WO2015133269A1 - Procédé de fabrication de plaque de polarisation - Google Patents

Procédé de fabrication de plaque de polarisation Download PDF

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Publication number
WO2015133269A1
WO2015133269A1 PCT/JP2015/054386 JP2015054386W WO2015133269A1 WO 2015133269 A1 WO2015133269 A1 WO 2015133269A1 JP 2015054386 W JP2015054386 W JP 2015054386W WO 2015133269 A1 WO2015133269 A1 WO 2015133269A1
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Prior art keywords
film
protective film
layer
polarizing plate
polyvinyl alcohol
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PCT/JP2015/054386
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English (en)
Japanese (ja)
Inventor
直子 竹之熊
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住友化学株式会社
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Application filed by 住友化学株式会社 filed Critical 住友化学株式会社
Priority to CN201580011342.6A priority Critical patent/CN106062595B/zh
Priority to KR1020167022955A priority patent/KR101942166B1/ko
Publication of WO2015133269A1 publication Critical patent/WO2015133269A1/fr

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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/30—Polarising elements
    • G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
    • G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid

Definitions

  • the present invention relates to a method for producing a polarizing plate.
  • Polarizing plates have been widely used in display devices such as liquid crystal display devices, particularly in recent years for flat-screen TVs and various mobile devices.
  • a polarizing plate the thing of the structure which bonded the protective film on the single side
  • the polarizing plate can be manufactured by a method in which a protective film is bonded to a polarizer (polarizing film) made of a single (single) film via an adhesive layer (hereinafter also referred to as “single film method”).
  • It can also manufacture by the method (henceforth a "coating method") including the process of bonding a protective film through an adhesive bond layer; The process of peeling and removing a base film after bonding of a protective film.
  • the latter method is advantageous in that the film is easily handled during the process and that a thin polarizer layer is easily obtained.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2009-098653 (Patent Document 1) and Japanese Patent Application Laid-Open No. 2009-093074 (Patent Document 2) describe that a polarizing plate is produced by a method similar to a coating method.
  • Patent Documents 1 and 2 describe that curling of a polarizing plate can be suppressed by a method similar to the above-described coating method.
  • the polarizing plate in which curling is referred to in these documents is a polarizing plate that is used as a protective film for the polarizer layer without peeling off and removing the base film in the above-described coating method.
  • the present invention provides the following method for producing a polarizing plate.
  • a protective film adjusted to a moisture content higher than the equilibrium moisture content at 25 ° C. and 55% RH on a polarizer layer of a polarizing laminated film having a polarizer layer on at least one surface of a base film.
  • the polarizing laminated film is After applying a coating liquid containing a polyvinyl alcohol-based resin on at least one surface of the base film, a step of forming a polyvinyl alcohol-based resin layer by drying to obtain a laminated film; Stretching the laminated film to obtain a stretched film; A step of obtaining a polarizing laminated film by dyeing a polyvinyl alcohol-based resin layer of the stretched film with a dichroic dye to form the polarizer layer;
  • the production method according to [1] or [2] which is produced by a method comprising:
  • the base film is peeled and removed, and the protective film is bonded to the polarizer layer and at least one surface thereof.
  • curling of the obtained polarizing plate can be suppressed.
  • FIG. 1 is a flowchart showing a preferred example of a method for producing a polarizing plate according to the present invention.
  • the production method of the present invention comprises the following steps: (1) First protection adjusted to a moisture content higher than the equilibrium moisture content at 25 ° C. and 55% RH on a polarizer layer of a polarizing laminate film having a polarizer layer on at least one surface of a base film. 1st protective film bonding process S10 which bonds a film through an adhesive bond layer, (2) Peeling step S20 for peeling and removing the base film after the first protective film bonding step, including.
  • the polarizing laminated film preferably has the following steps as in the above-described coating method: [A] A resin layer forming step of forming a polyvinyl alcohol resin layer by applying a coating liquid containing a polyvinyl alcohol resin on at least one surface of a substrate film and then drying to form a laminated film S1-1, [B] Stretching step S1-2 for stretching a laminated film to obtain a stretched film, [C] Dyeing step S1-3 for obtaining a polarizing laminated film by dyeing a polyvinyl alcohol resin layer of a stretched film with a dichroic dye to form a polarizer layer; Manufactured by a method comprising:
  • the single-sided protective film-attached polarizing plate in which the first protective film is bonded to one surface of the polarizer layer is obtained.
  • 2nd protective film bonding process S30 which bonds a 2nd protective film through the adhesive layer on the surface at the side of the polarizer layer of a polarizing plate with a single-sided protective film is carried out. It may be provided to obtain a polarizing plate with a double-sided protective film.
  • the polarizing plate in the present invention (the polarizing plate obtained by the production method of the present invention) is composed of a polarizer layer and a protective film laminated on at least one surface of the polarizing plate via an adhesive layer (that is, , A polarizing plate with a single-sided protective film or a polarizing plate with a double-sided protective film), which does not have a base film contained in a polarizing laminated film that is a precursor thereof.
  • the polarizing plate obtained by the production method of the present invention can be used as a composite polarizing plate by laminating other optical members (peripheral members) such as other films and layers on the polarizing plate. You can do it.
  • the polarizer layer can be obtained by adsorbing and orienting a dichroic dye on a uniaxially stretched polyvinyl alcohol-based resin layer (or film).
  • the light-polarizing laminated film in this invention is provided with a base material film and the polarizer layer laminated
  • polarizing laminated film with protective film Also called “film”.
  • the polyvinyl alcohol-based resin layer may be formed on both sides of the base film, but the case where it is mainly formed on one side will be described below.
  • the polarizing laminated film is preferably produced by a method including [a] resin layer forming step S1-1, [b] stretching step S1-2, and [c] dyeing step S1-3.
  • this step is a step of obtaining laminated film 100 by forming polyvinyl alcohol-based resin layer 6 on at least one surface of base film 30.
  • the polyvinyl alcohol resin layer 6 is a layer that becomes the polarizer layer 5 through the stretching step S1-2 and the dyeing step S1-3.
  • the polyvinyl alcohol-based resin layer 6 can be formed by applying a coating liquid containing a polyvinyl alcohol-based resin to one or both surfaces of the base film 30 and drying the coating layer.
  • the base film 30 can be composed of a thermoplastic resin, and is preferably composed of a thermoplastic resin excellent in transparency, mechanical strength, thermal stability, stretchability and the like.
  • thermoplastic resins include, for example, polyolefin resins such as chain polyolefin resins and cyclic polyolefin resins (norbornene resins, etc.); polyester resins; (meth) acrylic resins; cellulose triacetate, Cellulose ester resins such as cellulose diacetate; Polycarbonate resins; Polyvinyl alcohol resins; Polyvinyl acetate resins; Polyarylate resins; Polystyrene resins; Polyethersulfone resins; Polysulfone resins; Polyamide resins; System resins; and mixtures and copolymers thereof.
  • (meth) acryl means at least one selected from acrylic and methacrylic. The same applies to cases such as “(meth) acryloyl”.
  • the base film 30 may have a single-layer structure made of one resin layer made of one kind or two or more kinds of thermoplastic resins, or a plurality of resin layers made of one kind or two or more kinds of thermoplastic resins. A laminated multilayer structure may be used.
  • the base film 30 is made of a resin that can be stretched at a stretching temperature suitable for stretching the polyvinyl alcohol-based resin layer 6 when the laminated film 100 is stretched in the stretching step S1-2 described later. preferable.
  • the base film 30 can contain an additive.
  • the additive include an ultraviolet absorber, an antioxidant, a lubricant, a plasticizer, a release agent, an anti-coloring agent, a flame retardant, a nucleating agent, an antistatic agent, a pigment, and a coloring agent.
  • the content of the thermoplastic resin in the base film 30 is preferably 50 to 100% by weight, more preferably 50 to 99% by weight, still more preferably 60 to 98% by weight, and particularly preferably 70 to 97% by weight. .
  • the thickness of the base film 30 is usually 1 to 500 ⁇ m, preferably 1 to 300 ⁇ m, more preferably 5 to 200 ⁇ m, and still more preferably 5 to 150 ⁇ m from the viewpoint of workability such as strength and handleability.
  • the coating liquid applied to the base film 30 is preferably a polyvinyl alcohol resin solution obtained by dissolving a polyvinyl alcohol resin powder in a good solvent (for example, water).
  • a polyvinyl alcohol resin examples include polyvinyl alcohol resins and derivatives thereof. Derivatives of polyvinyl alcohol resins include polyvinyl formal, polyvinyl acetal, etc., as well as polyvinyl alcohol resins modified with olefins such as ethylene and propylene; unsaturated carboxylic acids such as acrylic acid, methacrylic acid and crotonic acid. Denatured; modified with alkyl ester of unsaturated carboxylic acid; modified with (meth) acrylamide.
  • the proportion of modification is preferably less than 30 mol%, and more preferably less than 10 mol%.
  • the proportion of modification is preferably less than 30 mol%, and more preferably less than 10 mol%.
  • the average degree of polymerization of the polyvinyl alcohol-based resin is preferably in the range of 100 to 10000, more preferably in the range of 1000 to 10000, still more preferably in the range of 1500 to 8000, and in the range of 2000 to 5000. Most preferably.
  • the average degree of polymerization can be determined by a method specified in JIS K 6726-1994 “Testing method for polyvinyl alcohol”. If the average degree of polymerization is less than 100, it is difficult to obtain a preferable polarization performance, and if it exceeds 10,000, the solubility in a solvent is deteriorated, and it becomes difficult to form a polyvinyl alcohol-based resin layer.
  • the polyvinyl alcohol resin is preferably a saponified product of a polyvinyl acetate resin.
  • the range of the saponification degree is preferably 80 mol% or more, more preferably 90 mol% or more, and particularly preferably 94 mol% or more. If the degree of saponification is too low, the water resistance and heat-and-moisture resistance may not be sufficient when a polarizing laminate film or a polarizing plate is formed. Further, it may be a completely saponified product (having a saponification degree of 100 mol%), but if the saponification degree is too high, the dyeing speed becomes slow, and the production time is required to give sufficient polarization performance. In some cases, a polarizer layer having sufficient polarization performance may not be obtained. Therefore, the saponification degree is preferably 99.5 mol% or less, more preferably 99.0 mol% or less.
  • the degree of saponification is the unit ratio (mol%) of the ratio of acetate groups (acetoxy groups: —OCOCH 3 ) contained in polyvinyl acetate resin, which is a raw material for polyvinyl alcohol resins, to hydroxyl groups by saponification treatment.
  • the following formula: Saponification degree (mol%) [(number of hydroxyl groups) ⁇ (number of hydroxyl groups + number of acetate groups)] ⁇ 100
  • the saponification degree can be determined according to JIS K 6726 (1994). The higher the degree of saponification, the higher the proportion of hydroxyl groups, and thus the lower the proportion of acetate groups that inhibit crystallization.
  • polyvinyl acetate resin examples include polyvinyl acetate, which is a homopolymer of vinyl acetate, and copolymers with other monomers copolymerizable with vinyl acetate.
  • examples of other monomers copolymerizable with vinyl acetate include unsaturated carboxylic acids, olefins, vinyl ethers, unsaturated sulfonic acids, and (meth) acrylamides having an ammonium group.
  • the coating liquid may contain additives such as a plasticizer and a surfactant as necessary.
  • a plasticizer polyol or a condensate thereof can be used, and examples thereof include glycerin, diglycerin, triglycerin, ethylene glycol, propylene glycol, and polyethylene glycol.
  • the blending amount of the additive is preferably 20% by weight or less of the polyvinyl alcohol resin.
  • the coating liquid is applied to the base film 30 by a wire bar coating method; a roll coating method such as reverse coating or gravure coating; a die coating method; a comma coating method; a lip coating method; a spin coating method;
  • the method can be appropriately selected from a method such as a fountain coating method, a dipping method, and a spray method.
  • the drying temperature and drying time of the coating layer are set according to the type of solvent contained in the coating solution.
  • the drying temperature is, for example, 50 to 200 ° C., preferably 60 to 150 ° C.
  • the drying temperature is preferably 80 ° C. or higher.
  • the polyvinyl alcohol-based resin layer 6 may be formed only on one side of the base film 30 or on both sides. When formed on both sides, two polarizing plates can be obtained from one polarizing laminated film 300, which is advantageous in terms of production efficiency of the polarizing plate.
  • the thickness of the polyvinyl alcohol resin layer 6 in the laminated film 100 is preferably 3 to 30 ⁇ m, and more preferably 5 to 20 ⁇ m. If the polyvinyl alcohol-based resin layer 6 has a thickness within this range, the dichroic dye has good dyeability and excellent polarization performance through a stretching step S1-2 and a dyeing step S1-3, which will be described later. A very thin (for example, a thickness of 10 ⁇ m or less) polarizer layer 5 can be obtained. If the thickness of the polyvinyl alcohol-based resin layer 6 is less than 3 ⁇ m, the film becomes too thin after stretching and the dyeability tends to deteriorate.
  • At least the surface of the base film 30 on the side where the polyvinyl alcohol resin layer 6 is formed is provided. Corona treatment, plasma treatment, flame (flame) treatment or the like may be performed.
  • the polyvinyl alcohol resin layer 6 Prior to coating the coating liquid, the polyvinyl alcohol resin layer 6 is provided on the base film 30 via a primer layer or the like in order to improve the adhesion between the base film 30 and the polyvinyl alcohol resin layer 6. May be formed.
  • the primer layer can be formed by applying a primer layer forming coating solution onto the surface of the base film 30 and then drying it.
  • the primer layer forming coating solution contains a component that exhibits a certain degree of strong adhesion to both the base film 30 and the polyvinyl alcohol-based resin layer 6.
  • the primer layer-forming coating solution usually contains a resin component that imparts such adhesion and a solvent.
  • a resin component a thermoplastic resin excellent in transparency, thermal stability, stretchability and the like is preferably used, and examples thereof include (meth) acrylic resins and polyvinyl alcohol resins. Among these, polyvinyl alcohol resins that give good adhesion are preferably used. More preferably, it is a polyvinyl alcohol resin.
  • As the solvent a general organic solvent or an aqueous solvent capable of dissolving the resin component is usually used, but it is preferable to form the primer layer from a coating solution containing water as a solvent.
  • a crosslinking agent may be added to the primer layer forming coating solution.
  • a suitable crosslinking agent is appropriately selected from known ones such as organic and inorganic based on the type of thermoplastic resin to be used.
  • cross-linking agents include epoxy-based, isocyanate-based, dialdehyde-based, metal-based (for example, metal salts, metal oxides, metal hydroxides, organometallic compounds), and polymer-based cross-linking agents. .
  • a polyvinyl alcohol resin is used as the resin component for forming the primer layer
  • a polyamide epoxy resin, a methylolated melamine resin, a dialdehyde crosslinking agent, a metal chelate compound crosslinking agent, or the like is preferably used.
  • the thickness of the primer layer is preferably about 0.05 to 1 ⁇ m, more preferably 0.1 to 0.4 ⁇ m.
  • the thickness is less than 0.05 ⁇ m, the effect of improving the adhesion between the base film 30 and the polyvinyl alcohol-based resin layer 6 is small, and when the thickness is more than 1 ⁇ m, it is disadvantageous for thinning the polarizing plate.
  • the method of applying the primer layer forming coating solution to the base film 30 can be the same as the coating solution for forming the polyvinyl alcohol-based resin layer.
  • the primer layer is applied to the surface on which the coating liquid for forming the polyvinyl alcohol-based resin layer is applied.
  • the drying temperature of the coating layer made of the primer layer forming coating solution is, for example, 50 to 200 ° C., and preferably 60 to 150 ° C. When the solvent contains water, the drying temperature is preferably 80 ° C. or higher.
  • Stretching step S1-2 With reference to FIG. 5, this process extends
  • the film 200 is obtained.
  • the stretching process is usually uniaxial stretching.
  • the stretching ratio of the laminated film 100 can be appropriately selected depending on the desired polarization characteristics, but is preferably more than 5 times and not more than 17 times, more preferably more than 5 times the original length of the laminated film 100. 8 times or less.
  • the draw ratio is 5 times or less, the polyvinyl alcohol-based resin layer 6 ′ is not sufficiently oriented, and the degree of polarization of the polarizer layer 5 may not be sufficiently high.
  • the draw ratio exceeds 17 times, the film is likely to be broken during stretching, and the thickness of the stretched film 200 becomes unnecessarily thin, and the workability and handleability in subsequent processes may be reduced.
  • the stretching process is not limited to one-stage stretching, and can be performed in multiple stages.
  • all of the multistage stretching processes may be performed continuously before the dyeing process S1-3, or the second and subsequent stretching processes may be performed as a dyeing process and / or a crosslinking process in the dyeing process S1-3. You may do it at the same time.
  • the stretching treatment may be longitudinal stretching that extends in the film longitudinal direction (film transport direction), and may be lateral stretching or oblique stretching that extends in the film width direction.
  • the longitudinal stretching method include inter-roll stretching using a roll, compression stretching, stretching using a chuck (clip), and the like
  • examples of the lateral stretching method include a tenter method.
  • the stretching treatment either a wet stretching method or a dry stretching method can be adopted. However, it is preferable to use the dry stretching method because the stretching temperature can be selected from a wide range.
  • the stretching temperature is set to be equal to or higher than the temperature at which the polyvinyl alcohol-based resin layer 6 and the entire base film 30 can be stretched, and preferably the phase transition temperature (melting point or glass transition temperature) of the base film 30. It is in the range of ⁇ 30 ° C. to + 30 ° C., more preferably in the range of ⁇ 30 ° C. to + 5 ° C., and still more preferably in the range of ⁇ 25 ° C. to + 0 ° C.
  • the phase transition temperature means the highest phase transition temperature among the phase transition temperatures exhibited by the plurality of resin layers.
  • the stretching temperature is lower than the phase transition temperature of ⁇ 30 ° C., it is difficult to achieve a high-magnification stretching of more than 5 times, or the fluidity of the base film 30 is too low and the stretching process tends to be difficult.
  • the stretching temperature exceeds + 30 ° C. of the phase transition temperature, the fluidity of the base film 30 is too large and stretching tends to be difficult. Since it is easier to achieve a high draw ratio of more than 5 times, the drawing temperature is within the above range, and more preferably 120 ° C. or higher.
  • a zone heating method for example, a method in which hot air is blown and heated in a stretching zone such as a heating furnace adjusted to a predetermined temperature
  • a heater heating method a method in which infrared heaters, halogen heaters, panel heaters, etc. are installed above and below the laminated film 100 and heated by radiant heat.
  • the zone heating method is preferable from the viewpoint of the uniformity of the stretching temperature.
  • a preheat treatment step for preheating the laminated film 100 may be provided.
  • the preheating method the same method as the heating method in the stretching process can be used.
  • the preheating temperature is preferably in the range of ⁇ 50 ° C. to ⁇ 0 ° C. of the stretching temperature, and more preferably in the range of ⁇ 40 ° C. to ⁇ 10 ° C. of the stretching temperature.
  • a heat setting treatment step may be provided after the stretching treatment in the stretching step S1-2.
  • the heat setting process is a process in which heat treatment is performed at a temperature equal to or higher than the crystallization temperature while maintaining the tensioned state with the end of the stretched film 200 held by a clip.
  • the crystallization of the polyvinyl alcohol-based resin layer 6 ' is promoted by this heat setting treatment.
  • the temperature of the heat setting treatment is preferably in the range of ⁇ 0 ° C. to ⁇ 80 ° C. of the stretching temperature, and more preferably in the range of ⁇ 0 ° C. to ⁇ 50 ° C. of the stretching temperature.
  • this step is a step of forming the polarizer layer 5 by dyeing the polyvinyl alcohol-based resin layer 6 ′ of the stretched film 200 with a dichroic dye and adsorbing and orienting it.
  • a polarizing laminated film 300 in which the polarizer layer 5 is laminated on one side or both sides of the base film 30 ′ is obtained.
  • iodine or a dichroic organic dye can be used as the dichroic dye.
  • the dyeing step can be performed by immersing the entire stretched film 200 in a solution (dye solution) containing a dichroic dye.
  • a solution in which the above dichroic dye is dissolved in a solvent can be used.
  • a solvent for the dyeing solution water is generally used, but an organic solvent compatible with water may be further added.
  • the concentration of the dichroic dye in the dyeing solution is preferably 0.01 to 10% by weight, more preferably 0.02 to 7% by weight, and further preferably 0.025 to 5% by weight. preferable.
  • iodine When iodine is used as the dichroic dye, it is preferable to further add an iodide to the dyeing solution containing iodine because the dyeing efficiency can be further improved.
  • iodide include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and titanium iodide. Is mentioned.
  • the concentration of iodide in the dyeing solution is preferably 0.01 to 20% by weight. Of the iodides, it is preferable to add potassium iodide.
  • the ratio of iodine to potassium iodide is preferably in the range of 1: 5 to 1: 100, more preferably in the range of 1: 6 to 1:80. Preferably, it is in the range of 1: 7 to 1:70.
  • the temperature of the dyeing solution is preferably in the range of 10 to 60 ° C, more preferably in the range of 20 to 40 ° C.
  • the dyeing step S1-3 can be performed before the stretching step S1-2, or these steps can be performed simultaneously, but the dichroic dye adsorbed on the polyvinyl alcohol-based resin layer can be well oriented. It is preferable to carry out the dyeing step S1-3 after subjecting the laminated film 100 to at least some degree of stretching treatment. That is, the stretched film 200 obtained by performing the stretching process until reaching the target magnification in the stretching step S1-2 can be used for the dyeing step S1-3, and at a lower magnification than the target in the stretching step S1-2. After the stretching process, the stretching process can be performed until the total stretching ratio reaches the target ratio in the dyeing step S1-3.
  • the stretching process is performed so that the total stretching ratio becomes the target ratio during the dyeing process in the dyeing process S1-3.
  • the crosslinking treatment is performed after the dyeing treatment as will be described later
  • 2) the dyeing treatment in the dyeing step S1-3 after the drawing treatment is performed at a lower magnification than the target in the drawing step S1-2.
  • the stretching process is performed until the total stretching ratio does not reach the target ratio, and then the stretching process is performed during the crosslinking process so that the final total stretching ratio becomes the target ratio. it can.
  • the dyeing step S1-3 can include a cross-linking treatment step performed subsequent to the dyeing treatment.
  • the crosslinking treatment can be performed by immersing the dyed film in a solution containing a crosslinking agent (crosslinking solution).
  • a crosslinking agent conventionally known substances can be used, and examples thereof include boron compounds such as boric acid and borax, glyoxal, and glutaraldehyde.
  • a crosslinking agent may be used individually by 1 type, and may use 2 or more types together.
  • the crosslinking solution can be a solution in which a crosslinking agent is dissolved in a solvent.
  • a solvent for example, water can be used, but an organic solvent compatible with water may be further included.
  • the concentration of the crosslinking agent in the crosslinking solution is preferably in the range of 1 to 20% by weight, more preferably in the range of 6 to 15% by weight.
  • the crosslinking solution can contain iodide.
  • iodide By adding iodide, the polarization performance in the plane of the polarizer layer 5 can be made more uniform.
  • iodide include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and titanium iodide. Is mentioned.
  • the concentration of iodide in the cross-linking solution is preferably 0.05 to 15% by weight, and more preferably 0.5 to 8% by weight.
  • the temperature of the crosslinking solution is preferably in the range of 10 to 90 ° C.
  • the crosslinking treatment can be performed simultaneously with the dyeing treatment by blending a crosslinking agent in the dyeing solution. Further, a stretching process may be performed during the crosslinking process.
  • the specific mode for carrying out the stretching treatment during the crosslinking treatment is as described above. Moreover, you may perform the process immersed in a crosslinking solution 2 or more times using 2 or more types of crosslinking solutions from which a composition differs.
  • the washing process usually includes a water washing process.
  • the water washing treatment can be performed by immersing the film after the dyeing treatment or after the crosslinking treatment in pure water such as ion exchange water or distilled water.
  • the water washing temperature is usually in the range of 3 to 50 ° C., preferably 4 to 20 ° C.
  • the washing step may be a combination of a water washing step and a washing step with an iodide solution.
  • any appropriate method such as natural drying, blow drying, and heat drying can be adopted.
  • the drying temperature is usually 20 to 95 ° C.
  • the thickness of the polarizer layer 5 included in the polarizing laminated film 300 can be, for example, 30 ⁇ m or less, and further 20 ⁇ m or less, but is preferably 10 ⁇ m or less from the viewpoint of thinning the polarizing plate, and is 8 ⁇ m or less. Is more preferable.
  • the thickness of the polarizer layer 5 is usually 2 ⁇ m or more.
  • the “equilibrium moisture content at 25 ° C. and 55% RH” of the protective film means the moisture content when left for 24 hours in an environment of 25 ° C. and 55% RH.
  • the base film 30 ′ Polarizing plate manufactured through peeling step S20 for peeling and removing (as described above, the polarizing plate here is a polarizer layer and a protective film laminated on at least one surface of the polarizing plate via an adhesive layer) Can be effectively suppressed.
  • Curling is a phenomenon in which a film such as a polarizing plate (including a laminated film) bends in an arcuate shape (or in a cylindrical shape if remarkable).
  • a film such as a polarizing plate (including a laminated film) bends in an arcuate shape (or in a cylindrical shape if remarkable).
  • a single-side protective film which is formed by laminating the first protective film 10 on one surface of the polarizer layer 5 via the adhesive layer 15, curl with the first protective film 10 side inward.
  • the state of being curled is called a normal curl
  • the state of curling with the polarizer layer 5 side inward is called a reverse curl.
  • Curling becomes a problem in a polarizing plate when the polarizing plate is curled when the polarizing plate is bonded to a display cell such as a liquid crystal cell via an adhesive layer. That is, at the time of bonding to a display cell such as a liquid crystal cell, the polarizing plate is usually a composite polarizing plate because other peripheral members such as various films and layers are bonded. In this case, it is important to suppress curling.
  • a protective film for preventing scratches bonded on a protective film As a peripheral member, a protective film for preventing scratches bonded on a protective film; on a protective film (for example, a polarizing plate with a double-sided protective film) or on a polarizer layer (for example, a polarizing plate with a single-sided protective film) Adhesive layer for laminating a polarizing plate to a display cell or other optical member; a separate film laminated on the outer surface of the adhesive layer; on a protective film (for example, with a double-sided protective film) In the case of a polarizing plate) or on a polarizer layer (for example, in the case of a polarizing plate with a single-sided protective film), an optical compensation film such as a retardation film, or other optical functional film; laminated on a protective film Surface treatment layer and the like.
  • a protective film for example, a polarizing plate with a double-sided protective film
  • a polarizer layer for example,
  • the composite polarizing plate should be flat with no curling or slightly curled with the pressure-sensitive adhesive layer side of the composite polarizing plate as the outside (convex). Thereby, when bonding a composite polarizing plate to a display cell, it can suppress that a bubble mixes between an adhesive layer and a display cell, and produces a malfunction on display in a display device, or a bonding surface. It can suppress that the malfunction which a defect generate
  • the curl of the polarizing plate formed by laminating a protective film on at least one surface of the polarizer layer is corrected to the extent that it can be corrected by laminating peripheral members regardless of whether the curl is a normal curl or a reverse curl. It is preferable to make it small, and it is more preferable that it be as flat as possible. This can be realized according to the present invention.
  • the base film is peeled and removed after the protective film is bonded to the polarizer layer, the obtained polarizing plate tended to curl greatly in the reverse curl direction. In particular, this reverse curl can be effectively suppressed.
  • the base film 30 ′ is peeled and removed after the first protective film 10 having a moisture content higher than the equilibrium moisture content at 25 ° C. and 55% RH is bonded to the polarizer layer 5 of the polarizing laminated film 300.
  • the reason why reverse curl can be effectively suppressed by this method is presumed to be as follows. That is, the first protective film 10 having a moisture content higher than the equilibrium moisture content is slightly expanded in size at the time of bonding, and the first protective film 10 in this state is changed to the polarizer layer 5. When pasted to 25 ° C.
  • the moisture content of the 1st protective film 10 bonded on the polarizer layer 5 is 70% or less of the saturated moisture content, and it is more preferable that it is 60% or less.
  • the saturated moisture content is a moisture content obtained by immersing the first protective film 10 in 30 ° C. water for 3 hours and removing the surface adhering water, and the definition of the moisture content is as described above.
  • a method for preparing the first protective film 10 having a moisture content higher than the equilibrium moisture content at 25 ° C. and 55% RH is not particularly limited.
  • the protective film is placed in a humidity control tank capable of adjusting temperature and humidity for a certain period of time. The method of leaving it is mentioned.
  • a commercially available humidity control booth or air conditioning equipment can be used as the humidity control tank.
  • a method in which the moisture content is excessively increased once through a protective film in a water bath and then dried is also preferably used. Since this method can adjust the moisture content to a desired value in a short time, it is suitable for improving productivity in continuous production.
  • the water bath may simply be a tank for storing warm water, but it is preferable that the water bath temperature can be adjusted and the temperature can be kept constant.
  • a method of spraying steam on the protective film a method of spraying water mist by a spray method or the like; a method of applying water by a coater or the like may be employed.
  • the drying method is arbitrary, and examples thereof include drying using a so-called hot air drying furnace in which hot air is blown, drying using an infrared heater, and the like. It is also preferable to adjust the humidity in the drying furnace in order to suppress a rapid decrease in moisture content and perform drying mildly.
  • the material constituting the first protective film 10 is preferably a light-transmitting (preferably optically transparent) thermoplastic resin.
  • a resin include a chain polyolefin resin (polypropylene resin). Resins), polyolefin resins such as cyclic polyolefin resins (norbornene resins, etc.); cellulose ester resins such as cellulose triacetate and cellulose diacetate; polyester resins; polycarbonate resins; (meth) acrylic resins; Examples thereof include polystyrene resins; or mixtures and copolymers thereof.
  • the method of the present invention employs a means for adjusting the moisture content to a predetermined value based on the equilibrium moisture content of the protective film at 25 ° C. and 55% RH, thereby suppressing curling.
  • a protective film with high moisture permeability such as cellulose ester resin (for example, cellulose triacetate) or (meth) acrylic resin (for example, polymethyl methacrylate resin) is used, the dimensional difference due to the change in moisture content is large. The force for correcting in the positive curl direction is large, and the merit of the present invention is great.
  • the first protective film 10 can also be a protective film having an optical function such as a retardation film and a brightness enhancement film.
  • a retardation film provided with an arbitrary retardation value by stretching a film made of the thermoplastic resin (uniaxial stretching or biaxial stretching) or by forming a liquid crystal layer or the like on the film. It can be.
  • chain polyolefin resin examples include a homopolymer of a chain olefin such as a polyethylene resin and a polypropylene resin, and a copolymer composed of two or more chain olefins.
  • Cyclic polyolefin-based resin is a general term for resins that are polymerized using cyclic olefins as polymerization units.
  • Specific examples of cyclic polyolefin resins include ring-opening (co) polymers of cyclic olefins, addition polymers of cyclic olefins, copolymers of cyclic olefins and chain olefins such as ethylene and propylene (typically Are random copolymers), graft polymers obtained by modifying them with unsaturated carboxylic acids or derivatives thereof, and hydrides thereof.
  • norbornene resins using norbornene monomers such as norbornene and polycyclic norbornene monomers as cyclic olefins are preferably used.
  • the cellulose ester resin is an ester of cellulose and a fatty acid.
  • Specific examples of the cellulose ester resin include cellulose triacetate, cellulose diacetate, cellulose tripropionate, and cellulose dipropionate.
  • these copolymers and those in which a part of the hydroxyl group is modified with other substituents can also be used.
  • cellulose triacetate triacetyl cellulose: TAC is particularly preferable.
  • the polyester-based resin is a resin having an ester bond, and is generally made of a polycondensate of a polyvalent carboxylic acid or a derivative thereof and a polyhydric alcohol.
  • a polyvalent carboxylic acid or a derivative thereof a divalent dicarboxylic acid or a derivative thereof can be used, and examples thereof include terephthalic acid, isophthalic acid, dimethyl terephthalate, and dimethyl naphthalenedicarboxylate.
  • a divalent diol can be used, and examples thereof include ethylene glycol, propanediol, butanediol, neopentyl glycol, and cyclohexanedimethanol.
  • polyester resin examples include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polybutylene naphthalate, polytrimethylene terephthalate, polytrimethylene naphthalate, polycyclohexanedimethyl terephthalate, and polycyclohexanedimethyl naphthalate.
  • Polycarbonate resin is made of a polymer in which monomer units are bonded via a carbonate group.
  • the polycarbonate-based resin may be a resin called a modified polycarbonate having a modified polymer skeleton, a copolymer polycarbonate, or the like.
  • the (meth) acrylic resin is a resin containing a compound having a (meth) acryloyl group as a main constituent monomer.
  • Specific examples of the (meth) acrylic resin include, for example, poly (meth) acrylic acid esters such as polymethyl methacrylate; methyl methacrylate- (meth) acrylic acid copolymer; methyl methacrylate- (meth) acrylic acid Ester copolymer; methyl methacrylate-acrylate ester- (meth) acrylic acid copolymer; (meth) methyl acrylate-styrene copolymer (MS resin, etc.); methyl methacrylate and alicyclic hydrocarbon group And a copolymer with the compound (for example, methyl methacrylate-cyclohexyl methacrylate copolymer, methyl methacrylate- (meth) acrylate norbornyl copolymer, etc.).
  • a polymer based on a poly (meth) acrylic acid C 1-6 alkyl ester such as poly (meth) acrylic acid methyl is used, and more preferably methyl methacrylate is used as a main component (50 to 100). % Methyl methacrylate-based resin is used.
  • thermoplastic resin which comprises the base film 30.
  • a surface treatment layer such as a hard coat layer, an antiglare layer, an antireflection layer, an antistatic layer and an antifouling layer is formed on the surface of the first protective film 10 opposite to the polarizer layer 5.
  • the method for forming the surface treatment layer on the surface of the protective film is not particularly limited, and a known method can be used.
  • the thickness of the first protective film 10 is preferably thin from the viewpoint of reducing the thickness of the polarizing plate, but if it is too thin, the strength is lowered and the processability is poor. Accordingly, the thickness of the first protective film 10 is preferably 5 to 90 ⁇ m or less, more preferably 5 to 60 ⁇ m, and still more preferably 5 to 50 ⁇ m.
  • the first protective film 10 with the moisture content adjusted is on the polarizer layer 5 of the polarizing laminated film 300 via the adhesive layer 15 (the surface on the opposite side of the polarizer film 5 from the base film 30 ′). Is laminated.
  • the polarizing laminated film 300 has the polarizer layers 5 on both surfaces of the base film 30 ′, usually, protective films are bonded onto the polarizer layers 5 on both surfaces. In this case, these protective films may be the same type of protective film or different types of protective films.
  • the bonding surface of the first protective film 10 is subjected to plasma treatment, corona treatment, ultraviolet ray in order to improve the adhesion with the polarizer layer 5.
  • Surface treatment (easy adhesion treatment) such as irradiation treatment, flame (flame) treatment, and saponification treatment can be performed, and among them, plasma treatment, corona treatment or saponification treatment is preferable.
  • plasma treatment or corona treatment is usually performed.
  • a saponification process is normally performed.
  • the saponification treatment include a method of immersing in an alkaline aqueous solution such as sodium hydroxide or potassium hydroxide.
  • a water-based adhesive or a photocurable adhesive can be used as an adhesive used for bonding.
  • the water-based adhesive include an adhesive made of a polyvinyl alcohol-based resin aqueous solution, an aqueous two-component urethane emulsion adhesive, and the like.
  • a cellulose ester resin film that has been surface-treated (hydrophilized) by saponification treatment or the like is used as the first protective film 10
  • it is preferable to use a water-based adhesive comprising a polyvinyl alcohol-based resin aqueous solution.
  • Polyvinyl alcohol resins include vinyl alcohol homopolymers obtained by saponifying polyvinyl acetate, which is a homopolymer of vinyl acetate, and copolymers of vinyl acetate and other monomers copolymerizable therewith.
  • a polyvinyl alcohol copolymer obtained by saponifying the polymer or a modified polyvinyl alcohol polymer obtained by partially modifying the hydroxyl group thereof can be used.
  • the water-based adhesive can contain additives such as polyvalent aldehydes, water-soluble epoxy compounds, melamine compounds, zirconia compounds, and zinc compounds.
  • a water-based adhesive is applied to the bonding surface of the polarizer layer 5 and / or the first protective film 10 of the polarizing laminated film 300, and these films are bonded via the adhesive layer, preferably a bonding roll.
  • a pasting process is carried out by applying pressure and making close contact with each other.
  • the coating method of the water-based adhesive (same for the photo-curable adhesive) is not particularly limited, and casting method, Meyer bar coating method, gravure coating method, comma coater method, doctor plate method, die coating method, dip coating method A conventionally known method such as a spraying method can be used.
  • drying step for drying the film in order to remove water contained in the water-based adhesive after performing the above-mentioned bonding. Drying can be performed, for example, by introducing the film into a drying furnace.
  • the drying temperature is preferably 30 to 90 ° C. When the temperature is lower than 30 ° C., the first protective film 10 is easily peeled off from the polarizer layer 5. If the drying temperature exceeds 90 ° C., the polarization performance of the polarizer layer 5 may be deteriorated by heat.
  • a curing step for curing at room temperature or slightly higher temperature for example, a temperature of about 20 to 45 ° C. may be provided.
  • the curing temperature is generally set lower than the drying temperature.
  • a photocurable adhesive refers to an adhesive that cures by irradiating an active energy ray such as ultraviolet rays.
  • examples include those containing a resin and a photoreactive crosslinking agent.
  • the polymerizable compound include photopolymerizable monomers such as a photocurable epoxy monomer, a photocurable acrylic monomer, and a photocurable urethane monomer, and oligomers derived from the photopolymerizable monomer.
  • photoinitiator what contains the substance which generate
  • active species such as a neutral radical, an anion radical, and a cation radical by irradiation of active energy rays like an ultraviolet-ray
  • the photocurable adhesive containing a polymerizable compound and a photopolymerization initiator an adhesive containing a photocurable epoxy monomer and a photocationic polymerization initiator can be preferably used.
  • a drying process is performed as necessary (such as when the photocurable adhesive contains a solvent), and then light is irradiated by activating active energy rays.
  • a curing step for curing the curable adhesive is performed.
  • the light source of the active energy ray is not particularly limited, but an active energy ray having a light emission distribution at a wavelength of 400 nm or less is preferable.
  • the low-pressure mercury lamp, the medium-pressure mercury lamp, the high-pressure mercury lamp, the ultrahigh-pressure mercury lamp, the chemical lamp, and the black light lamp A microwave excited mercury lamp, a metal halide lamp, or the like is preferably used.
  • this process is a process which peels and removes base-material film 30 'after 1st protective film bonding process S10.
  • the polarizing plate 1 with a single-side protective film is obtained.
  • the polarizing laminated film 300 has the polarizer layers 5 on both surfaces of the base film 30 ′, and a protective film is bonded to both the polarizer layers 5, a single polarized light is obtained by the peeling step S 40.
  • the polarizing plate 1 with a single-sided protective film is obtained from the conductive laminated film 300.
  • the method for peeling and removing the base film 30 ′ is not particularly limited, and can be peeled by the same method as the peeling step of a separator (peeling film) performed with a normal pressure-sensitive adhesive polarizing plate.
  • Substrate film 30 ' may peel immediately as it is after 1st protective film bonding process S10, and after 1st protective film bonding process S10, it winds up in roll shape once, and winds in the subsequent process. You may peel off while taking out.
  • ⁇ 2nd protective film bonding process S30> With reference to FIG.3 and FIG.9, if this process of bonding the 2nd protective film 20 to the surface by the side of the polarizer layer 5 in the polarizing plate 1 with a single-sided protective film through the adhesive layer 25 is implemented, it will be double-sided.
  • the polarizing plate 2 with a protective film can be obtained.
  • the first protective film 10 and the second protective film 20 may be the same type of protective film or different types of protective films.
  • the adhesive layer 15 and the adhesive layer 25 may be formed of the same type of adhesive, or may be formed of different types of adhesive.
  • the moisture content was adjusted in the same manner as the first protective film 10, that is, when the second protective film 20 having a moisture content higher than the equilibrium moisture content at 25 ° C. and 55% RH was used.
  • the curl may be further improved.
  • the obtained polarizing plate 1 with a single-sided protective film and the polarizing plate 2 with a double-sided protective film are obtained by pasting peripheral members as exemplified above into a composite polarizing plate, or such a composite polarizing plate. Or can be used as
  • the pressure-sensitive adhesive layer as an example of the peripheral member can be laminated on the outer surface of any protective film in the polarizing plate 2 with a double-sided protective film. It can laminate
  • the pressure-sensitive adhesive forming the pressure-sensitive adhesive layer is usually based on a (meth) acrylic resin, styrene resin, silicone resin or the like, and a crosslinking agent such as an isocyanate compound, an epoxy compound, or an aziridine compound is added thereto. It consists of an adhesive composition. Furthermore, it can also be set as the adhesive layer which contains microparticles
  • the thickness of the pressure-sensitive adhesive layer is usually 1 to 40 ⁇ m, preferably 3 to 25 ⁇ m.
  • a reflective polarizing film that transmits a certain kind of polarized light and reflects polarized light that shows the opposite property; anti-glare having an uneven shape on the surface
  • a film with a function a film with a surface antireflection function; a reflection film having a reflection function on the surface; a transflective film having both a reflection function and a transmission function; and a viewing angle compensation film.
  • Example 1 (1) Primer layer forming step Polyvinyl alcohol powder (“Z-200” manufactured by Nippon Synthetic Chemical Industry Co., Ltd., average polymerization degree 1100, saponification degree 99.5 mol%) was dissolved in 95 ° C. hot water, A polyvinyl alcohol aqueous solution having a concentration of 3% by weight was prepared. The resulting aqueous solution was mixed with a crosslinking agent (“Smiles Resin 650” manufactured by Taoka Chemical Co., Ltd.) at a ratio of 5 parts by weight to 6 parts by weight of the polyvinyl alcohol powder to form a primer layer forming coating solution. Got.
  • a crosslinking agent (“Smiles Resin 650” manufactured by Taoka Chemical Co., Ltd.)
  • an unstretched polypropylene (PP) film (melting point: 163 ° C.) having a thickness of 110 ⁇ m is prepared as a base film, and after corona treatment is performed on one surface thereof, the above-described microgravure coater is used on the corona treatment surface.
  • the primer layer-forming coating solution was applied and dried at 80 ° C. for 10 minutes to form a primer layer having a thickness of 0.2 ⁇ m.
  • polarizing plate Preparation of polarizing plate (protective film bonding step and peeling step)
  • Polyvinyl alcohol powder (“KL-318” manufactured by Kuraray Co., Ltd., average polymerization degree 1800) was dissolved in 95 ° C. hot water to prepare an aqueous polyvinyl alcohol solution having a concentration of 3% by weight.
  • the resulting aqueous solution was mixed with a crosslinking agent (“Smile Resin 650” manufactured by Taoka Chemical Co., Ltd.) at a ratio of 1 part by weight to 2 parts by weight of the polyvinyl alcohol powder to obtain an aqueous adhesive solution.
  • a crosslinking agent (“Smile Resin 650” manufactured by Taoka Chemical Co., Ltd.)
  • the adhesive aqueous solution is applied to the outer surface (bonding surface) of the polarizer layer of the polarizing laminate film prepared in (4) above, and then left in an environment of 25 ° C. and 85% RH for 24 hours.
  • a protective film with adjusted moisture content [transparent protective film made of triacetylcellulose (TAC) (“KC4UY” manufactured by Konica Minolta Opto Co., Ltd.), thickness 40 ⁇ m] is bonded and passed between a pair of bonding rolls.
  • TAC triacetylcellulose
  • the adhesive layer was dried to obtain a polarizing laminated film with a protective film comprising base film / primer layer / polarizer layer / adhesive layer / protective film.
  • the equilibrium moisture content of the protective film at 25 ° C. and 55% RH is 1.08%.
  • the saturated moisture content of the protective film is 3.53%.
  • the base film was peeled and removed from the polarizing laminated film with a protective film.
  • the base film was easily peeled off to obtain a polarizing plate with a single-side protective film.
  • Example 2 A polarizing plate with a single-sided protective film was produced in the same manner as in Example 1 except that the protective film was left for 24 hours in an environment of 25 ° C. and 70% RH.
  • Example 1 A polarizing plate with a single-sided protective film was produced in the same manner as in Example 1 except that the protective film was left for 24 hours in an environment of 25 ° C. and 55% RH.
  • ⁇ Comparative example 2> A polarizing plate with a single-sided protective film was produced in the same manner as in Example 1 except that the protective film was left for 24 hours in an environment of 40 ° C. and 55% RH.
  • Table 1 shows the moisture content (wt / wt%) when the protective film used in each Example / Comparative Example was bonded to the polarizer layer together with the humidity control conditions of the protective film.
  • the moisture content was determined based on the above-described calculation formula.
  • A The curl amount is less than 28 mm, and the curling of the polarizing plate is sufficiently suppressed.
  • B The curl amount is 28 mm or more, and the curling of the polarizing plate is remarkable.
  • the above evaluation criteria are for the following reasons.
  • a protective film polyethylene terephthalate film with an adhesive layer
  • a substantially flat composite polarizing plate is obtained. I was able to. Furthermore, even if the adhesive layer for bonding to a liquid crystal cell was bonded to the outer surface of the polarizer layer of the composite polarizing plate, the composite polarizing plate was kept almost flat.
  • the obtained composite polarizing plate was curled in the reverse curl direction even when the protective film was bonded to the outer surface of the protective film. Furthermore, even if the adhesive layer for bonding to a liquid crystal cell was bonded to the outer surface of the polarizer layer of the composite polarizing plate, the reverse curled state was maintained. Moreover, when it was left to stand in an environment of 23 ° C. and 55% RH for several days and observed again, there was a problem that reverse curl was further increased.
  • Polarizing plate with single-sided protective film 2. Polarizing plate with double-sided protective film, 5. Polarizer layer, 6. Polyvinyl alcohol-based resin layer, 6 'stretched polyvinyl alcohol-based resin layer, 10. First protective film, 15, 25 adhesive. Layer, 20 second protective film, 30 base film, 30 ′ stretched base film, 100 laminated film, 200 stretched film, 300 polarizing laminated film, 400 polarizing laminated film with protective film.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Polarising Elements (AREA)

Abstract

L'invention concerne un procédé de fabrication de plaque de polarisation qui comprend, dans l'ordre, les étapes suivantes : une étape consistant à faire adhérer un film de protection, qui a été ajusté de sorte à présenter un taux de reprise d'humidité qui est plus élevé que le taux de reprise d'humidité d'équilibre à une température de 25 °C et à un taux d'humidité relative de 55 %, à une couche de polarisation dans un film de polarisation stratifié obtenu par agencement d'une couche de polarisation sur au moins une surface d'un film de base, une couche adhésive étant intercalée entre ces derniers ; et une étape consistant à détacher et à enlever le film de base.
PCT/JP2015/054386 2014-03-06 2015-02-18 Procédé de fabrication de plaque de polarisation WO2015133269A1 (fr)

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JP5951870B1 (ja) * 2015-05-26 2016-07-13 住友化学株式会社 偏光板の製造方法
JP6566993B2 (ja) * 2017-06-02 2019-08-28 日東電工株式会社 偏光フィルムおよび画像表示装置
CN107300729A (zh) * 2017-08-28 2017-10-27 宁波维真显示科技股份有限公司 高洁净度光学薄膜保护方法
JP7169160B2 (ja) * 2018-10-26 2022-11-10 住友化学株式会社 液晶層積層体

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JP2009093074A (ja) 2007-10-11 2009-04-30 Nitto Denko Corp 偏光板の製造方法、偏光板、光学フィルムおよび画像表示装置
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JP2006030480A (ja) * 2004-07-14 2006-02-02 Nitto Denko Corp 偏光板の製造方法、それにより得られる偏光板、およびそれを用いた画像表示装置
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KR20160130225A (ko) 2016-11-10
JP6302293B2 (ja) 2018-03-28
CN106062595A (zh) 2016-10-26
TW201539065A (zh) 2015-10-16
KR101942166B1 (ko) 2019-01-24
CN106062595B (zh) 2018-11-13

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