, it is more preferably about 5 to 100 ⁇ m.
- the hindered amine-based compound moves (stays) inside the image display device together with the water present inside the image display device (water present in the pressure-sensitive adhesive layer or the adhesive layer) to form a polarizing film.
- the water vapor transmission rate is preferably 50 g / (m 2 ⁇ 24 h or more, more preferably 100 g / (m 2 ⁇ 24 h) or more, and 200 g / (m 2 ⁇ 24 h) or more.
- the water vapor transmission rate is in accordance with the water vapor transmission rate test (cup method) of JIS Z0208, and a sample cut into a diameter of 60 mm is set in a water vapor transmission cup containing about 15 g of calcium chloride, and the temperature is 40 ° C. It can be calculated by measuring the increase in weight of calcium chloride before and after leaving it in a thermostat having a humidity of 90% RH for 24 hours.
- the transparent protective films on both sides may be the same or different.
- a retardation plate having a front surface retardation of 40 nm or more and / or a thickness direction retardation of 80 nm or more can be used.
- the front retardation is usually controlled in the range of 40 to 200 nm
- the thickness direction retardation is usually controlled in the range of 80 to 300 nm.
- the retardation plate also functions 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.
- the phase plate may be attached to a transparent protective film having no retardation.
- the transparent protective film contains any appropriate additive such as an ultraviolet absorber, an antioxidant, a lubricant, a plasticizer, a release agent, an anti-coloring agent, a flame retardant, an antistatic agent, a pigment and a colorant. You may stay. In particular, when the transparent protective film contains an ultraviolet absorber, the light resistance of the polarizing film can be improved.
- a functional layer such as a hard coat layer, an antireflection layer, a sticking prevention layer, a diffusion layer or an antiglare layer can be provided on the surface of the transparent protective film on which the polarizing film is not attached.
- the hard coat layer, the antireflection layer, the antisticking layer, the functional layer such as the diffusion layer and the antiglare layer may be provided on the protective film itself, or may be provided separately from the protective film. it can.
- the polarizing film and the transparent protective film, or the polarizing film and the functional layer are usually attached via the pressure-sensitive adhesive layer or the adhesive layer.
- the transparent protective film and the polarizing film, or the polarizing film and the functional layer may be laminated via an intervening layer such as a surface modification treatment layer, an easy-adhesive layer, a block layer, and a refractive index adjusting layer. ..
- Examples of the surface modification treatment for forming the surface modification layer include corona treatment, plasma treatment, primer treatment, saponification treatment and the like.
- Examples of the easy-adhesive agent for forming the easy-adhesion layer include a forming material containing various resins having a polyester skeleton, a polyether skeleton, a polycarbonate skeleton, a polyurethane skeleton, a silicone-based, a polyamide skeleton, a polyimide skeleton, a polyvinyl alcohol skeleton, or the like. Can be mentioned.
- the easy-adhesion layer is usually provided in advance on the protective film, and the easy-adhesion layer side of the protective film and the polarizing film are laminated with the pressure-sensitive adhesive layer or the adhesive layer.
- the blocking layer is a layer that has a function of preventing impurities (such as oligomers and ions) eluted from the transparent protective film and the like from moving (entering) into the polarizing film.
- the block layer may be any layer as long as it has transparency and can prevent impurities eluted from the transparent protective film and the like, and examples of the material for forming the block layer include urethane prepolymer-based forming material and cyanoacrylate. Examples include a system forming material and an epoxy forming material.
- the refractive index adjusting layer is a layer provided for suppressing a decrease in transmittance due to reflection between the transparent protective film and a layer such as a polarizing film having a different refractive index.
- the refractive index adjusting material for forming the refractive index adjusting layer include various resins having a silica type, an acrylic type, an acryl-styrene type, a melamine type, etc., and a forming agent containing an additive.
- the polarizing film of the present invention has a general formula (1): X (% by weight)> 0.01 (in the general formula (1), from the viewpoint of suppressing a decrease in simple substance transmittance due to coloring of the polarizing film in a high temperature environment, X is a laminated body in which a glass plate is bonded to both surfaces of a polarizing film having the transparent protective film bonded to at least one surface of the polarizing film via the adhesive layer at 105 ° C. , Shows the content of the hindered amine-based compound in the polarizing film in the laminate left for 24 hours.).
- the X (% by weight) is preferably 0.02 or more, and more preferably 0.05 or more.
- the laminated polarizing film (optical laminate) of the present invention has an optical layer bonded to at least one surface of the single-sided protective polarizing film or the double-sided protective polarizing film via the pressure-sensitive adhesive layer or the adhesive layer. There is something.
- the optical layer is not particularly limited, but for example, for forming a liquid crystal display device such as a reflection plate, a semi-transmission plate, a retardation plate (including a wave plate such as 1/2 or 1/4), and a viewing angle compensation film.
- a liquid crystal display device such as a reflection plate, a semi-transmission plate, a retardation plate (including a wave plate such as 1/2 or 1/4), and a viewing angle compensation film.
- One or two or more optical layers that may be used can be used.
- the laminated polarizing film in particular, a reflective polarizing film or a semi-transmissive polarizing film obtained by further laminating a reflecting plate or a semi-transmissive reflecting plate on the polarizing film, and further comprising a retardation plate laminated on the polarizing film.
- Examples thereof include an elliptically polarizing film or a circularly polarizing film, a wide viewing angle polarizing film obtained by further laminating a viewing angle compensation film on the polarizing film, or a polarizing film obtained by further laminating a brightness improving film on the polarizing film.
- One side or both sides of the single-sided protective polarizing film, the double-sided protective polarizing film, or the laminated polarizing film has an image display cell such as a liquid crystal cell or an organic EL element, and a front transparent plate or a touch panel on the viewing side.
- the pressure-sensitive adhesive layer or the adhesive layer may be attached in advance in order to bond other members such as the front transparent member.
- the polarizing film or the laminated polarizing film having a pressure-sensitive adhesive layer provided on at least one surface thereof has a pressure-sensitive adhesive layer-attached single-sided protective polarizing film, a pressure-sensitive adhesive layer-attached double-sided protective polarizing film, or a pressure-sensitive adhesive layer.
- the exposed surface of the pressure-sensitive adhesive layer or the adhesive layer is temporarily covered with a separator for the purpose of preventing contamination, etc. until it is put into practical use.
- a separator for example, a plastic film, a rubber sheet, a paper, a cloth, a non-woven fabric, a net, a foam sheet or a metal foil, an appropriate thin sheet such as a laminate thereof, a silicone-based or long-chain alkyl-based, if necessary, Those coated with an appropriate release agent such as fluorine-based or molybdenum sulfide are used.
- the front transparent member of the present invention is a front transparent member arranged on the visible side of the image display cell.
- the front transparent member include a front transparent plate (window layer) and a touch panel.
- a front transparent plate a front transparent plate having appropriate mechanical strength and thickness is used.
- a transparent plate for example, a transparent resin plate such as an acrylic resin or a polycarbonate resin, or a glass plate is used.
- the touch panel for example, various touch panels such as a resistance film type, a capacitance type, an optical type, an ultrasonic type, and a glass plate or a transparent resin plate having a touch sensor function are used.
- a capacitive touch panel is used as the front transparent member, it is preferable that a front transparent plate made of glass or a transparent resin plate is provided on the side closer to the viewer than the touch panel.
- Examples of the image display cell of the present invention include a liquid crystal cell and an organic EL cell.
- Examples of the liquid crystal cell include a reflective liquid crystal cell that uses external light, a transmissive liquid crystal cell that uses light from a light source such as a backlight, and a semi-transmissive liquid crystal cell that uses both external light and light from a light source. Any of the semi-reflective liquid crystal cells may be used.
- the image display device liquid crystal display device
- the image display device has a polarizing film arranged on the side opposite to the viewing side of the image display cell (liquid crystal cell). Will be placed.
- the polarizing film on the light source side and the liquid crystal cell are bonded together via an appropriate adhesive layer.
- a driving method of the liquid crystal cell for example, any type such as a VA mode, an IPS mode, a TN mode, an STN mode, a bend alignment ( ⁇ type), or the like can be used.
- organic EL cell for example, one in which a transparent electrode, an organic light emitting layer, and a metal electrode are laminated in this order on a transparent substrate to form a light emitting body (organic electroluminescent light emitting body) is preferably used.
- 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 or the like and a light emitting layer made of a fluorescent organic solid such as anthracene, or the like.
- Various layer configurations such as a laminated body of the above-mentioned light emitting layer and an electron injection layer composed of a perylene derivative or a laminated body of a hole injection layer, a light emitting layer, and an electron injection layer can be adopted.
- ⁇ Example 1> ⁇ Production of polarizing film> A polyvinyl alcohol film having an average degree of polymerization of 2,400, a degree of saponification of 99.9 mol% and a thickness of 45 ⁇ m was prepared. The polyvinyl alcohol film was dipped in a swelling bath (water bath) at 20 ° C. for 30 seconds between rolls having different peripheral speed ratios and stretched to 2.2 times in the transport direction while swelling (swelling step). The iodine concentration of the polarizing film finally obtained in a dyeing bath at 30 ° C.
- a swelling bath water bath
- an iodine aqueous solution obtained by mixing iodine and potassium iodide in a weight ratio of 1: 7 to 100 parts by weight of water is 4 It is soaked for 30 seconds while adjusting the concentration to be 0.47% by weight, and dyed 3.3 times in the transport direction based on the original polyvinyl alcohol film (polyvinyl alcohol film that has not been stretched in the transport direction) while dyeing. Was stretched (dyeing step). Then, the dyed polyvinyl alcohol film is immersed in a crosslinking bath at 40 ° C.
- the hindered amine compound represented by the following general formula (6) is a compound that dissolves in 1 part by weight or more in 100 parts by weight of water at 25 ° C.
- iodine concentration (% by weight) was determined using the following formula using a fluorescent X-ray analyzer (Rigaku Corporation, trade name “ZSX-PRIMUS IV”, measurement diameter: ⁇ 20 mm).
- Iodine concentration (wt%) 14.474 x (fluorescent X-ray intensity) / (film thickness) (kcps / ⁇ m)
- the coefficient for calculating the concentration differs depending on the measuring device, the coefficient is an appropriate calibration curve. Can be obtained using.
- ⁇ Production of polarizing film> polyvinyl alcohol resin containing acetoacetyl group (average polymerization degree: 1,200, saponification degree: 98.5 mol%, acetoacetylation degree: 5 mol%) and methylolmelamine in a weight ratio of 3: The aqueous solution contained in 1 was used.
- a triacetyl cellulose film having a hard coat layer and a thickness of 47 ⁇ m moisture permeability 342 g / (m 2 ⁇ 24 h)
- Konica Minolta (Product name: "KC4UYW”) is pasted with a roll laminating machine, and then dried by heating in an oven (temperature is 60 ° C, time is 4 minutes), and transparent protective films are pasted on both sides of the polarizing film.
- the obtained polarizing film was produced.
- the single transmittance of the polarizing film was 37.4%.
- the pressure-sensitive adhesive layer was applied so as to have a thickness of 20 ⁇ m and dried at 90 ° C. for 1 minute to form a pressure-sensitive adhesive layer on the surface of the separator film.
- the pressure-sensitive adhesive layer formed on the separator film was transferred onto one surface of the polarizing film prepared above to prepare a polarizing film with a pressure-sensitive adhesive layer.
- the pseudo image display device (laminated body) obtained above was allowed to stand in a hot air oven at a temperature of 105 ° C. for 48 hours, and the single-body transmittance ( ⁇ Ts) before and after charging (heating) was measured.
- the simple substance transmittance was measured using a spectrophotometer (Murakami Color Research Laboratory Co., Ltd., product name "DOT-3"), and evaluated according to the following criteria.
- the single-piece transmittance is a Y value which has been subjected to luminosity correction by a 2 degree visual field (C light source) of JLS Z 8701-1982.
- the measurement wavelength is 380 to 700 nm (every 10 nm).
- Ts (%) Ts 48 ⁇ Ts 0
- Ts 0 the single transmittance of the pseudo image display device (laminate) before heating
- Ts 48 the single transmittance of the pseudo image display device (laminate) after heating for 48 hours.
- the ⁇ Ts (%) is preferably 5 ⁇ ⁇ Ts (%) ⁇ 0, more preferably 4 ⁇ ⁇ Ts (%) ⁇ 0.
- the pseudo image display device (laminate) obtained above is allowed to stand in a hot-air oven at a temperature of 105 ° C. for 24 hours, and the content of the hindered amine-based compound contained in the polarizing film after charging (heating) is as follows. It asked by the method.
- the heated pseudo image display device was immersed in about 1000 mL of a solution of methylene chloride or toluene for 3 days or more, and the protective film was dissolved to take out the polarizing film. As a result, the polarizing film was about 40 mg.
- ⁇ Example 2> ⁇ Production of polarizing film, optical film, pseudo image display device (laminate)>
- the hindered amine-based compound represented by the general formula (6) is used for both adhesives used in the production of the polarizing film without adding the hindered amine-based compound represented by the general formula (6) to the cleaning bath.
- a polarizing film, a polarizing film, and a pseudo image display device (laminate) were produced in the same manner as in Example 1 except that the compound was added so that the weight ratio with the polyvinyl alcohol resin was 4: 3. did.
- the single transmittance of the polarizing film was 39.7%.
- ⁇ Example 3> ⁇ Production of polarizing film, polarizing film, pseudo image display device (laminate)>
- the hindered amine-based compound represented by the general formula (7) is used for both adhesives used in the production of the polarizing film without adding the hindered amine-based compound represented by the general formula (6) to the cleaning bath.
- the compound is added to the polyvinyl alcohol resin in a weight ratio of 4: 3, and water is added to the hindered amine compound in a molar ratio of 1: 1 so as not to affect the curing reaction of the adhesive.
- a polarizing film, a polarizing film, and a pseudo image display device (laminate) were produced in the same manner as in Example 1 except that pH was adjusted (neutralized) by adding potassium oxide.
- the single transmittance of the polarizing film was 40.0%.
- the hindered amine compound represented by the following general formula (7) is a compound that dissolves in 1 part by weight or more in 100 parts by weight of water at 25 ° C.
- ⁇ Example 4> ⁇ Production of polarizing film, polarizing film, pseudo image display device (laminate)>
- the hindered amine-based compound represented by the general formula (8) is used for both adhesives used in the production of the polarizing film without adding the hindered amine-based compound represented by the general formula (6) to the cleaning bath.
- the compound is added to the polyvinyl alcohol resin in a weight ratio of 4: 3, and hydrochloric acid is added to the hindered amine compound in a molar ratio of 1: 1 so as not to affect the curing reaction of the adhesive.
- the hindered amine compound represented by the following general formula (8) is a compound that dissolves in 1 part by weight or more in 100 parts by weight of water at 25 ° C.
- ⁇ Example 5> ⁇ Production of polarizing film, polarizing film, pseudo image display device (laminate)> A polyvinyl alcohol resin containing an acetoacetyl group as both adhesives used in the production of the polarizing film without adding the hindered amine compound represented by the general formula (6) to the washing bath in the production of the polarizing film. And a methylolmelamine and a hindered amine compound represented by the general formula (6) in a weight ratio of 7: 2: 1, except that an aqueous solution was used, the same operation as in Example 1, a polarizing film, a polarizing film , And a pseudo image display device (laminate). The single transmittance of the polarizing film was 39.7%.
- ⁇ Example 6> ⁇ Production of polarizing film, polarizing film, pseudo image display device (laminate)>
- 40 parts by weight of N-hydroxyethylacrylamide (HEAA), 60 parts by weight of acryloylmorpholine (ACMO) and 3 parts by weight of a photoinitiator “IRGACURE 819” are used as both adhesives used in the production of the polarizing film.
- HEAA N-hydroxyethylacrylamide
- ACMO acryloylmorpholine
- IRGACURE 819 manufactured by BASF
- a polarizing film, a polarizing film, and a pseudo image display device were produced by the same operation as in Example 1 except that the above was produced.
- Ultraviolet irradiation is performed using a gallium-encapsulated metal halide lamp, irradiation device: Fusion UV Systems, Inc.
- thermoplastic resin base material an amorphous isophthalic copolymer polyethylene terephthalate film (thickness: 100 ⁇ m) having a long shape, a water absorption rate of 0.75% and a Tg of about 75 ° C. was used. Corona treatment was applied to one surface of the resin substrate.
- Polyvinyl alcohol (polymerization degree: 4200, saponification degree: 99.2 mol%) and acetoacetyl-modified PVA (manufactured by Nippon Synthetic Chemical Industry Co., Ltd., trade name "Gosephimmer Z410") in a ratio of 9: 1 100 weight of PVA-based resin
- 13 parts by weight of potassium iodide was added to prepare a PVA aqueous solution (coating solution).
- the PVA aqueous solution was applied to the corona-treated surface of the resin substrate and dried at 60 ° C. to form a PVA-based resin layer having a thickness of 13 ⁇ m, and a laminate was prepared.
- the obtained laminate was uniaxially stretched 2.4 times in the longitudinal direction (longitudinal direction) between rolls having different peripheral speeds in an oven at 130 ° C. (in-air auxiliary stretching treatment).
- the laminate was immersed in an insolubilizing bath (solution of boric acid having a concentration of 4.0% by weight) having a liquid temperature of 40 ° C. for 30 seconds (insolubilizing treatment).
- a dyeing bath having a liquid temperature of 30 ° C. (an iodine aqueous solution obtained by mixing iodine and potassium iodide in a weight ratio of 1: 7 with respect to 100 parts by weight of water) was added to the finally obtained polarizing film.
- the laminate was immersed in a cleaning bath (potassium iodide concentration 3% by weight) at a liquid temperature of 30 ° C. (cleaning treatment). Then, while being dried in an oven kept at 90 ° C., it was brought into contact with a SUS heating roll whose surface temperature was kept at 75 ° C. for about 2 seconds (dry shrinkage treatment). In this way, a polarizing film having a thickness of 5 ⁇ m was formed on the resin substrate.
- a cleaning bath potential iodide concentration 3% by weight
- a polyvinyl alcohol resin containing an acetoacetyl group (average polymerization degree: 1,200, saponification degree: 98.5 mol%, acetoacetylation degree: 5 mol%) and methylolmelamine were used in a weight ratio.
- An aqueous solution containing 3: 1 was used.
- a transparent protective film (thickness: 30 ⁇ m) made of a (meth) acrylic resin (modified acrylic polymer having a lactone ring structure) is formed on the surface of the polarizing film obtained above, which is opposite to the resin substrate.
- a film (manufactured by Nippon Shokubai Co., Ltd., moisture permeability of 125 g / (m 2 ⁇ 24 h)) was bonded using a roll bonding machine. Then, the resin substrate was peeled off, and the acrylic pressure-sensitive adhesive layer containing the hindered amine compound was transferred to the peeled surface to prepare a polarizing film with a pressure-sensitive adhesive layer.
- the acrylic pressure-sensitive adhesive containing the hindered amine compound is 20 parts by weight of the general formula (6) as a hindered amine compound, 80% by weight of the solid content of the solution of the acrylic polymer, an isocyanate cross-linking agent (manufactured by Tosoh Corporation, a product Name "Takenate D110N", trimethylol propane / xylylene diisocyanate adduct 0.02 parts by weight, silane coupling agent (Shin-Etsu Chemical Co., Ltd., trade name "X-41-1056”) 0.2 parts by weight It was made.
- an isocyanate cross-linking agent manufactured by Tosoh Corporation, a product Name "Takenate D110N", trimethylol propane / xylylene diisocyanate adduct 0.02 parts by weight
- silane coupling agent Shin-Etsu Chemical Co., Ltd., trade name "X-41-1056
- the acrylic acid monomer-free adhesive described in Example 1 was attached to the transparent protective film surface of the polarizing film with an adhesive layer, and glass plates were attached via the adhesive layers on both sides to obtain a pseudo image display device. (Laminate) was prepared.
- ⁇ Comparative Example 1> ⁇ Production of polarizing film, polarizing film, pseudo image display device (laminate)>
- the polarizing film, the polarizing film, and the pseudo image display device were operated in the same manner as in Example 1 except that the hindered amine compound represented by the general formula (6) was not added to the washing bath.
- (Laminate) was prepared.
- the obtained polarizing film had a hindered amine content of 0% by weight and a thickness of 18 ⁇ m.
- the single transmittance of the polarizing film was 39.6%.
- ⁇ Comparative example 3> ⁇ Production of polarizing film, polarizing film, pseudo image display device (laminate)>
- the hindered amine compound represented by the general formula (6) was not added to the washing bath, and 35 parts by weight of N-hydroxyethylacrylamide (HEAA) and acryloylmorpholine (ACMO) were used as the adhesive.
- 50 parts by weight, 5 parts by weight of a photoinitiator "IRGACURE 819" (manufactured by BASF) and 10 parts by weight of a compound represented by the general formula (9) (trade name "ADEKA STAB LA-52", manufactured by ADEKA) are mixed.
- the polarizing film was prepared by coating the polarizing film so that the cured adhesive layer had a thickness of 1.0 ⁇ m, irradiating ultraviolet rays as active energy rays, and curing the adhesive.
- a polarizing film, a polarizing film, and a pseudo image display device (laminate) were produced.
- Ultraviolet irradiation is performed using a gallium-encapsulated metal halide lamp, irradiation device: Fusion UV Systems, Inc.
- the hindered amine compound represented by the following general formula (9) is a compound that does not dissolve in 1 part by weight or more in 100 parts by weight of water at 25 ° C.
- Polarizing film 11 Polarizing film 12 and 13: Transparent protective film 20, 30, 40, and 50: Adhesive layer or adhesive layer 80: Front transparent member 90: Image display cell 100: Image display device 101: One side Protective polarizing film 102: Double-sided protective polarizing film
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Abstract
Description
本発明のヒンダードアミン系化合物とは、アミノ基に隣接する炭素にアルキル基が置換されてアミノ基を立体的に保護している二級アミンまたは三級アミンであり、例えば、以下の構造の有機基を有する化合物等が挙げられる。なお、例示する化合物には、25℃の水100重量部に対して1重量部以上溶解できない構造が含まれる可能性があるが、当業者であれば、技術常識を考慮して、例示する化合物が、25℃の水100重量部に対して1重量部以上溶解できるかは、直ちに確認できる。
本発明の偏光フィルムは、ポリビニルアルコール系フィルムにヨウ素が吸着配向して形成される偏光膜を有する。
前記偏光膜の製造方法は、前記ポリビニルアルコール系フィルムに、任意の膨潤工程および洗浄工程と、少なくとも、染色工程、架橋工程、および延伸工程を施して得られる。前記偏光膜が、前記ヒンダードアミン系化合物を含有する場合、前記膨潤工程、前記洗浄工程、前記染色工程、前記架橋工程、および前記延伸工程のいずれか1つ以上の処理工程における処理浴が、前記ヒンダードアミン系化合物を含んでいればよい。前記偏光膜中に含まれる前記ヒンダードアミン系化合物の含有量および前記ヨウ素の含有量は、膨潤工程、染色工程、架橋工程、延伸工程および洗浄工程における各処理浴のいずれかに含まれる前記ヒンダードアミン系化合物の濃度、およびヨウ素ならびにヨウ化カリウム等の濃度、上記の各処理浴による処理温度および処理時間によって制御できる。とくに、染色工程、架橋工程、および延伸工程を施した後に、洗浄工程を施す場合、洗浄工程は、染色工程、架橋工程、および延伸工程等での処理条件を考慮したうえで、ヒンダードアミン系化合物やヨウ素等の成分をポリビニルアルコール系フィルムから溶出、あるいはポリビニルアルコール系フィルムに吸着させることができる観点から、前記ヒンダードアミン系化合物の含有量および前記ヨウ素の含有量を所望の範囲に調整し易い。
偏光膜(薄型の偏光膜)の製造方法は、長尺状の熱可塑性樹脂基材の片側に、ポリビニルアルコール系樹脂を含むポリビニルアルコール系樹脂層を形成して積層体を準備する工程と、得られた積層体を長手方向に搬送しながら、前記積層体に、任意の不溶化処理工程、架橋処理工程、および洗浄処理工程と、少なくとも、空中補助延伸処理工程、染色処理工程、および水中延伸処理工程を施して得られる。前記偏光膜が、前記ヒンダードアミン系化合物を含有する場合、前記不溶化処理工程、前記架橋処理工程、前記洗浄処理工程、前記染色処理工程、および前記水中延伸処理工程のいずれか1つ以上の処理工程における処理浴が、前記ヒンダードアミン系化合物を含んでいればよい。前記偏光膜中に含まれる前記ヒンダードアミン系化合物の含有量および前記ヨウ素の含有量は、前記不溶化処理工程、前記架橋処理工程、前記洗浄処理工程、前記染色処理工程、および前記水中延伸処理工程における各処理浴のいずれかに含まれる前記ヒンダードアミン系化合物の濃度、およびヨウ素ならびにヨウ化カリウム等の濃度、上記の各処理浴による処理温度および処理時間によって制御できる。とくに、洗浄処理工程を施す場合、洗浄処理工程は、染色処理工程、および水中延伸処理工程等での処理条件を考慮したうえで、ヒンダードアミン系化合物やヨウ素等の成分をポリビニルアルコール系フィルムから溶出、あるいはポリビニルアルコール系フィルムに吸着させることができる観点から、前記ヒンダードアミン系化合物の含有量および前記ヨウ素の含有量を所望の範囲に調整し易い。
前記積層体を作製する方法としては、任意の適切な方法が採用され、例えば、前記熱可塑性樹脂基材の表面に、前記ポリビニルアルコール系樹脂(PVA系樹脂)を含む塗布液を塗布し、乾燥することに方法が挙げられる。前記熱可塑性樹脂基材の厚みは、20~300μm程度であることが好ましく、50~200μm程度であることがより好ましい。前記PVA系樹脂層の厚みは、3~40μm程度であることが好ましく、3~20μm程度であることがより好ましい。
前記空中補助延伸処理工程は、熱可塑性樹脂基材の結晶化を抑制しながら延伸することができるため、積層体を高倍率に延伸することができる。前記空中補助延伸処理工程の延伸方法は、固定端延伸(例えば、テンター延伸機を用いて延伸する方法)でもよいし、自由端延伸(例えば、周速の異なるロール間に積層体を通して一軸延伸する方法)でもよいが、高い光学特性を得る観点から、自由端延伸が好ましい。
必要に応じて、前記空中補助延伸処理工程の後、染色処理工程や水中延伸処理工程の前に、不溶化処理工程を施してもよい。前記不溶化処理工程は、代表的には、ホウ酸水溶液にPVA系樹脂層を浸漬することにより行う。不溶化処理工程を施すことにより、PVA系樹脂層に耐水性を付与し、水に浸漬した時のPVAの配向低下を防止することができる。当該ホウ酸水溶液の濃度は、水100重量部に対して、1~5重量部程度であることが好ましい。不溶化処理浴の液温は、20~50℃程度であることが好ましい。
前記染色処理工程は、PVA系樹脂層をヨウ素で染色することにより行う。当該吸着方法としては、例えば、ヨウ素を含む染色液にPVA系樹脂層(積層体)を浸漬させる方法、PVA系樹脂層に当該染色液を塗工する方法、当該染色液をPVA系樹脂層に噴霧する方法等が挙げられ、ヨウ素を含む染色液にPVA系樹脂層(積層体)を浸漬させる方法が好ましい。
必要に応じて、前記染色処理工程の後、水中延伸処理工程の前に、架橋処理工程を施してもよい。前記架橋処理工程は、代表的には、ホウ酸水溶液にPVA系樹脂層を浸漬させることにより行う。架橋処理工程を施すことにより、PVA系樹脂層に耐水性を付与し、後の水中延伸で、高温の水中へ浸漬した際のPVAの配向低下を防止することができる。当該ホウ酸水溶液のホウ酸濃度は、水100重量部に対して、1~5重量部程度であることが好ましい。また、架橋処理工程を行う場合、さらに、架橋浴には前記ヨウ化物を配合することが好ましい。前記ヨウ化物を配合することにより、PVA系樹脂層に吸着させたヨウ素の溶出を抑制することができる。前記ヨウ化物の配合量は、水100重量部に対して、1~5重量部程度であることが好ましい。架橋浴(ホウ酸水溶液)の液温は、20~50℃程度であることが好ましい。
前記水中延伸処理工程は、積層体を延伸浴に浸漬させて行う。水中延伸処理工程によれば、上記熱可塑性樹脂基材やPVA系樹脂層のガラス転移温度(代表的には、80℃程度)よりも低い温度で延伸でき、PVA系樹脂層を、その結晶化を抑えながら、高倍率に延伸することができる。前記水中延伸処理工程の延伸方法は、固定端延伸(たとえば、テンター延伸機を用いて延伸する方法)でもよいし、自由端延伸(たとえば、周速の異なるロール間に積層体を通して一軸延伸する方法)でもよいが、高い光学特性を得る観点から、自由端延伸が好ましい。
前記水中延伸処理工程の後、洗浄処理工程を施すことが好ましい。前記洗浄処理工程は、代表的には、ヨウ化カリウム水溶液にPVA系樹脂層を浸漬させることにより行う。
本発明の粘着剤層を形成する粘着剤としては、偏光フィルムに用いられている各種の粘着剤を適用でき、例えば、ゴム系粘着剤、アクリル系粘着剤、シリコーン系粘着剤、ウレタン系粘着剤、ビニルアルキルエーテル系粘着剤、ポリビニルアルコール系粘着剤、ポリビニルポロリドン系粘着剤、ポリアクリルアミド系粘着剤、セルロース系粘着剤等が挙げられる。これらの中でも、アクリル系粘着剤が好適である。前記アクリル系粘着剤は、ベースポリマーとしてアクリル系ポリマーを含有するものであり、例えば、特開2017-75998号公報等に記載のアクリル系粘着剤が例示できる。
本発明の接着剤層を形成する接着剤としては、偏光フィルムに用いられている各種の接着剤を適用でき、例えば、イソシアネート系接着剤、ポリビニルアルコール系接着剤、ゼラチン系接着剤、ビニル系ラテックス系、水系ポリエステル等が挙げられる。これら接着剤は、通常、水溶液からなる接着剤(水系接着剤)として用いられ、0.5~60重量%の固形分を含有してなる。これらの中でも、ポリビニルアルコール系接着剤が好ましく、アセトアセチル基含有ポリビニルアルコール系接着剤がより好ましい。
本発明の片面保護偏光フィルムは、前記偏光膜の少なくとも一方の面に、前記粘着剤層または前記接着剤層を介して透明保護フィルムが貼り合わされているものである。また、本発明の両面保護偏光フィルムは、前記偏光膜の両面に、前記粘着剤層または前記接着剤層を介して透明保護フィルムが貼り合わされているものである。
本発明の積層偏光フィルム(光学積層体)は、前記片面保護偏光フィルムまたは前記両面保護偏光フィルムの少なくとも一方の面に、光学層が、前記粘着剤層または前記接着剤層を介して貼り合わされているものである。
本発明の前面透明部材は、画像表示セルの視認側に配置される前面透明部材である。前記前面透明部材としては、例えば、前面透明板(ウインドウ層)やタッチパネル等が挙げられる。前記前面透明板としては、適宜の機械強度および厚みを有する前面透明板が用いられる。このような透明板としては、例えば、アクリル系樹脂やポリカーボネート系樹脂のような透明樹脂板、あるいはガラス板等が用いられる。前記タッチパネルとしては、例えば、抵抗膜方式、静電容量方式、光学方式、超音波方式等の各種タッチパネルや、タッチセンサー機能を備えるガラス板や透明樹脂板等が用いられる。前記前面透明部材として静電容量方式のタッチパネルが用いられる場合、タッチパネルよりもさらに視認側に、ガラスや透明樹脂板からなる前面透明板が設けられることが好ましい。
本発明の画像表示セルとしては、例えば、液晶セルや有機ELセル等が挙げられる。前記液晶セルとしては、例えば、外光を利用する反射型液晶セル、バックライト等の光源からの光を利用する透過型液晶セル、外部からの光と光源からの光の両者を利用する半透過半反射型液晶セルのいずれを用いてもよい。前記液晶セルが光源からの光を利用するものである場合、画像表示装置(液晶表示装置)は、画像表示セル(液晶セル)の視認側と反対側にも偏光フィルムが配置され、さらに光源が配置される。当該光源側の偏光フィルムと液晶セルとは、適宜の接着剤層を介して貼り合せられていることが好ましい。前記液晶セルの駆動方式としては、例えば、VAモード、IPSモード、TNモード、STNモードやベンド配向(π型)等の任意なタイプのものを用いうる。
<偏光膜の作製>
平均重合度が2,400、ケン化度が99.9モル%、厚みが45μmであるポリビニルアルコールフィルムを用意した。ポリビニルアルコールフィルムを、周速比の異なるロール間で、20℃の膨潤浴(水浴)中に30秒間浸漬して膨潤しながら搬送方向に2.2倍に延伸し(膨潤工程)、続いて、30℃の染色浴(水100重量部に対して、ヨウ素とヨウ化カリウムを1:7の重量比で配合して得られたヨウ素水溶液)中で最終的に得られる偏光膜のヨウ素濃度が4.47重量%となるように濃度を調整しながら30秒間浸漬して染色しながら元のポリビニルアルコールフィルム(搬送方向に全く延伸していないポリビニルアルコールフィルム)を基準にして搬送方向に3.3倍に延伸した(染色工程)。次いで、染色したポリビニルアルコールフィルムを、40℃の架橋浴(ホウ酸濃度が3.0重量%、ヨウ化カリウム濃度が3.0重量%である水溶液)中で28秒間浸漬して元のポリビニルアルコールフィルムを基準にして搬送方向に3.6倍まで延伸した(架橋工程)。さらに、得られたポリビニルアルコールフィルムを、61℃の延伸浴(ホウ酸濃度が4.0重量%、ヨウ化カリウム濃度が5.0重量%である水溶液)中で60秒間浸漬して元のポリビニルアルコールフィルムを基準にして搬送方向に6.0倍まで延伸した(延伸工程)後、35℃の洗浄浴(ヨウ化カリウム濃度が2.0重量%、下記一般式(6)で示されるヒンダードアミン系化合物濃度が0.4重量%である水溶液)中で10秒間浸漬した(洗浄工程)。洗浄したポリビニルアルコールフィルムを、40℃で30秒間乾燥して偏光膜を作製した。以下の測定方法にて求めた、偏光膜中のヒンダードアミン含有量は0.28重量%であり、また、偏光膜の厚みは18μmであった。なお、下記一般式(6)で示されるヒンダードアミン系化合物は、25℃の水100重量部に対して1重量部以上溶解する化合物である。
偏光膜約20mgを採取、定量し、水1mL中で加熱溶解させた後、メタノール4.5mLで希釈し、得られた抽出液をメンブレンフィルターでろ過し、ろ液をHPLC(Waters社製 ACQUITY UPLC H-class Bio)を用いてヒンダードアミン系化合物の濃度を測定した。
偏光膜について、蛍光X線分析装置(リガク社製、商品名「ZSX-PRIMUS IV」、測定径:ψ20mm)を用いて、下記式を用いてヨウ素濃度(重量%)を求めた。
ヨウ素濃度(wt%)=14.474×(蛍光X線強度)/(フィルム厚み)(kcps/μm)なお、濃度を算出する際の係数は測定装置によって異なるが、当該係数は適切な検量線を用いて求めることができる。
接着剤として、アセトアセチル基を含有するポリビニルアルコール樹脂(平均重合度が1,200、ケン化度が98.5モル%、アセトアセチル化度が5モル%)とメチロールメラミンとを重量比3:1で含有する水溶液を用いた。この接着剤を用いて、上記で得られた偏光膜の両面に、透明保護フィルムとして、ハードコート層を有する厚み47μmのトリアセチルセルロースフィルム(透湿度が342g/(m2・24h)、コニカミノルタ製、商品名「KC4UYW」)をロール貼合機で貼り合わせた後、引き続きオーブン内で加熱乾燥(温度が60℃、時間が4分間)させて、偏光膜の両面に透明保護フィルムが貼り合わせられた偏光フィルムを作製した。偏光フィルムの単体透過率は37.4%であった。
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート99重量部、4-ヒドロキシブチルアクリレート1重量部を含有するモノマー混合物を仕込んだ。さらに、前記モノマー混合物(固形分)100重量部に対して、重合開始剤として2,2’-アゾビスイソブチロニトリル0.1重量部を酢酸エチル100重量部と共に仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を55℃付近に保って8時間重合反応を行って、重量平均分子量(Mw)180万のアクリル系ポリマーの溶液を調製した。その後、得られたアクリル系ポリマーの溶液の固形分100重量部に対して、イソシアネート架橋剤(東ソー社製、商品名「タケネートD110N」、トリメチロールプロパン/キシリレンジイソシアネート付加物)0.02重量部、シランカップリング剤(信越化学工業社製、商品名「X-41-1056」)0.2重量部を配合して、アクリル系粘着剤組成物の溶液を調製した。次いで、上記で得られたアクリル系粘着剤組成物の溶液を、シリコーン系剥離剤で処理されたポリエチレンテレフタレートフィルム(三菱化学ポリエステルフィルム製、商品名「MRF38」、セパレータフィルム)の片面に、乾燥後の粘着剤層の厚さが20μmになるように塗布し、90℃で1分間乾燥を行い、セパレータフィルムの表面に粘着剤層を形成した。次いで、上記で作製した偏光フィルムの一方の面に、セパレータフィルム上に形成した粘着剤層を転写して、粘着剤層付き偏光フィルムを作製した。
上記で得られた粘着剤層付き偏光フィルムを、偏光膜の吸収軸が長辺となるように40×40mmのサイズに切断し、粘着剤層を介してガラス板(疑似画像表示セル)を貼り合わせ、偏光フィルムの他方の面に厚み200μmのアクリル酸モノマーフリー粘着剤(日東電工(株)製、商品名「LUCIACS CS9868」)を介して別のガラス板(疑似前面透明部材)を貼り合わせて、疑似画像表示装置(積層体)を作製した。
上記で得られた疑似画像表示装置(積層体)を、温度105℃の熱風オーブン内に48時間静置し、投入(加熱)前後の単体透過率(ΔTs)を測定した。単体透過率は、分光光度計(村上色彩技術研究所(株)製、製品名「DOT-3」)を用いて測定し、以下の基準で評価した。当該単体透過率は、JlS Z 8701-1982の2度視野(C光源)により、視感度補正を行ったY値である。なお、測定波長は、380~700nm(10nm毎)である。結果を表1に示す。
ΔTs(%)=Ts48-Ts0
ここで、Ts0は加熱前の疑似画像表示装置(積層体)の単体透過率であり、Ts48は48時間加熱後の疑似画像表示装置(積層体)の単体透過率である。
○:5≧ΔTs(%)≧0
×:ΔTs(%)>5、あるいはΔTs(%)<0
上記で得られた疑似画像表示装置(積層体)を、温度105℃の熱風オーブン内に24時間静置し、投入(加熱)後の偏光膜中に含まれるヒンダードアミン系化合物の含有量を以下の方法にて求めた。加熱後の疑似画像表示装置を約1000mLの塩化メチレンまたはトルエンの溶液に3日間以上浸漬させ、保護フィルムを溶解させることで偏光膜を取り出したところ、偏光膜は約40mgであった。前記偏光膜を純粋な塩化メチレンまたはトルエンで洗浄した後、偏光膜約1mgを採取、定量し、水0.5mL中で加熱溶解させた後、メタノール1mLで希釈し、得られた抽出液をメンブレンフィルターでろ過し、ろ液をLCMS(Thermo Fisher Scientific製 UltiMate3000/ LTQ orbitrap XL)を用いてヒンダードアミン系化合物の濃度を測定した。
<偏光膜、光フィルム、疑似画像表示装置(積層体)の作製>
偏光膜の作製において、洗浄浴に一般式(6)で示されるヒンダードアミン系化合物を添加せずに、かつ偏光フィルムの作製において、使用する両方の接着剤に一般式(6)で示されるヒンダードアミン系化合物をポリビニルアルコール樹脂との重量比で4:3となるように添加したこと以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。偏光フィルムの単体透過率は39.7%であった。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光膜の作製において、洗浄浴に一般式(6)で示されるヒンダードアミン系化合物を添加せずに、かつ偏光フィルムの作製において、使用する両方の接着剤に一般式(7)で示されるヒンダードアミン系化合物をポリビニルアルコール樹脂との重量比で4:3となるように添加し、接着剤の硬化反応に影響を与えないように、ヒンダードアミン系化合物に対してモル比で1:1となるように水酸化カリウムを添加して、pHを調整したこと(中和したこと)以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。偏光フィルムの単体透過率は40.0%であった。なお、下記一般式(7)で示されるヒンダードアミン系化合物は、25℃の水100重量部に対して1重量部以上溶解する化合物である。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光膜の作製において、洗浄浴に一般式(6)で示されるヒンダードアミン系化合物を添加せずに、かつ偏光フィルムの作製において、使用する両方の接着剤に一般式(8)で示されるヒンダードアミン系化合物をポリビニルアルコール樹脂との重量比で4:3となるように添加し、接着剤の硬化反応に影響を与えないように、ヒンダードアミン系化合物に対してモル比で1:1となるように塩酸を添加して、pHを調整したこと(中和したこと)以外は、以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。偏光フィルムの単体透過率は39.9%であった。なお、下記一般式(8)で示されるヒンダードアミン系化合物は、25℃の水100重量部に対して1重量部以上溶解する化合物である。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光膜の作製において、洗浄浴に一般式(6)で示されるヒンダードアミン系化合物を添加せずに、かつ偏光フィルムの作製において、使用する両方の接着剤として、アセトアセチル基を含有するポリビニルアルコール樹脂とメチロールメラミンと一般式(6)で示されるヒンダードアミン系化合物とを重量比7:2:1で含有する水溶液を用いたこと以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。偏光フィルムの単体透過率は39.7%であった。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光フィルムの作製において、使用する両方の接着剤として、N-ヒドロキシエチルアクリルアミド(HEAA)40重量部とアクリロイルモルホリン(ACMO)60重量部と光開始剤「IRGACURE 819」(BASF社製)3重量部を混合し、接着剤を調製し、硬化後の接着剤層の厚みが1.0μmとなるように偏光フィルム上に塗布し、活性エネルギー線として紫外線を照射し、接着剤を硬化させて偏光フィルムを作製したこと以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。紫外線照射は、ガリウム封入メタルハライドランプ、照射装置:Fusion UV Systems,Inc社製のLight HAMMER10、バルブ:Vバルブ、ピーク照度:1600mW/cm2、積算照射量1000/mJ/cm2(波長380~440nm)を使用し、紫外線の照度は、Solatell社製のSola-Checkシステムを使用して測定した。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
熱可塑性樹脂基材として、長尺状で、吸水率0.75%、Tg約75℃である、非晶質のイソフタル共重合ポリエチレンテレフタレートフィルム(厚み:100μm)を用いた。樹脂基材の片面に、コロナ処理を施した。ポリビニルアルコール(重合度4200、ケン化度99.2モル%)およびアセトアセチル変性PVA(日本合成化学工業社製、商品名「ゴーセファイマーZ410」)を9:1で混合したPVA系樹脂100重量部に、ヨウ化カリウム13重量部を添加し、PVA水溶液(塗布液)を調製した。樹脂基材のコロナ処理面に、上記PVA水溶液を塗布して60℃で乾燥することにより、厚み13μmのPVA系樹脂層を形成し、積層体を作製した。得られた積層体を、130℃のオーブン内で周速の異なるロール間で縦方向(長手方向)に2.4倍に自由端一軸延伸した(空中補助延伸処理)。次いで、積層体を、液温40℃の不溶化浴(ホウ酸濃度4.0重量%である水溶液)に30秒間浸漬させた(不溶化処理)。次いで、液温30℃の染色浴(水100重量部に対して、ヨウ素とヨウ化カリウムを1:7の重量比で配合して得られたヨウ素水溶液)に、最終的に得られる偏光膜のヨウ素濃度が8.11%となるように濃度を調整しながら60秒間浸漬させた(染色処理)。次いで、液温40℃の架橋浴(ヨウ化カリウム濃度3.0重量%、ホウ酸濃度5.0重量%である水溶液)に30秒間浸漬させた(架橋処理)。その後、積層体を、液温70℃のホウ酸水溶液(ホウ酸濃度4.0重量%)に浸漬させながら、周速の異なるロール間で縦方向(長手方向)に総延伸倍率が5.5倍となるように一軸延伸を行った(水中延伸処理)。その後、積層体を液温30℃の洗浄浴(ヨウ化カリウム濃度3重量%)に浸漬させた(洗浄処理)。その後、90℃に保たれたオーブン中で乾燥しながら、表面温度が75℃に保たれたSUS製の加熱ロールに約2秒接触させた(乾燥収縮処理)。このようにして、樹脂基材上に厚み5μmの偏光膜を形成した。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光膜の作製において、洗浄浴に一般式(6)で示されるヒンダードアミン系化合物を添加しなかったこと以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。得られた偏光膜は、ヒンダードアミン含有量が0重量%であり、厚みが18μmであった。偏光フィルムの単体透過率は39.6%であった。
<偏光膜偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光フィルムの作製において、アクリル系粘着剤にヒンダードアミン系化合物を添加しなかったこと以外は、実施例7と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。
<偏光膜、偏光フィルム、疑似画像表示装置(積層体)の作製>
偏光膜の作製において、洗浄浴に一般式(6)で示されるヒンダードアミン系化合物を添加しなかったこと、また、接着剤として、N-ヒドロキシエチルアクリルアミド(HEAA)35重量部とアクリロイルモルホリン(ACMO)50重量部と光開始剤「IRGACURE 819」(BASF社製)5重量部と一般式(9)で示される化合物(商品名「アデカスタブ LA-52」、ADEKA社製)を10重量部とを混合し、硬化後の接着剤層の厚みが1.0μmとなるように偏光膜上に塗布し、活性エネルギー線として、紫外線を照射し、接着剤を硬化させて偏光フィルムを作製したこと以外は、実施例1と同様の操作にて、偏光膜、偏光フィルム、および疑似画像表示装置(積層体)を作製した。紫外線照射は、ガリウム封入メタルハライドランプ、照射装置:Fusion UV Systems,Inc社製のLight HAMMER10、バルブ:Vバルブ、ピーク照度:1600mW/cm2、積算照射量1000/mJ/cm2(波長380~440nm)を使用し、紫外線の照度は、Solatell社製のSola-Checkシステムを使用して測定した。なお、下記一般式(9)で示されるヒンダードアミン系化合物は、25℃の水100重量部に対して1重量部以上溶解しない化合物である。
11:偏光膜
12、および13:透明保護フィルム
20、30、40、および50:粘着剤層または接着剤層
80:前面透明部材
90:画像表示セル
100:画像表示装置
101:片面保護偏光フィルム
102:両面保護偏光フィルム
Claims (6)
- 前面透明部材、偏光フィルム、および画像表示セルが、粘着剤層または接着剤層を介してこの順に設けられた画像表示装置であって、
前記偏光フィルムは、ポリビニルアルコール系フィルムにヨウ素が吸着配向して形成される偏光膜を有し、
前記偏光フィルム、前記粘着剤層、および前記接着剤層の少なくとも1つが、ヒンダードアミン系化合物を含有し、
前記ヒンダードアミン系化合物は、25℃の水100重量部に対して1重量部以上溶解できる、水溶性ヒンダードアミン系化合物であり、
前記偏光フィルムが、一般式(1):X(重量%)>0.01
(一般式(1)中、Xは、前記偏光膜の少なくとも片面に前記接着剤層を介して透明保護フィルムが貼り合わされている偏光フィルムの両面に、前記粘着剤層を介してガラス板を貼り合わせた積層体が、105℃、24時間の条件で放置された積層体における当該偏光膜中のヒンダードアミン系化合物の含有量を示す。)で表される条件を満たすことを特徴とする画像表示装置。 - 前記ヒンダードアミン系化合物が一般式(2):
一般式(3):
一般式(4):
一般式(5):
- 前記偏光フィルムは、前記偏光膜の少なくとも一方の面に、前記粘着剤層または前記接着剤層を介して透明保護フィルムが貼り合わされている片面保護偏光フィルムであることを特徴とする請求項1~3のいずれかに記載の画像表示装置。
- 前記偏光フィルムは、前記偏光膜の両面に、透明保護フィルムが前記粘着剤層または前記接着剤層を介して貼り合わされている両面保護偏光フィルムであることを特徴とする請求項1~3のいずれかに記載の画像表示装置。
- 前記片面保護偏光フィルムまたは前記両面保護偏光フィルムの少なくとも一方の面に、光学層が、前記粘着剤層または前記接着剤層を介して貼り合わされている積層偏光フィルムであることを特徴とする請求項4または5記載の画像表示装置。
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KR20200105959A (ko) | 2020-09-09 |
TW202024687A (zh) | 2020-07-01 |
WO2020100869A1 (ja) | 2020-05-22 |
TWI844577B (zh) | 2024-06-11 |
JP2020184078A (ja) | 2020-11-12 |
KR102266084B1 (ko) | 2021-06-17 |
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CN111819617B (zh) | 2021-12-28 |
JP6724269B1 (ja) | 2020-07-15 |
TWI828796B (zh) | 2024-01-11 |
CN111819617A (zh) | 2020-10-23 |
KR20210075966A (ko) | 2021-06-23 |
CN111819260B (zh) | 2021-05-11 |
JPWO2020100870A1 (ja) | 2021-02-15 |
TW202024688A (zh) | 2020-07-01 |
KR20200108079A (ko) | 2020-09-16 |
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KR102281482B1 (ko) | 2021-07-26 |
CN111819260A (zh) | 2020-10-23 |
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