WO2018164176A1 - 偏光フィルム、偏光板、及びそれらの製造方法 - Google Patents

偏光フィルム、偏光板、及びそれらの製造方法 Download PDF

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WO2018164176A1
WO2018164176A1 PCT/JP2018/008738 JP2018008738W WO2018164176A1 WO 2018164176 A1 WO2018164176 A1 WO 2018164176A1 JP 2018008738 W JP2018008738 W JP 2018008738W WO 2018164176 A1 WO2018164176 A1 WO 2018164176A1
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Prior art keywords
film
polarizing film
pva
polarizing
stretching
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PCT/JP2018/008738
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English (en)
French (fr)
Japanese (ja)
Inventor
達也 大園
辻　嘉久
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株式会社クラレ
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Priority to CN201880016626.8A priority Critical patent/CN110352369B/zh
Priority to KR1020197028377A priority patent/KR102595403B1/ko
Priority to JP2019504633A priority patent/JP7234105B2/ja
Publication of WO2018164176A1 publication Critical patent/WO2018164176A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
    • B29C55/06—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique parallel with the direction of feed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/30—Polarising elements
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors

Definitions

  • the present invention relates to a polarizing film, a polarizing plate, and a method for producing them, which are excellent in the balance between the polarizing performance and hue of a polyvinyl alcohol film containing an iodine-based dichroic dye, and shrinkage stress.
  • a polarizing film used for a polarizing plate having a light transmission and shielding function is a basic component of a liquid crystal display (LCD).
  • LCD liquid crystal display
  • Many polarizing plates have a structure in which a protective film such as a cellulose triacetate (TAC) film is bonded to the surface of a polarizing film.
  • a polarizing film constituting the polarizing plate a polyvinyl alcohol film (hereinafter referred to as “polyvinyl”).
  • alcohol "and” PVA "and that there is referred) uniaxially stretched iodine to stretched film was oriented dye (I 3 - and I 5 -, etc.) dichroic dye to what has mainstream adsorption of such It has become.
  • Such a polarizing film is manufactured by a method of subjecting a PVA film to a swelling process, a dyeing process, a crosslinking process, a stretching process, an immobilizing process, and a drying process.
  • LCDs are widely used in mobile applications such as notebook computers and mobile phones. Such LCDs for mobile devices are used in various environments. Therefore, there is a demand for a polarizing film that has low shrinkage stress at high temperatures and excellent dimensional stability.
  • Patent Documents 1 to 5 describe polarizing films obtained by stretching a PVA film dyed with an iodine-based dye and then drying at 50 to 70 ° C. for 2 to 4 minutes.
  • the polarizing film thus obtained had high shrinkage stress.
  • the polarizing film contracts and the glass plate warps. It was.
  • the present invention has been made to solve the above-described problems, and an object of the present invention is to provide a polarizing film excellent in the balance between polarization performance and hue and shrinkage stress, and a method for producing the same. Moreover, it aims at providing the polarizing plate using such a polarizing film, and its manufacturing method.
  • An object of the present invention is to provide a polarizing film made of a PVA film containing an iodine dichroic dye, having a polarization degree of 99.5% or more and satisfying the following formulas (1) and (2) It is solved by doing.
  • A is the shrinkage stress (N / mm 2 ) of the polarizing film heated at 80 ° C. for 4 hours
  • B is the simple substance b value of the polarizing film.
  • B is 1.0 or more. It is also preferable that the degree of polymerization of the PVA is 1,500 to 6,000. It is also preferable that the polarizing film has a thickness of 1 to 30 ⁇ m. It is also preferable that the shrinkage stress A is 15 to 35 N / mm 2 .
  • the object is to perform an annealing treatment step of heating the PVA film having a fixed stretching direction at 70 to 90 ° C. for 120 minutes or more after performing the step of dyeing the PVA film with an iodine dichroic dye and the step of stretching. It is also solved by providing a method for producing the polarizing film.
  • a polarizing plate formed by laminating the polarizing film and the protective film is a preferred embodiment of the present invention. After performing the step of dyeing the PVA film with an iodine dichroic dye and the step of stretching, the PVA film and the protective film are laminated to obtain a multilayer film, and the multilayer film in which the stretching direction is fixed is 70.
  • a method for producing the polarizing plate in which an annealing treatment step of heating at 90 ° C. for 120 minutes or more is also a preferred embodiment of the present invention.
  • the polarizing film of the present invention has good polarization performance and hue, and has small shrinkage stress and excellent dimensional stability. Therefore, the polarizing plate using the polarizing film is suitably used for high-performance LCDs, particularly LCDs used at high temperatures. Moreover, according to the manufacturing method of this invention, such a polarizing film and a polarizing plate can be manufactured simply.
  • FIG. 6 is a graph plotting the contraction stress A and the simple substance b value B of polarizing films in Examples 1 to 3 and Comparative Examples 3 to 5 and 7 to 9.
  • FIG. 6 is a diagram plotting the shrinkage stress A and the simple substance b value B of the polarizing films in Examples 1 to 3, Comparative Examples 1 to 5 and 7 to 12, and Reference Example 1.
  • the polarizing film of the present invention is a polarizing film made of a PVA film containing an iodine dichroic dye, having a polarization degree of 99.5% or more and satisfying the following formulas (1) and (2): It is. B ⁇ 3.0 (1) B + 0.035A ⁇ 3.9 (2)
  • A is the shrinkage stress (N / mm 2 ) of the polarizing film heated at 80 ° C. for 4 hours
  • B is the simple substance b value of the polarizing film.
  • the polarizing film of the present invention solves these points, and is characterized by low shrinkage stress while maintaining good polarization performance and hue.
  • the manufacturing method of such a polarizing film is not particularly limited, but the present inventor succeeded in manufacturing a polarizing film having such performance for the first time by adopting a new manufacturing method. Specifically, after performing a step of dyeing a PVA film with an iodine dichroic dye and a step of stretching, an annealing treatment step of heating the PVA film in which the stretching direction is fixed at 70 to 90 ° C. for 120 minutes or more. By carrying out the above, it is possible to produce a polarizing film having good polarizing performance and hue, having a small shrinkage stress and excellent dimensional stability.
  • the said manufacture is used suitably for manufacture of various polarizing films including the polarizing film of this invention.
  • the manufacturing method will be described in detail.
  • the PVA contained in the raw PVA film used in the production of the polarizing film of the present invention should be obtained by saponifying a polyvinyl ester obtained by polymerizing one or more vinyl esters.
  • a polyvinyl ester obtained by polymerizing one or more vinyl esters.
  • the vinyl ester include vinyl acetate, vinyl formate, vinyl propionate, vinyl butyrate, vinyl pivalate, vinyl versatate, vinyl laurate, vinyl stearate, vinyl benzoate, and isopropenyl acetate.
  • vinyl acetate is preferable from the viewpoint of ease of production, availability, and cost of PVA.
  • the polyvinyl ester may be obtained using only one or two or more kinds of vinyl esters as a monomer, but one or two as long as the effects of the present invention are not impaired. It may be a copolymer of at least one kind of vinyl ester and another monomer copolymerizable therewith.
  • Examples of other monomers copolymerizable with the vinyl ester include ⁇ -olefins having 2 to 30 carbon atoms such as ethylene, propylene, 1-butene and isobutene; (meth) acrylic acid or a salt thereof; (meth) Methyl acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, i-propyl (meth) acrylate, n-butyl (meth) acrylate, i-butyl (meth) acrylate, (meth) (Meth) acrylic acid esters such as t-butyl acrylate, 2-ethylhexyl (meth) acrylate, dodecyl (meth) acrylate, octadecyl (meth) acrylate; (meth) acrylamide, N-methyl (meth) Acrylamide, N-ethyl (meth) acrylamide, N, N-
  • the proportion of structural units derived from other monomers in the polyvinyl ester is preferably 15 mol% or less, preferably 10 mol% or less, based on the number of moles of all structural units constituting the polyvinyl ester. More preferred is 5 mol% or less.
  • the other monomer is a monomer that may promote water solubility of the obtained PVA, such as (meth) acrylic acid or unsaturated sulfonic acid
  • the polarizing film In order to prevent PVA from being dissolved in the production process, the proportion of structural units derived from these monomers in the polyvinyl ester is 5 mol% or less based on the number of moles of all structural units constituting the polyvinyl ester. It is preferable that it is 3 mol% or less.
  • the PVA used in the present invention may be modified with one or two or more types of graft copolymerizable monomers as long as the effects of the present invention are not impaired.
  • examples of the graft copolymerizable monomer include unsaturated carboxylic acids or derivatives thereof; unsaturated sulfonic acids or derivatives thereof; ⁇ -olefins having 2 to 30 carbon atoms, and the like.
  • the proportion of structural units derived from the graft copolymerizable monomer in PVA (structural units in the graft modified portion) is preferably 5 mol% or less based on the number of moles of all structural units constituting PVA. .
  • a part of the hydroxyl group may be cross-linked or may not be cross-linked.
  • said PVA may react with aldehyde compounds, such as acetaldehyde and a butyraldehyde, etc., and a part of the hydroxyl group may form the acetal structure.
  • the polymerization degree of the PVA is preferably in the range of 1500 to 6000, more preferably in the range of 1800 to 5000, and still more preferably in the range of 2000 to 4000.
  • the degree of polymerization of PVA in the present specification means an average degree of polymerization measured according to the description of JIS K6726-1994.
  • PVA in a polarizing film contains the crosslinked structure by boron compounds, such as a boric acid, if it dissociates by hydrolyzing boric acid ester etc., it will be a substantial change in the average degree of polymerization of PVA itself. There is no.
  • the degree of saponification of PVA is preferably 98 mol% or more, more preferably 98.5 mol% or more, and further preferably 99 mol% or more from the viewpoint of the polarizing performance of the polarizing film.
  • the degree of saponification is less than 98 mol%, PVA tends to be eluted during the production process of the polarizing film, and the eluted PVA may adhere to the film and reduce the polarizing performance of the polarizing film.
  • the degree of saponification of PVA refers to the total number of moles of structural units (typically vinyl ester units) that can be converted into vinyl alcohol units by saponification and the vinyl alcohol units of PVA.
  • the degree of saponification can be measured according to the description of JIS K6726-1994.
  • PVA in a raw film and PVA in the obtained polarizing film have substantially the same saponification degree.
  • a PVA film is formed using the stock solution.
  • the film forming method include a cast film forming method, an extrusion film forming method, a wet film forming method, and a gel film forming method. These film forming methods may be used alone or in combination of two or more. Among these film forming methods, the cast film forming method and the extrusion film forming method are preferable because a PVA film having uniform thickness and width and good physical properties can be obtained.
  • the formed PVA film can be dried or heat-treated as necessary.
  • the film-forming stock solution can be obtained, for example, by mixing a liquid medium with one or more of the PVA and, if necessary, a surfactant, a plasticizer and an additive.
  • PVA may be in a dissolved state in a liquid medium or in a molten state. The mixing is preferably performed under heating.
  • liquid medium used for the preparation of the membrane forming stock solution examples include water, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, N-methylpyrrolidone, ethylene glycol, glycerin, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol. , Trimethylolpropane, ethylenediamine, diethylenetriamine and the like, and one or more of them can be used. Among these, water is preferable from the viewpoint of environmental load and recoverability.
  • the volatile fraction of the film-forming stock solution (content ratio in the film-forming stock solution of volatile components such as liquid media removed by volatilization or evaporation during film formation) varies depending on the film-forming method, film-forming conditions, etc. Specifically, it is preferably in the range of 50 to 95% by mass, more preferably in the range of 55 to 90% by mass, and still more preferably in the range of 60 to 85% by mass.
  • the volatile fraction of the film-forming stock solution is 50% by mass or more, the viscosity of the film-forming stock solution does not become too high, and filtration and defoaming are smoothly performed during preparation of the film-forming stock solution, and there are few foreign matters and defects. Film production is facilitated.
  • the volatile fraction of the film-forming stock solution is 95% by mass or less, the concentration of the film-forming stock solution does not become too low, and the production of an industrial PVA film becomes easy.
  • the film forming stock solution preferably contains a surfactant.
  • a surfactant By including the surfactant, the film-forming property is improved and the occurrence of uneven thickness of the film is suppressed, and the film is easily peeled off from the metal roll or belt used for film formation.
  • the PVA film may contain a surfactant.
  • the kind of said surfactant is not specifically limited, From a viewpoint of the peelability from a metal roll or a belt, an anionic surfactant or a nonionic surfactant is preferable.
  • anionic surfactant for example, a carboxylic acid type such as potassium laurate; a sulfuric acid ester type such as polyoxyethylene lauryl ether sulfate and octyl sulfate; and a sulfonic acid type such as dodecylbenzene sulfonate are suitable.
  • a carboxylic acid type such as potassium laurate
  • a sulfuric acid ester type such as polyoxyethylene lauryl ether sulfate and octyl sulfate
  • a sulfonic acid type such as dodecylbenzene sulfonate
  • Nonionic surfactants include, for example, alkyl ether types such as polyoxyethylene oleyl ether; alkylphenyl ether types such as polyoxyethylene octylphenyl ether; alkyl ester types such as polyoxyethylene laurate; polyoxyethylene laurylamino Alkylamine type such as ether; alkylamide type such as polyoxyethylene lauric acid amide; polypropylene glycol ether type such as polyoxyethylene polyoxypropylene ether; alkanolamide type such as lauric acid diethanolamide and oleic acid diethanolamide; polyoxy An allyl phenyl ether type such as alkylene allyl phenyl ether is preferred.
  • surfactants can be used alone or in combination of two or more.
  • the content thereof is preferably 0.01 to 0.5 parts by weight, preferably 0.02 to 0.00 parts, per 100 parts by weight of PVA contained in the film-forming stock solution.
  • the amount is more preferably 3 parts by mass, and particularly preferably 0.05 to 0.1 parts by mass.
  • the content is 0.01 parts by mass or more, the film forming property and the peelability are further improved.
  • the content is 0.5 parts by mass or less, it is possible to prevent the surfactant from bleeding out on the surface of the PVA film to cause blocking and deterioration in handleability.
  • the content of PVA in the raw PVA film used in the present invention is preferably 50 to 99% by mass from the viewpoint of ease of production of the polarizing film.
  • the content is more preferably 75% by mass or more, further preferably 80% by mass or more, and particularly preferably 85% by mass or more.
  • the content is more preferably 98% by mass or less, further preferably 96% by mass or less, and particularly preferably 95% by mass or less.
  • the PVA film preferably contains a plasticizer.
  • the plasticizer include polyhydric alcohols such as ethylene glycol, glycerin, propylene glycol, diethylene glycol, diglycerin, triethylene glycol, tetraethylene glycol, and trimethylol propane.
  • One or more of the agents can be included. Among these, glycerin is preferable from the viewpoint of the effect of improving stretchability.
  • the content of the plasticizer in the PVA film is preferably 1 to 20 parts by mass with respect to 100 parts by mass of PVA.
  • the content is more preferably 2 parts by mass or more, further preferably 4 parts by mass or more, and particularly preferably 5 parts by mass or more. Further, the content is more preferably 15 parts by mass or less.
  • the PVA film may further contain components such as an antioxidant, an antifreezing agent, a pH adjuster, a hiding agent, an anti-coloring agent, an oil agent, and a surfactant as necessary.
  • the thickness of the PVA film is preferably 5 to 100 ⁇ m. When the thickness is 100 ⁇ m or less, a thin polarizing film can be easily obtained. The thickness is more preferably 60 ⁇ m or less. On the other hand, when the thickness is less than 5 ⁇ m, it may be difficult to produce a polarizing film, and uneven staining may easily occur.
  • the thickness of the PVA film is more preferably 7 ⁇ m or more. The thickness here refers to the thickness of the PVA layer in the case of a multilayer film.
  • the PVA film may be a single layer film or a multilayer film having a PVA layer and a base resin layer.
  • the film thickness is preferably 20 ⁇ m or more in order to ensure handling.
  • the thickness of the PVA layer can be 20 ⁇ m or less, or 15 ⁇ m or less.
  • the thickness of the base resin layer in the multilayer film is usually 20 to 500 ⁇ m.
  • the base resin When using a multilayer film having a PVA layer and a base resin layer as the PVA film, the base resin must be capable of being stretched together with PVA.
  • Polyester, polyolefin resin, or the like can be used.
  • an amorphous polyester resin is preferable, and an amorphous polyester resin obtained by copolymerizing polyethylene terephthalate and a copolymer component such as isophthalic acid or 1,4-cyclohexanedimethanol is preferably used.
  • the surface of the base resin film may be modified, or an adhesive layer may be formed between both layers.
  • the shape of the PVA film is not particularly limited, but is preferably a long PVA film because it can be continuously supplied when a polarizing film is produced.
  • the length of the long PVA film (length in the long direction) is not particularly limited, and can be set as appropriate according to the application of the polarizing film to be produced, for example, within a range of 5 to 20000 m. be able to.
  • the width of the PVA film is not particularly limited, and can be appropriately set according to the use of the polarizing film to be produced. In recent years, since the enlargement of screens of liquid crystal televisions and liquid crystal monitors has progressed, it is suitable for these applications when the width of the PVA film is 0.5 m or more, more preferably 1.0 m or more. On the other hand, if the width of the PVA film is too wide, it tends to be difficult to uniformly stretch the polarizing film when the polarizing film is produced by a device that has been put to practical use. Therefore, the width of the PVA film is 7 m or less. Is preferred.
  • the polarizing film of the present invention is produced using the PVA film described above as a raw fabric. Specifically, the step of dyeing the PVA film with an iodine dichroic dye (hereinafter sometimes referred to as “dyeing step”) and the step of stretching the PVA film (hereinafter referred to as “stretching step”). It is preferable to manufacture a polarizing film by a method of performing an annealing treatment step of heating the PVA film having a fixed stretching direction at 70 to 90 ° C. for 120 minutes or more.
  • a step of swelling the original PVA film (hereinafter, sometimes referred to as “swelling step”) before performing the above steps.
  • an annealing treatment step after performing a step of crosslinking the PVA film using a crosslinking agent (hereinafter sometimes referred to as “crosslinking step”).
  • crosslinking treatment step After performing the dyeing step and the stretching step, it is also preferable to perform an annealing treatment step after further performing a step of fixing the PVA film (hereinafter sometimes referred to as “fixing treatment step”).
  • drying step After performing the dyeing step and the stretching step, it is also preferable to further perform an annealing treatment step after performing a step of drying the PVA film (hereinafter sometimes referred to as “drying step”). Prior to the drying step, a step of appropriately washing the PVA film may be performed. Moreover, in the said manufacturing method, you may perform one type of process in multiple times. Moreover, you may perform a several process simultaneously in one bath.
  • a method of performing the dyeing step, the stretching step, and the annealing treatment step in this order is preferable, and a method of performing the dyeing step, the crosslinking step, the stretching step, and the annealing treatment step in this order is more preferable, and the swelling step, the dyeing step. More preferably, the crosslinking step, the stretching step, the fixing treatment step, the drying step and the annealing treatment step are carried out in this order.
  • each step will be described in detail.
  • the manufacturing method it is preferable to first perform a step of swelling the original PVA film.
  • the PVA film is swollen by dipping in water at 10 to 50 ° C.
  • the temperature of the water is preferably 20 ° C. or higher, and more preferably 40 ° C. or lower.
  • the time for immersing the PVA film in water is preferably 0.1 to 5 minutes, and more preferably 0.5 to 3 minutes. By setting it as such immersion time, a PVA film can be efficiently swollen uniformly.
  • the water in which the PVA film is immersed is not limited to pure water, and may be an aqueous solution in which various components are dissolved, or a mixture of water and a water-soluble organic solvent.
  • a step of dyeing the PVA film with an iodine dichroic dye is performed. It is preferable to perform the dyeing process after the swelling process. Moreover, although the dyeing
  • the dyeing process is generally performed by immersing the PVA film in a solution (particularly an aqueous solution) containing iodine-potassium iodide as a dyeing bath. In the present invention, such a dyeing method is suitably employed.
  • the iodine concentration in the dyeing bath is preferably 0.01 to 0.5% by mass, and the potassium iodide concentration is preferably 0.01 to 10% by mass.
  • the temperature of the dyeing bath is preferably 10 to 50 ° C., more preferably 20 to 40 ° C.
  • the time for immersing the PVA film in the dyeing bath is preferably 0.1 to 10 minutes, more preferably 0.2 to 5 minutes.
  • the dyeing bath may contain a boron compound, but its content is usually less than 5% by mass, preferably 1% by mass or less, in terms of boric acid. As said boron compound, what is mentioned later as what is used for a bridge
  • the production method it is preferable to perform a step of crosslinking the PVA film using a crosslinking agent.
  • a crosslinking step for crosslinking By subjecting the PVA film to a crosslinking step for crosslinking, it is possible to effectively prevent PVA from eluting into water when wet-stretching at a high temperature.
  • the crosslinking step is preferably performed before the stretching step.
  • crosslinking process after a dyeing process it is preferable to perform a bridge
  • the crosslinking treatment can be performed by immersing the PVA film in an aqueous solution containing a crosslinking agent.
  • the crosslinking agent one or more of boron compounds such as boric acid and borate such as borax can be used.
  • the concentration of the crosslinking agent in the aqueous solution containing the crosslinking agent is preferably 1 to 15% by mass, and more preferably 2 to 7% by mass. Sufficient stretchability can be maintained when the concentration of the crosslinking agent is 1 to 15% by mass.
  • the aqueous solution containing a crosslinking agent may contain an auxiliary agent such as potassium iodide.
  • the temperature of the aqueous solution containing the cross-linking agent is preferably 20 to 50 ° C., particularly 25 to 40 ° C. By setting the temperature to 20 to 50 ° C., crosslinking can be performed efficiently.
  • the PVA film may be stretched during or between the above-described processes. By performing such stretching (pre-stretching), wrinkles can be prevented from entering the PVA film.
  • the total stretching ratio of pre-stretching (the ratio obtained by multiplying the stretching ratios in each step) is 4 based on the polarization performance in the case of producing a polarizing film. It is preferable that it is less than 2 times.
  • the draw ratio in the swelling process is preferably 1.05 to 3 times, the draw ratio in the dyeing process is preferably 3 times or less, and the draw ratio in the crosslinking process is preferably 2 times or less.
  • a step of stretching the PVA film is performed.
  • the stretching step can be performed by uniaxially stretching the PVA film using a wet stretching method or a dry stretching method.
  • a wet stretching method it can be carried out in an aqueous solution containing a boron compound, or can be carried out in the above-described dyeing bath or crosslinking bath.
  • a boron compound what was mentioned above as what is used for a bridge
  • the stretching may be performed at room temperature, may be performed while heating, or may be performed in the air using a PVA film after water absorption.
  • the wet stretching method is preferable, and it is more preferable to perform uniaxial stretching in an aqueous solution containing a boron compound.
  • concentration of the boron compound in the aqueous solution of the boron compound is preferably 0.5 to 6.0% by mass in terms of boric acid, more preferably 1.0 to 5.0% by mass, and 1.5 to 4.5% by mass. Particularly preferred.
  • the aqueous solution may contain potassium iodide, and the concentration is preferably 0.01 to 10% by mass.
  • the temperature at which the PVA film is stretched in the stretching step is preferably 30 to 90 ° C, more preferably 40 to 80 ° C, and even more preferably 50 to 70 ° C.
  • the draw ratio in the drawing step is preferably 1.2 times or more, more preferably 1.5 times or more, and 2 times or more. Is more preferable.
  • the total draw ratio including the draw ratio of the above-mentioned pre-stretch (the ratio obtained by multiplying the stretch ratio in each step) is 5.2 times or more based on the original length of the original PVA film before stretching. Preferably, it is 5.5 times or more, more preferably 5.8 times or more.
  • the upper limit of the total stretching ratio is not particularly limited, but the stretching ratio is preferably 8 times or less in order to prevent stretching.
  • uniaxial stretching in the longitudinal direction is preferable from the viewpoint of obtaining a film having excellent polarizing performance.
  • Uniaxial stretching in the longitudinal direction can be performed by changing the peripheral speed between the rolls using a stretching apparatus including a plurality of rolls parallel to each other.
  • lateral uniaxial stretching can be performed using a tenter type stretching machine.
  • the fixing treatment bath used for the fixing treatment an aqueous solution containing one or more of boron compounds can be used.
  • the boron compound those described above as being used for the crosslinking treatment can be used. it can.
  • the concentration of the boron compound in the fixing treatment bath is preferably 1 to 15% by mass.
  • the concentration of the boron compound is more preferably 10% by mass or less. When potassium iodide is contained in the aqueous solution, the concentration is preferably 0.01 to 10% by mass.
  • the temperature of the fixing treatment bath is preferably 15 to 60 ° C, and more preferably 20 to 40 ° C.
  • the drying temperature is preferably 30 ° C or higher, more preferably 40 ° C or higher, and further preferably 50 ° C or higher.
  • the drying temperature is preferably 90 ° C. or lower, and more preferably 85 ° C. or lower.
  • the drying time is preferably 10 seconds or more, more preferably 30 seconds or more, and further preferably 1 minute or more.
  • the drying time is preferably 30 minutes or less, more preferably 15 minutes or less, further preferably 10 minutes or less, and particularly preferably 5 minutes or less.
  • the drying step is preferably performed in a gas such as air or an inert gas, and the former is more preferable from the viewpoint of simple treatment.
  • the humidity at the time of performing a drying process in the air is not specifically limited, It is preferable that relative humidity is 35% or less, and it is more preferable that it is 15% or less.
  • an annealing process step of heating at 70 to 90 ° C. for 120 minutes or more is performed.
  • the degree of polarization of the PVA film subjected to the annealing process is 99.7% or more.
  • the single b value of the PVA film subjected to the annealing treatment step is 2.8 or less.
  • the drying process and the annealing process may be performed for a total of 120 minutes or more.
  • the PVA film roll needs to be annealed for 120 minutes or more.
  • the moisture content of the PVA film used in the step is 1 to 25 mass%.
  • the moisture content is more preferably 20% by mass or less, and further preferably 15% by mass or less.
  • the annealing process it is necessary to anneal the PVA film with the stretching direction fixed.
  • the method at this time is not particularly limited, and after winding the PVA film in the stretching direction to obtain a film roll, the method of heating the film roll or the end of the PVA film in the stretching direction was fixed with a clip or the like. A method of annealing, etc. is adopted later, and the former is preferable from the viewpoint of productivity.
  • the annealing process is performed at 70 to 90 ° C.
  • the shrinkage stress can be reduced while maintaining good polarization performance and hue of the PVA film.
  • the temperature is preferably 75 ° C. or higher.
  • the said temperature exceeds 90 degreeC, the polarization performance and hue of the said PVA film will fall.
  • the temperature is preferably 85 ° C. or lower.
  • the annealing process is preferably performed in a gas such as air or an inert gas, and the former is more preferable from the viewpoint of simple processing.
  • the humidity when the annealing process is performed in air is not particularly limited, but the relative humidity is preferably 35% or less, and more preferably 15% or less.
  • the PVA film is heated for 120 minutes or more.
  • the shrinkage stress can be lowered while maintaining the good polarization performance and hue of the PVA film.
  • the heating time is preferably 240 minutes or more.
  • the heating time is preferably 500 minutes or more, more preferably 1000 minutes or more, and further preferably 2000 minutes or more.
  • the heating time is preferably 5000 minutes or less, and more preferably 3500 minutes or less.
  • the heating time is preferably 2500 minutes or less, and more preferably 1000 minutes or less.
  • the inventors examined the annealing treatment of the polarizing film. Although the shrinkage stress is reduced by increasing the treatment temperature, Performance and hue deteriorated, making it difficult to achieve both. As a result of further investigations, the present inventors have surprisingly been able to reduce the shrinkage stress while maintaining excellent polarization performance and hue by annealing at 70 to 90 ° C. for 120 minutes or more. I found out that I can do it. Although this mechanism is not clear, annealing the PVA film under the above conditions contributes to the above effect by suppressing the decomposition of the pigment and PVA and relaxing the amorphous part that is stretched more than necessary. It is considered a thing.
  • the polarization degree of the polarizing film of the present invention needs to be 99.5% or more.
  • Such a polarizing film having a high degree of polarization is suitably used in LCDs and the like.
  • the polarization degree is preferably 99.6% or more, and more preferably 99.7% or more.
  • the polarizing film needs to satisfy the following formula (1).
  • B is a single b value of the polarizing film.
  • the polarizing film of the present invention having a low simple substance b value B and excellent hue is suitably used in LCDs and the like.
  • the simple substance b value B is preferably 2.8 or less.
  • the single b value B is usually 0 or more.
  • the simple substance b value B is preferably 1.0 or more.
  • the polarizing film needs to satisfy the following formula (2).
  • A is the contraction stress (N / mm ⁇ 2 >) of the said polarizing film heated at 80 degreeC for 4 hours
  • B is synonymous with the said Formula (1).
  • FIG. 1 is a diagram plotting the contraction stress A and the simple substance b value B of the polarizing film obtained in Examples described later.
  • the present inventors have studied an annealing method. When the annealing temperature was increased until the shrinkage stress A was sufficiently reduced, the simple substance b value B increased and the hue deteriorated, making it difficult to achieve both [Comparative Examples 3 to 5 (120 ° C. , 60-360 minutes), 7-9 (100 ° C., 60-360 minutes)].
  • the shrinkage stress A of the polarizing film is preferably 15 to 35 N / mm 2 .
  • the shrinkage stress A is less than 15 N / mm 2 , the polarization performance may be deteriorated.
  • Shrinkage stress A is more preferably 20 N / mm 2 or more, more preferably 23N / mm 2 or more, 28N / mm 2 or more is particularly preferable.
  • the shrinkage stress A exceeds 35 N / mm 2 , the glass plate may be warped when the polarizing film is used in an LCD.
  • the shrinkage rate of the polarizing film heated at 80 ° C. for 4 hours is preferably 1 to 1.3%.
  • the shrinkage rate is less than 1%, the polarization performance may be insufficient.
  • the shrinkage rate is more preferably 1.1% or more, and further preferably 1.2% or more.
  • the shrinkage rate exceeds 1.3%, the dimensional stability is lowered, and when the polarizing film is used for an LCD, the warpage of the glass plate may be increased.
  • the methods described in Examples described later are employed.
  • the contraction stress A and the contraction rate are measured in the stretching direction of the polarizing film, and when stretching in a plurality of directions, the measurement is performed in the direction in which the stretching ratio is high.
  • the thickness of the polarizing film is preferably 1 to 30 ⁇ m. Such a thin polarizing film is suitably used for LCDs such as LCDs, especially for mobile devices. When the thickness is less than 1 ⁇ m, it may be difficult to produce a polarizing film, and uneven dyeing may easily occur.
  • the thickness is preferably 5 ⁇ m or more. On the other hand, the thickness is more preferably 20 ⁇ m or less.
  • the content of PVA in the polarizing film is preferably 50 to 99% by mass.
  • the content is more preferably 75% by mass or more, further preferably 80% by mass or more, and particularly preferably 85% by mass or more.
  • it is more preferable that it is 98 mass% or less, it is more preferable that it is 96 mass% or less, and it is especially preferable that it is 95 mass% or less.
  • a polarizing plate formed by laminating the polarizing film and the protective film is a preferred embodiment of the present invention.
  • the polarizing plate using the polarizing film has excellent polarization performance and hue, and has excellent dimensional stability due to the low shrinkage rate of the polarizing film. Therefore, the polarizing plate is suitably used for LCDs such as LCDs, especially for mobile devices. .
  • the protective film is not particularly limited as long as it is optically transparent and has mechanical strength.
  • cellulose triacetate (TAC) film, cellulose acetate / butyrate (CAB) film, acrylic film, polyester film A film, a cyclic olefin (COP) film, etc. can be used.
  • the polarizing plate may be one in which the protective film is attached to one side of the polarizing film, or may be one in which the protective film is attached to both sides of the polarizing film.
  • examples of the adhesive for bonding include a PVA adhesive, a urethane adhesive, and an ultraviolet curable adhesive.
  • the manufacturing method of the said polarizing plate is not specifically limited, After performing the process of dyeing
  • the polarizing plate is produced in the same manner as the polarizing film production method described above except that the step of obtaining a multilayer film by laminating the PVA film and the protective film (hereinafter sometimes referred to as “lamination step”) is further performed.
  • lamination step the step of obtaining a multilayer film by laminating the PVA film and the protective film.
  • a lamination step is further performed.
  • a lamination process when performing a drying process, a lamination process may be performed before a drying process and a lamination process may be performed after a drying process.
  • a lamination process when performing a crosslinking process or a fixing process, it is preferable to perform a lamination process after performing these processes.
  • the polarizing plate thus obtained is bright, has good polarization characteristics, and is excellent in dimensional stability even when used under high temperature conditions. Therefore, it is suitably used for high performance LCDs, particularly LCDs for mobile devices.
  • shrinkage stress of polarizing film The shrinkage stress was measured using an autograph AG-X with a thermostatic bath manufactured by Shimadzu Corporation and a video extensometer TR ViewX120S. For the measurement, a polarizing film conditioned at 20 ° C. and 20% RH for 18 hours was used. After the temperature chamber of Autograph AG-X was set to 20 ° C., a polarizing film (length direction: 15 cm, width direction: 1.5 cm) was attached to a chuck (chuck interval: 5 cm). Tensile (speed 1 mm / min) and temperature increase (10 ° C./min) of the thermostat to 80 ° C. were started simultaneously. When the tension reached 2N after about 3 seconds, the tension was stopped and kept in that state.
  • the tension until 4 hours after the temperature in the thermostatic chamber reached 80 ° C. was measured. At this time, because the distance between chucks changes due to thermal expansion, a gauge sticker is attached to the chuck, and the distance between chucks is corrected by the amount of movement of the gauge seal attached to the chuck using the video extensometer TR ViewX120S. Measurements were taken as possible.
  • the value obtained by subtracting the initial tension 2N from the measured value of the tension (N) after 4 hours is the contraction force (N) of the polarizing film, and the value (N) is divided by the sample cross-sectional area (mm 2 ). It was defined as shrinkage stress (N / mm 2 ).
  • the shrinkage rate was measured using a thermomechanical measuring device (Q400) manufactured by TA Instruments.
  • a polarizing film conditioned at 20 ° C. and 20% RH for 18 hours was used.
  • a measurement sample obtained by cutting the polarizing film in the length direction of 3 cm and the width direction of 0.3 cm was attached to the apparatus so that the distance between the chucks was about 2 cm.
  • the temperature inside the apparatus was increased from 20 ° C. to 80 ° C. at 10 ° C./min, and then the polarizing film was heated by holding at 80 ° C. for 4 hours, and the shrinkage was calculated by the following formula.
  • Example 1 [Preparation of polarizing film] 100 parts by mass of PVA (saponification degree 99.9 mol%, polymerization degree 2500), 10 parts by mass of glycerin as a plasticizer, and 0.1 parts by mass of sodium polyoxyethylene lauryl ether sulfate as a surfactant, the content of PVA A 9% by mass aqueous solution was used as a film-forming stock solution. This was dried on a metal roll at 80 ° C., and the obtained film was heat-treated at a temperature of 112 ° C. for 10 minutes in a hot air dryer to produce a PVA film having a thickness of 30 ⁇ m.
  • PVA response degree 99.9 mol%, polymerization degree 2500
  • glycerin glycerin
  • sodium polyoxyethylene lauryl ether sulfate sodium polyoxyethylene lauryl ether sulfate
  • a sample having a width of 5 cm and a length of 11 cm is cut from the central portion of the obtained PVA film in the width direction, and the range of 5 cm and the length of 5 cm is uniaxially stretched in the MD (machine axis) direction during film formation.
  • the sample was fixed to a drawing jig. As a swelling process, this sample was immersed in pure water at 30 ° C., and uniaxially stretched in the length direction 1.1 times during that time.
  • iodine is adsorbed by immersing in an aqueous solution (dye bath, temperature 30 ° C.) containing iodine and potassium iodide at a mass ratio of 1:20 for 60 seconds, and 2.2 times ( A total of 2.4 times) was uniaxially stretched in the length direction.
  • aqueous solution die bath, temperature 30 ° C.
  • iodine and potassium iodide containing iodine and potassium iodide at a mass ratio of 1:20 for 60 seconds, and 2.2 times ( A total of 2.4 times) was uniaxially stretched in the length direction.
  • the iodine concentration in the dyeing bath was adjusted so that the transmittance of the polarizing film after drying was 44%.
  • the substrate is immersed in an aqueous solution (crosslinking bath, temperature 32 ° C.) containing 2.6% by mass of boric acid, and the length is 1.1 times (2.7 times as a whole) during that time. Uniaxially stretched in the direction.
  • the film was immersed in an aqueous solution (stretching bath, temperature 60 ° C.) containing 3% by mass of boric acid and 5% by mass of potassium iodide, and 2.2 times (totally 6. (0 times) was uniaxially stretched in the length direction.
  • the stretched PVA film was immersed in a boric acid aqueous solution (boric acid concentration 1.5 mass%, potassium iodide concentration 4 mass%, temperature 22 ° C.) for 10 seconds.
  • a cleaning step the substrate was immersed for 5 seconds in an aqueous solution (cleaning bath, temperature 20 ° C.) containing 3.5% by mass of potassium iodide.
  • the obtained PVA film was dried in air at 80 ° C. for 4 minutes. The drying process was performed in a state of being released to the atmosphere using a hot air dryer.
  • the optical properties, shrinkage rate, shrinkage stress, thickness, moisture content, and boron element content of the PVA film (Reference Example 1) before the annealing treatment thus obtained were measured.
  • the moisture content of the PVA film before the annealing treatment step was 8.1%, and the boron content was 3.46% by mass [boric acid (B (OH) 3 ) content 19.8% by mass].
  • Other results are shown in Table 1.
  • the obtained PVA film was cut so as to be 20 cm in the MD direction and 7 cm in the TD direction.
  • Two stainless steel frames were sandwiched between the ends of the PVA film in the MD direction so as not to be loosened, and the frames were further clipped from both outsides. In this way, both ends of the PVA film in the MD direction were fixed.
  • the PVA film was annealed in air at 80 ° C. for 360 minutes using a thermostatic bath. The annealing treatment was performed in a state released to the atmosphere.
  • the optical properties, shrinkage rate, and shrinkage stress A of the polarizing film thus obtained were measured. The results are shown in Table 1. Moreover, the contraction stress A and the simple substance b value B of the obtained polarizing film were plotted in FIG.
  • Examples 2 and 3 and Comparative Examples 1-5 and 7-12 A polarizing film was prepared and evaluated in the same manner as in Example 1 except that the annealing temperature and time were changed as shown in Table 1. These results are shown in Table 1.
  • the shrinkage stress A and the simple substance b value B of the polarizing film in Examples 2 and 3 and Comparative Examples 3 to 5 and 7 to 9 are plotted in FIG.
  • the shrinkage stress A and the simple substance b value B of the polarizing films in Examples 1 to 3, Comparative Examples 1 to 5 and 7 to 12, and Reference Example 1 are plotted in FIG.
  • Example 4 [Production of multilayer film]
  • a PVA film before the annealing process was obtained.
  • Cellulose triacetate (TAC) film coated with PVA glue (PVA content is 3% by mass) on one side is placed on both sides of the PVA film and laminated with a laminator, followed by drying at 60 ° C. for 10 minutes
  • TAC Cellulose triacetate
  • PVA content is 3% by mass
  • the obtained multilayer film before the annealing treatment step was immersed in methylene chloride, which is a good solvent for TAC, for 1 week, and then dried in a draft at room temperature for 24 hours to remove TAC from the PVA film.
  • the optical properties, shrinkage rate, shrinkage stress and thickness of the PVA film from which TAC was removed were measured. The results are shown in Table 1.
  • a polarizing film (polarizing plate) was obtained by performing the annealing process in the same manner as in Example 3 except that the obtained multilayer film before the annealing process was used. After removing TAC from the obtained polarizing film (polarizing plate) in the same manner as described above, the optical properties, shrinkage rate, shrinkage stress and thickness of the polarizing film from which TAC was removed were measured. The results are shown in Table 1.
  • Comparative Example 6 A polarizing film (polarizing plate) was produced and evaluated in the same manner as in Example 4 except that the annealing temperature and time were changed as shown in Table 1. These results are shown in Table 1.

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