WO2017073639A1 - Film à base d'alcool polyvinylique pour fabrication de pellicule polarisante ainsi que pellicule polarisante mettant en œuvre celui-ci, plaque de polarisation, et procédé de fabrication de film à base d'alcool polyvinylique pour fabrication de pellicule polarisante - Google Patents

Film à base d'alcool polyvinylique pour fabrication de pellicule polarisante ainsi que pellicule polarisante mettant en œuvre celui-ci, plaque de polarisation, et procédé de fabrication de film à base d'alcool polyvinylique pour fabrication de pellicule polarisante Download PDF

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Publication number
WO2017073639A1
WO2017073639A1 PCT/JP2016/081793 JP2016081793W WO2017073639A1 WO 2017073639 A1 WO2017073639 A1 WO 2017073639A1 JP 2016081793 W JP2016081793 W JP 2016081793W WO 2017073639 A1 WO2017073639 A1 WO 2017073639A1
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WO
WIPO (PCT)
Prior art keywords
film
polyvinyl alcohol
producing
polarizing film
polarizing
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PCT/JP2016/081793
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English (en)
Japanese (ja)
Inventor
秀一 北村
裕一 寺本
早川　誠一郎
Original Assignee
日本合成化学工業株式会社
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Application filed by 日本合成化学工業株式会社 filed Critical 日本合成化学工業株式会社
Priority to KR1020187009707A priority Critical patent/KR102629982B1/ko
Priority to CN201680058384.XA priority patent/CN108139528B/zh
Publication of WO2017073639A1 publication Critical patent/WO2017073639A1/fr

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Classifications

    • 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
    • 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
    • B29C55/08—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique transverse to the direction of feed
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02—Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • 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
    • 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
    • G02F1/13363—Birefringent elements, e.g. for optical compensation

Definitions

  • the present invention relates to a polyvinyl alcohol film for producing a polarizing film (hereinafter, sometimes simply referred to as “polyvinyl alcohol film”), particularly having excellent dyeability, a high degree of polarization, and color unevenness.
  • the present invention relates to a polyvinyl alcohol film capable of obtaining a small amount of polarizing film, a polarizing film using the polyvinyl alcohol film, a polarizing plate, and a method for producing a polarizing film-producing polyvinyl alcohol film.
  • a polyvinyl alcohol film has been used in many applications as a film having excellent transparency, and one of its useful applications is a polarizing film.
  • a polarizing film is used as a basic component of a liquid crystal display, and in recent years, its use has been expanded to a device requiring high quality and high reliability.
  • a polarizing film having excellent polarization performance is required as the screens of liquid crystal televisions and multi-function mobile terminals are increased in brightness, definition, area, and thickness. Specifically, the degree of polarization is further improved and color unevenness is eliminated.
  • a polyvinyl alcohol film for producing a polarizing film is produced from an aqueous solution of a polyvinyl alcohol resin by a continuous casting method.
  • an aqueous solution of a polyvinyl alcohol-based resin is cast on a cast mold such as a cast drum or an endless belt to form a film, and the formed film is peeled off from the cast mold and then flowed using a nip roll or the like. It is manufactured by drying using a hot roll or a floating dryer while transporting in the direction (MD direction). In such a conveyance process, since the film formed is pulled in the flow direction (MD direction), the polyvinyl alcohol polymer is easily oriented in the MD direction.
  • a polarizing film is produced by swelling a polyvinyl alcohol film, which is a raw material, with water (including warm water), dyeing with a dichroic dye such as iodine, and stretching.
  • the In such a swelling process it is necessary to quickly swell the polyvinyl alcohol film in the thickness direction. Furthermore, in the dyeing process, it is necessary to swell uniformly so that the dye smoothly enters the film.
  • the stretching step is a step of stretching the dyed film in the flow direction (MD direction) to highly orient the dichroic dye in the film.
  • MD direction flow direction
  • the case where the order of the stretching process and the dyeing process is opposite to the above is also carried out. That is, in this case, the polyvinyl alcohol film, which is the raw fabric, is swollen with water (including warm water), stretched, and dyed with a dichroic dye such as iodine. In order to improve the polarization performance, the polyvinyl alcohol-based film needs to have good swelling properties in the thickness direction and good stretchability in the MD direction.
  • polyvinyl alcohol films have also been made thinner in order to make the polarizing film thinner.
  • Such a thin film has a problem in productivity, such as being broken by stretching when the polarizing film is produced.
  • a technique for improving the swelling property for example, a technique of adding a polyhydric alcohol as a water swelling aid to a polyvinyl alcohol resin (for example, see Patent Document 1) has been proposed.
  • a technique for improving stretchability for example, a technique for specifying the ratio of the speed of the cast drum when the film is formed to the final film winding speed (see, for example, Patent Document 2), film formation with the cast drum
  • a method of floating and drying the film later see, for example, Patent Document 3
  • a method of controlling the tension in the drying process of the formed film for example, see Patent Document 4).
  • Patent Document 1 even if the swelling property of the entire polyvinyl alcohol film can be improved, the orientation state of the polyvinyl alcohol polymer is not taken into consideration, and the flow direction (MD direction) during the production of the polarizing film is not considered. It is difficult to improve the stretchability of the resin efficiently. Conversely, the addition of the water swelling agent tends to disturb the orientation of the polymer and make it difficult to uniformly stretch in the flow direction (MD direction).
  • the said patent document 2 specifies the extending
  • Patent Document 2 there is an example that does not stretch so much in the MD direction at the time of producing a polyvinyl alcohol-based film (an example that does not pull), but only the shrinkage stress depending on the Poisson's ratio and the shrinkage stress due to dehydration are high in the TD direction. There is a problem that the molecular orientation cannot be sufficiently uniformized.
  • the film is stretched to some extent in the TD direction or at least the width direction is not fixed, a uniform orientation state of the polymer in the TD direction cannot be obtained, and the stretchability in the MD direction during the production of the polarizing film is improved. Is insufficient. Moreover, there is no description regarding the orientation in the thickness direction, and the swelling property during the production of the polarizing film cannot be controlled.
  • the film after film formation can be dried uniformly, but the orientation of the polymer cannot be controlled, and is insufficient to improve the swelling property and stretchability during the production of the polarizing film.
  • the disclosed technique of Patent Document 4 can make the film thickness of the polyvinyl alcohol film uniform, the orientation of the polymer cannot be controlled, and is insufficient to improve the swelling property and stretchability during the production of the polarizing film. is there.
  • a polyvinyl alcohol system for producing a polarizing film which is excellent in swelling property and stretchability at the time of producing a polarizing film, can obtain a polarizing film having high polarizing performance and little color unevenness.
  • a polyvinyl alcohol film for producing a polarizing film that does not break when producing a film, particularly a thin polarizing film, and further comprises a polarizing film comprising the polyvinyl alcohol film for producing a polarizing film, a polarizing plate, and a polarizing film
  • the manufacturing method of the polyvinyl alcohol-type film for manufacture is provided.
  • the ratio of the swelling degree X (%) in the width direction (TD direction) and the swelling degree Y (%) in the flow direction (MD direction) is A polyvinyl alcohol film in a specific range is excellent in swelling property and stretchability at the time of producing a polarizing film, and a polarizing film obtained using such a polyvinyl alcohol film has high polarizing performance and has uneven color. It has been found that the polarizing film has a small amount.
  • the first gist of the present invention is a polyvinyl alcohol film having a thickness of 5 to 60 ⁇ m, a width of 2 m or more, and a length of 2 km or more, and when the polyvinyl alcohol film is immersed in water at 30 ° C. for 15 minutes.
  • Polarized light characterized in that the swelling degree X (%) in the width direction (TD direction) and the swelling degree Y (%) in the length direction (MD direction) satisfy the following conditions (1) and (2): It is a polyvinyl alcohol film for film production.
  • (1) 110 ⁇ Y ⁇ 140 1.01 ⁇ Y / X ⁇ 1.2
  • the degree of swelling Z (%) in the thickness direction satisfies the following condition (3): Is the second gist of the present invention.
  • the third aspect of the present invention is a polyvinyl alcohol film for producing a polarizing film, wherein the deviation ⁇ Z (%) of (%) is 5% or less.
  • the polyvinyl alcohol-type film for polarizing film manufacture characterized by satisfying the following conditions (4) and (5) is a fourth gist of the present invention.
  • the orientation axis, that is, the slow axis and the width direction, that is, the crossing angle ⁇ (°) in the TD direction is 20 ° or less.
  • the in-plane retardation Rxy (nm) is the width direction (TD (Direction) is a value calculated by the following formula (A), where nx is the refractive index in the direction (ny), ny is the refractive index in the length direction (MD direction), and d (nm) is the thickness.
  • A) Rxy (nm)
  • a polyvinyl alcohol-based film for producing a polarizing film is characterized in that the deviation ⁇ Rxy (nm) of the in-plane retardation Rxy (nm) in the width direction (TD direction) is 10 nm or less.
  • the gist is characterized in that the deviation ⁇ Rxy (nm) of the in-plane retardation Rxy (nm) in the width direction (TD direction) is 10 nm or less.
  • a sixth aspect of the present invention is a polyvinyl alcohol-based film for producing a polarizing film, wherein the deflection ⁇ (°) of the crossing angle ⁇ (°) is 10 ° or less.
  • a seventh aspect of the present invention is a polyvinyl alcohol film for manufacturing a polarizing film, wherein the thickness of the polyvinyl alcohol film is 5 to 30 ⁇ m.
  • the eighth gist of the present invention is a polarizing film characterized in that the polyvinyl alcohol film for producing the polarizing film is used.
  • the ninth aspect of the present invention is a polarizing plate comprising the polarizing film and a protective film provided on at least one surface of the polarizing film.
  • an aqueous solution of a polyvinyl alcohol resin is formed into a film by a continuous casting method, and after peeling from the cast mold, it is continuously dried and transported in the flow direction (MD direction) and in the width direction (TD direction).
  • MD direction flow direction
  • TD direction width direction
  • the swelling degree Y (%) in the flow direction (MD direction) satisfy the following conditions (1) and (2):
  • the eleventh aspect of the present invention is a method for producing a polyvinyl alcohol-based film for producing a polarizing film, characterized by stretching in the width direction (TD direction) at a draw ratio of 1.05 to 1.5 times.
  • a twelfth aspect of the present invention is a method for producing a polyvinyl alcohol film for producing a polarizing film, characterized in that stretching in the width direction (TD direction) is performed at 50 to 150 ° C.
  • a method for producing a polyvinyl alcohol film for producing a polarizing film according to the present invention is characterized in that the moisture content of the film before stretching in the width direction (TD direction) is 0.5 to 15% by weight. Thirteen abstracts.
  • a method for producing a polyvinyl alcohol film for producing a polarizing film, which is contracted, is a fourteenth aspect of the present invention.
  • the method for producing a polyvinyl alcohol film for producing a polarizing film characterized in that the rate of dimensional change in the flow direction (MD direction) of the film before and after stretching in the width direction (TD direction) is 0.8 to 1.0. Is the fifteenth aspect of the present invention.
  • the polyvinyl alcohol-based film for producing a polarizing film of the present invention is excellent in swelling property and stretchability at the time of producing a polarizing film, does not break even when a thin polarizing film is produced, exhibits high polarization performance, and has uneven color.
  • a small number of polarizing films can be provided.
  • this invention is invention based on the technical idea of improving the swelling property and stretchability at the time of polarizing film manufacture by improving the swelling property to the flow direction (MD direction) of a polyvinyl alcohol-type film.
  • the polyvinyl alcohol film for producing a polarizing film of the present invention is a polyvinyl alcohol film having a thickness of 5 to 60 ⁇ m, a width of 2 m or more, and a length of 2 km or more and having the following characteristics. Specifically, an aqueous solution of a polyvinyl alcohol-based resin is formed into a film by a continuous casting method, and after the formed film is peeled off from the cast mold, it is continuously dried and width direction ( It is a polyvinyl alcohol film obtained by stretching in the (TD direction).
  • the above conditions (1) and (2) can be achieved by, for example, a stretching process in the width direction (TD direction) of the film formed, and the stretching ratio in that case is 1.05 to 1.5.
  • the ratio is preferably double, particularly preferably 1.1 to 1.45 times, and more preferably 1.2 to 1.4 times. Control of the degree of swelling X (%) in the width direction (TD direction) and the degree of swelling Y (%) in the flow direction (MD direction) regardless of whether the draw ratio in the width direction (TD direction) is too low or too high. Control of the phase difference tends to be difficult, and swelling and stretchability during the production of the polarizing film tend to decrease.
  • Condition (1) specifies the degree of swelling Y (%) in the flow direction (MD direction), but is within the scope of known techniques.
  • the swelling degree Y (%) needs to be 110% or more and 140% or less, preferably 115% or more and 135% or less, and particularly preferably 120% or more and 130% or less. If the degree of swelling Y (%) is less than the lower limit, the stretchability during the production of the polarizing film is unfavorable, and conversely, if it exceeds the upper limit, the degree of polarization of the polarizing film is undesirably lowered.
  • Condition (2) specifies the ratio (Y / X) of the swelling degree Y (%) in the flow direction (MD direction) and the swelling degree X (%) in the width direction (TD direction).
  • the greatest feature of the present invention is that the swelling degree Y (%) in the flow direction (MD direction) is larger in a specific range than the swelling degree X (%) in the width direction (TD direction).
  • Many conventional polyvinyl alcohol films have a ratio of 1 or less. This is because the molecular chain of the polyvinyl alcohol polymer is normally oriented in the flow direction (MD direction) and is not easily swollen in this direction.
  • the ratio (Y / X) of the degree of swelling Y (%) in the flow direction (MD direction) and the degree of swelling X (%) in the width direction (TD direction) is as follows: Condition (2) 1.01 ⁇ Y / X ⁇ 1.2 must be satisfied, the following condition (2 ′) is preferably satisfied, and the following condition (2 ′′) is particularly preferably satisfied.
  • the degree of swelling Z (%) in the thickness direction preferably satisfies the following condition (3): Particularly preferably, the following condition (3 ′) is satisfied, and further preferably, the following condition (3 ′′) is satisfied. (3) 140 ⁇ Z ⁇ 170 (3 ′) 143 ⁇ Z ⁇ 169 (3 ′′) 145 ⁇ Z ⁇ 168
  • the degree of swelling Z (%) is larger than the degree of swelling in the width direction (TD direction) and the degree of swelling in the flow direction (MD direction). This is because the molecular chain of the polyvinyl alcohol-based polymer is mainly oriented in the plane direction and has a chemical structure that easily swells in the thickness direction. With this chemical structure, the polyvinyl alcohol film can be swollen quickly and uniformly in the swelling step during the production of the polarizing film.
  • the polyvinyl alcohol film of the present invention has a deflection ⁇ X (%) in the swelling degree X (%) in the width direction (TD direction) and a deflection ⁇ Y (%) in the swelling degree Y (%) in the flow direction (MD direction).
  • the swelling ⁇ Z (%) of the degree of swelling Z (%) in the thickness direction are preferably within 5%, particularly preferably within 4%, and more preferably within 3%. If the deflection is too large, color unevenness tends to occur in the polarizing film.
  • the film peeled off from the cast mold as in the present invention is arranged in the width direction (TD direction).
  • TD direction width direction
  • the polyvinyl alcohol-type film manufactured by the said method satisfies the physical-property value of both following conditions (4) and (5).
  • the crossing angle ⁇ (°) between the orientation axis (slow axis) and the width direction (TD direction) is 20 ° or less.
  • the in-plane retardation Rxy (nm) is the width direction (TD) in the polyvinyl alcohol film.
  • Direction is nx
  • the flow direction (MD direction) is ny
  • the thickness is d (nm).
  • A) Rxy (nm)
  • the in-plane retardation Rxy (nm) is particularly preferably 110 to 180 nm, and more preferably 130 to 170 nm. If the in-plane retardation Rxy (nm) is too small, the stretchability in the MD direction during the production of the polarizing film tends to be reduced, and if it is too large, color unevenness tends to occur in the polarizing film.
  • the deviation ⁇ Rxy (nm) of the in-plane retardation Rxy (nm) in the width direction (TD direction) is preferably 10 nm or less, particularly preferably 5 nm or less, and more preferably 3 nm or less. If the deflection ⁇ Rxy is too large, color unevenness tends to occur in the polarizing film.
  • the crossing angle ⁇ (°) between the orientation axis (slow axis) and the width direction (TD direction) is preferably 20 ° or less, particularly preferably 10 ° or less, and further preferably 5 ° or less.
  • the crossing angle ⁇ (°) is too large, the stretchability in the MD direction during the production of the polarizing film tends to be reduced.
  • the deflection ⁇ (°) of the crossing angle ⁇ (°) in the width direction (TD direction) is preferably 10 ° or less, particularly preferably 5 ° or less, and more preferably 3 ° or less. If the deflection ⁇ (°) is too large, color unevenness tends to occur in the polarizing film.
  • the polyvinyl alcohol resin used in the present invention and an aqueous solution thereof will be described.
  • the polyvinyl alcohol resin constituting the polyvinyl alcohol film is usually an unmodified polyvinyl alcohol resin, that is, a resin produced by saponifying polyvinyl acetate obtained by polymerizing vinyl acetate. Used. If necessary, a resin obtained by saponifying a copolymer of vinyl acetate and a small amount (usually 10 mol% or less, preferably 5 mol% or less) of a copolymerizable component with vinyl acetate may be used. it can.
  • components copolymerizable with vinyl acetate include unsaturated carboxylic acids (including salts, esters, amides, nitriles, etc.), and olefins having 2 to 30 carbon atoms (eg, ethylene, propylene, n-butene). , Isobutene, etc.), vinyl ethers, unsaturated sulfonates and the like.
  • the modified polyvinyl alcohol-type resin obtained by chemically modifying the hydroxyl group after saponification can also be used. These may be used alone or in combination of two or more.
  • a polyvinyl alcohol resin having a 1,2-diol structure in the side chain can be used as the polyvinyl alcohol resin.
  • a polyvinyl alcohol resin having a 1,2-diol structure in the side chain includes, for example, (i) a method of saponifying a copolymer of vinyl acetate and 3,4-diacetoxy-1-butene, and (ii) acetic acid.
  • the weight average molecular weight of the polyvinyl alcohol resin is preferably 100,000 to 300,000, particularly preferably 110,000 to 280,000, and more preferably 120,000 to 260,000. If the weight average molecular weight is too small, it tends to be difficult to obtain sufficient optical performance when the polyvinyl alcohol resin is used as an optical film, and if it is too large, the film is stretched when a polarizing film is produced using the polyvinyl alcohol film. Tend to be difficult.
  • the weight average molecular weight of the polyvinyl alcohol resin is a weight average molecular weight measured by GPC-MALS method.
  • the average saponification degree of the polyvinyl alcohol resin used in the present invention is usually preferably 98 mol% or more, particularly preferably 99 mol% or more, further preferably 99.5 mol% or more, and particularly preferably 99.mol%. It is 8 mol% or more. If the average saponification degree is too small, there is a tendency that sufficient optical performance cannot be obtained when a polyvinyl alcohol film is used as a polarizing film.
  • the average saponification degree in the present invention is measured according to JIS K 6726.
  • polyvinyl alcohol resin used in the present invention two or more kinds having different modified species, modified amount, weight average molecular weight, average saponification degree, etc. may be used in combination.
  • the polyvinyl alcohol-based resin aqueous solution may include plastics commonly used such as glycerin, diglycerin, triglycerin, ethylene glycol, triethylene glycol, polyethylene glycol, and trimethylolpropane as necessary. It is preferable from the point of film forming property to contain an agent and at least one surfactant of nonionic property, anionic property, and cationic property. These may be used alone or in combination of two or more.
  • the resin concentration of the aqueous polyvinyl alcohol resin solution thus obtained is preferably 15 to 60% by weight, particularly preferably 17 to 55% by weight, and further preferably 20 to 50% by weight. If the resin concentration of such an aqueous solution is too low, the drying load increases and the production capacity tends to decrease. If it is too high, the viscosity becomes too high and uniform dissolution tends to be difficult.
  • the obtained polyvinyl alcohol resin aqueous solution is defoamed.
  • the defoaming method include static defoaming and defoaming with a multi-screw extruder.
  • the multi-screw extruder may be a multi-screw extruder having a vent, and a biaxial extruder having a vent is usually used.
  • the polyvinyl alcohol-based resin aqueous solution is introduced into a T-shaped slit die by a certain amount, discharged and cast on a rotating cast drum, and formed into a film by a continuous casting method.
  • the continuous casting method in the present invention is, for example, a method of forming a film by discharging and casting an aqueous solution of a polyvinyl alcohol-based resin from a T-shaped slit die to a casting mold such as a rotating cast drum, an endless belt, or a resin film. It is.
  • the film formed may be peeled off from the cast mold, and then continuously dried with a hot roll while being conveyed in the flow direction (MD direction), and may be heat-treated, for example, with a floating dryer.
  • the resin temperature of the polyvinyl alcohol resin aqueous solution at the exit of the T-shaped slit die is preferably 80 to 100 ° C., and particularly preferably 85 to 98 ° C. If the resin temperature of such an aqueous polyvinyl alcohol resin solution is too low, there is a tendency to cause poor flow, and if it is too high, foaming tends to occur.
  • the viscosity of the aqueous polyvinyl alcohol resin solution is preferably 50 to 200 Pa ⁇ s, and particularly preferably 70 to 150 Pa ⁇ s at the time of discharge.
  • the viscosity of the aqueous solution is too low, the flow tends to be poor, and when it is too high, casting tends to be difficult.
  • the discharge speed of the aqueous polyvinyl alcohol resin solution discharged from the T-type slit die onto the cast drum is preferably 0.2 to 5 m / min, particularly preferably 0.4 to 4 m / min, and more preferably 0.8. 6-3 m / min. If the discharge speed is too slow, the productivity tends to decrease, and if it is too fast, casting tends to be difficult.
  • the diameter of the cast drum is preferably 2 to 5 m, particularly preferably 2.4 to 4.5 m, and more preferably 2.8 to 4 m. If the diameter is too small, the drying section on the cast drum is shortened, so that the speed tends to be difficult to increase. If the diameter is too large, the transportability tends to decrease.
  • the width of the cast drum is preferably 4 m or more, particularly preferably 4.5 m or more, more preferably 5 m or more, and particularly preferably 5 to 6 m. If the width of the cast drum is too small, the productivity tends to decrease.
  • the rotational speed of such a cast drum is preferably 3 to 50 m / min, particularly preferably 4 to 40 m / min, and further preferably 5 to 35 m / min. If the rotational speed is too slow, the productivity tends to decrease, and if it is too fast, drying tends to be insufficient.
  • the surface temperature of such a cast drum is preferably 40 to 99 ° C., particularly preferably 60 to 95 ° C. If the surface temperature is too low, drying tends to be poor, and if it is too high, foaming tends to occur.
  • the water content of the film thus formed is preferably 0.5 to 15% by weight, particularly preferably 1 to 13% by weight, More preferably, it is 2 to 12% by weight. If the water content is too low or too high, the orientation of the target polymer, that is, the desired degree of swelling or stretchability tends to be difficult.
  • the film is preferably dried before stretching in the width direction (TD direction).
  • the humidity before stretching in the width direction (TD direction) More preferably, the conditions of the drying process are adjusted so that the moisture content falls within the above range.
  • Such drying can be performed by a known method using a heating roll, an infrared heater, or the like, but in the present invention, it is preferably performed with a plurality of heating rolls, and particularly preferably, the temperature of the heating roll is 40 to 150 ° C. More preferably, it is 50 to 120 ° C. Moreover, you may provide a humidity control area before extending
  • the film shrinks slightly in the flow direction (MD direction).
  • the dimensional change rate in the flow direction (MD direction) is preferably 0.8 to 1.0, particularly preferably 0.9 to 1.0, more preferably 0. .95 to 1.0. If the rate of dimensional change is too small or too large, the degree of swelling tends to increase, and the orientation of the target polymer, that is, the desired degree of swelling tends to be difficult.
  • a preferable range of the conveying speed of the formed film in the flow direction (MD direction) is 5 to 30 m / min, particularly preferably 7 to 25 m / min, and further preferably 8 to 20 m / min. If the transport speed is too slow, the productivity tends to decrease, and if it is too fast, the color unevenness of the polarizing film tends to increase.
  • the method of simultaneously transporting the formed film in the flow direction (MD direction) and stretching in the width direction (TD direction) is not particularly limited.
  • both ends in the width direction of the film are formed with a plurality of clips. It is preferable to sandwich and carry and stretch simultaneously.
  • the arrangement of the clips at each end is preferably 200 mm or less, particularly preferably 100 mm or less, and more preferably 50 mm or less.
  • the clip clamping position (the tip of the clip) is preferably 100 mm or less from both ends in the width direction of the film formed. If the clip clamping position (tip portion) is located too far in the center of the film in the width direction, the film end to be discarded tends to increase and the product width tends to narrow.
  • the polyvinyl alcohol film specified in the present invention can be achieved by stretching in the width direction (TD direction) with respect to the formed film. It is preferably 05 to 1.5 times, particularly preferably 1.1 to 1.45 times, more preferably 1.15 to 1.4 times, and particularly preferably 1.2 to 1.3 times. . Even if the draw ratio in the width direction (TD direction) is too low or too high, the swellability and stretchability during the production of the polarizing film tend to decrease.
  • Such a continuous stretching process in the width direction (TD direction) may be one stage (one time), or may be a plurality of stages (multiple times) so that the total stretching ratio falls within the range of the above-mentioned stretching ratio (also called sequential stretching). be called).
  • simple transport with the width direction (TD direction) fixed may be performed, and the second and subsequent stages of stretching may be performed.
  • the stress of the film is relaxed and it is possible to avoid breakage.
  • the fixed width can be narrower than the width after the first stage of stretching.
  • the film immediately after stretching is easily shrunk for stress relaxation, and shrinkage due to dehydration also occurs. Therefore, it is possible to narrow the fixed width to these shrinkage widths. However, it is not preferable to make the width narrower than the contraction width because the film will bend.
  • the stretching step is preferably performed after the film drying step, but may be performed alone at least before or after the film drying step, or may be performed during the drying step.
  • the film is stretched temporarily in the width direction (TD direction) exceeding 1.3 times, and then the final draw ratio in the width direction (TD direction) is 1.05 to 1. It is also possible to use a technique of dimensional shrinkage so as to be 5 times. In such a case, after the film is temporarily stretched over 1.3 times, the film may be simply conveyed with a fixed width of a stretch ratio of 1.05 to 1.5 times. By this method, the stress of the film is relaxed, and it is possible to avoid breakage particularly in the case of a thin film.
  • stretching in the width direction (TD direction) of the formed film is preferably performed at 50 to 150 ° C., particularly preferably 60 to 140 ° C., and further preferably 70 to 130 ° C. If the stretching temperature is too low or too high, the stretchability during the production of the polarizing film tends to decrease.
  • the stretching temperature may be changed at each stretching step, or a temperature gradient may be provided during stretching.
  • the stretching time for stretching the film formed in the width direction is preferably 2 to 60 seconds, particularly preferably 5 to 45 seconds, and more preferably 10 to 30 seconds. If the stretching time is too short, the film tends to break, and conversely, if it is too long, the equipment load tends to increase. When performing sequential stretching, the stretching time may be changed at each stretching stage.
  • heat treatment may be performed with a floating dryer or the like after stretching the film formed in the width direction (TD direction).
  • the temperature of the heat treatment is preferably 60 to 200 ° C., particularly preferably 70 to 150 ° C., and further preferably 100 to 140 ° C. If the heat treatment temperature is too low, the dimensional stability tends to decrease, and conversely, if it is too high, the stretchability during the production of the polarizing film tends to decrease.
  • the heat treatment time is preferably 1 to 60 seconds, and particularly preferably 5 to 30 seconds. If the heat treatment time is too short, the dimensional stability tends to decrease. Conversely, if the heat treatment time is too long, the swellability and stretchability during the production of the polarizing film tend to decrease.
  • the polyvinyl alcohol film for producing the polarizing film of the present invention is obtained, and is finally wound up on a roll to become a product.
  • the thickness of such a polyvinyl alcohol film is from 5 to 60 ⁇ m from the viewpoint of in-plane retardation, particularly preferably from 5 to 45 ⁇ m, more preferably from 5 to 30 ⁇ m, particularly preferably from the viewpoint of thinning the polarizing film. Is 10 to 20 ⁇ m from the viewpoint of avoiding breakage.
  • the thickness of the polyvinyl alcohol film is adjusted by the resin concentration in the aqueous polyvinyl alcohol resin solution, the discharge amount (discharge speed) to the cast mold, the draw ratio, and the like.
  • the width of the polyvinyl alcohol film is 2 m or more, particularly preferably 3 m or more from the viewpoint of increasing the area, and further preferably 4 to 6 m from the viewpoint of avoiding breakage.
  • the length of such a polyvinyl alcohol film is 2 km or more, particularly preferably 3 km or more from the viewpoint of increasing the area, and more preferably 3 to 50 km from the viewpoint of transport weight.
  • the polyvinyl alcohol film for manufacturing a polarizing film of the present invention is very useful as an original film of a polarizing film.
  • a polarizing film made of the polyvinyl alcohol film and a method for manufacturing a polarizing plate will be described.
  • the polarizing film of the present invention is produced through steps such as swelling, dyeing, boric acid crosslinking, stretching, washing, and drying by feeding the polyvinyl alcohol film out of a roll and transferring it in the horizontal direction.
  • the swelling process is performed before the dyeing process.
  • water is usually used as the treatment liquid.
  • the treatment solution may contain a small amount of an iodide compound, an additive such as a surfactant, alcohol, or the like.
  • the temperature of the swelling bath is usually about 10 to 45 ° C., and the immersion time in the swelling bath is usually about 0.1 to 10 minutes.
  • the degree of swelling of the polyvinyl alcohol film of the present invention is measured in the width direction (TD direction) when immersed in water at 30 ° C. for 15 minutes and the degree of swelling of the film is measured.
  • the degree of swelling X (%) and the degree of swelling Y (%) in the flow direction (MD direction) satisfy both physical property values of the following conditions (1) and (2).
  • the degree of swelling Z (%) in the thickness direction preferably satisfies the following condition (3).
  • the dyeing step is performed by bringing the film into contact with a liquid containing iodine or a dichroic dye.
  • a liquid containing iodine or a dichroic dye usually, an iodine-potassium iodide aqueous solution is used.
  • the iodine concentration is suitably 0.1-2 g / L, and the potassium iodide concentration is 1-100 g / L.
  • the dyeing time is practically about 30 to 500 seconds.
  • the temperature of the treatment bath is preferably 5 to 50 ° C.
  • the aqueous solution may contain a small amount of an organic solvent compatible with water in addition to the aqueous solvent.
  • the boric acid crosslinking step is performed using a boron compound such as boric acid or borax.
  • the boron compound is used in the form of an aqueous solution or a water-organic solvent mixture at a concentration of about 10 to 100 g / L, and it is preferable that potassium iodide coexists in the solution from the viewpoint of stabilizing the polarization performance.
  • the temperature during the treatment is preferably about 30 to 70 ° C., and the treatment time is preferably about 0.1 to 20 minutes. If necessary, the stretching operation may be performed during the treatment.
  • the film is preferably stretched 3 to 10 times, preferably 3.5 to 6 times in the uniaxial direction.
  • a slight stretching may be performed in a direction perpendicular to the stretching direction.
  • the temperature during stretching is preferably 40 to 170 ° C.
  • the draw ratio may be finally set within the above range, and the drawing operation may be performed not only once but also plural times in the production process.
  • the washing step is performed, for example, by immersing a polyvinyl alcohol film in an aqueous solution of iodide such as water or potassium iodide, thereby removing deposits generated on the surface of the film.
  • iodide such as water or potassium iodide
  • the concentration of potassium iodide may be about 1 to 80 g / L.
  • the temperature during the washing treatment is usually 5 to 50 ° C., preferably 10 to 45 ° C.
  • the treatment time is usually 1 to 300 seconds, preferably 10 to 240 seconds.
  • the film is dried in the atmosphere at 40 to 80 ° C. for 1 to 10 minutes.
  • the degree of polarization of the polarizing film is preferably 99.5% or more, particularly preferably 99.8% or more. If the degree of polarization is too low, the contrast in the liquid crystal display tends to decrease.
  • the single transmittance of the polarizing film of the present invention is preferably 44% or more. If the single transmittance is too low, it tends to be impossible to achieve high brightness of the liquid crystal display.
  • the single transmittance is a value obtained by measuring the light transmittance of a single polarizing film using a spectrophotometer.
  • the polarizing film of the present invention is suitable for producing a polarizing plate with little color unevenness and excellent polarization performance.
  • the polarizing plate of the present invention is produced by bonding an optically isotropic resin film as a protective film to one or both sides of the polarizing film of the present invention via an adhesive.
  • the protective film include cellulose triacetate, cellulose diacetate, polycarbonate, polymethyl methacrylate, cycloolefin polymer, cycloolefin copolymer, polystyrene, polyethersulfone, polyarylene ester, poly-4-methylpentene, polyphenylene oxide, and the like. Or a sheet.
  • the bonding method is performed by a known method. For example, after the liquid adhesive composition is uniformly applied to the polarizing film, the protective film, or both, the both are bonded and pressure-bonded. It is performed by irradiating active energy rays.
  • a curable resin such as urethane resin, acrylic resin, urea resin or the like on one side or both sides of the polarizing film and cure to form a cured layer to obtain a polarizing plate. If it does in this way, the said hardened layer becomes a substitute of the said protective film, and can attain thinning.
  • the polarizing film and polarizing plate using the polyvinyl alcohol film of the present invention are excellent in polarizing performance, and are portable information terminals, personal computers, televisions, projectors, signage, electronic desk calculators, electronic watches, word processors, electronic paper, game machines. , Video, camera, photo album, thermometer, audio, liquid crystal display devices such as automobiles and machinery instruments, sunglasses, anti-glare glasses, stereoscopic glasses, wearable display, display elements (CRT, LCD, organic EL, electronic paper) Etc.) for antireflection layers, optical communication equipment, medical equipment, building materials, toys and the like.
  • the degree of swelling X (%) in the width direction (TD direction) and the degree of swelling Y (%) in the flow direction (MD direction) were calculated according to the following formula.
  • the degree of swelling Z (%) in the thickness direction was determined by cutting out a film of width 100 mm ⁇ length 100 mm one by one from the width direction center and both left and right ends of the polyvinyl alcohol film, and immersing in water at 30 ° C. for 15 minutes. After swelling, the film is taken out and placed on the filter paper (5A), and the filter paper (5A) is placed on the film, and 150 mm ⁇ 150 mm ⁇ 4 mm (4.4 ⁇ 10 ⁇ on top).
  • a 2 g / mm 2 ) SUS plate was placed for 5 seconds to remove water adhering to the film surface. This film was immediately put into a weighing bottle, and the weight was measured. This was defined as “weight after immersion”. The above operation was performed in an environment of 23 ° C. and 50% RH. Next, the film is left in a drier at 105 ° C. for 16 hours to remove moisture in the film, and then the film is taken out, immediately put into a weighing bottle, and the weight is measured. Weight ”. Then, the degree of swelling Z (%) in the thickness direction was calculated according to the following formula.
  • Swelling degree X (%) 100 ⁇ width in TD direction after immersion (mm) / width in TD direction before immersion (mm)
  • Swelling degree Y (%) 100 ⁇ width in MD direction after immersion (mm) / width in MD direction before immersion (mm)
  • Swelling degree Z (%) 1000000 ⁇ weight after immersion (g) / weight after drying (g) / X / Y
  • a 4 cm long ⁇ 4 cm wide test piece was cut out from the center in the width direction of the obtained polyvinyl alcohol film and both left and right ends (10 cm inside from the film end), and a retardation measuring device (“KOBRA-WR”) was cut.
  • In-plane retardation Rxy (nm) and crossing angle ⁇ (°) between the orientation axis (slow axis) and the width direction (TD direction) were measured using Oji Scientific Instruments.
  • the difference ⁇ Rxy (nm) of the in-plane phase difference is obtained by taking the difference between the maximum value and the minimum value from the in-plane phase difference Rxy (nm) between the central portion and the left and right end portions in the width direction obtained by the above measurement. It was. Further, the crossing angle ⁇ (°) of the crossing angle ⁇ (°) is obtained by taking the difference between the maximum value and the minimum value from the crossing angle ⁇ (°) between the central part and the left and right ends in the width direction obtained by the above measurement. It was.
  • Example 1 (Preparation of polyvinyl alcohol film)
  • 1,000 kg of polyvinyl alcohol resin having a weight average molecular weight of 142,000 and a saponification degree of 99.8 mol%, 2,500 kg of water, 105 kg of glycerin as a plasticizer, and polyoxy as a surfactant 0.25 kg of ethylene laurylamine was added, and the mixture was heated to 150 ° C. with stirring and dissolved under pressure.
  • concentration an aqueous solution of a polyvinyl alcohol resin having a resin concentration of 25% by weight was obtained.
  • the polyvinyl alcohol-based resin aqueous solution is supplied to a twin screw extruder and defoamed, and then the temperature of the aqueous solution is set to 95 ° C. and discharged from a T-type slit die discharge port onto a rotating cast drum (discharge speed of 2. 5 m / min) and cast to form a film.
  • the film formed was peeled off from the cast drum and dried while being conveyed in the flow direction (MD direction) while alternately bringing the front and back surfaces of the film into contact with a total of 10 hot rolls. Thereby, a film (width 2 m, thickness 60 ⁇ m) having a water content of 10% by weight was obtained.
  • the left and right ends of the film are clamped at a clip pitch of 45 mm, and the film is conveyed in the flow direction (MD direction) at a speed of 8 m / min, while using a stretching machine at 120 ° C. in the width direction (TD direction). .2 stretched.
  • the dimensional change rate in the flow direction (MD direction) before and after stretching in the width direction (TD direction) was 0.96.
  • heat treatment was performed at 120 ° C. for 10 seconds to obtain a polyvinyl alcohol film (width 2.4 m, thickness 50 ⁇ m, length 2 km).
  • the properties of the obtained polyvinyl alcohol film were as shown in Tables 1 and 2.
  • Example 2 In Example 1, the film formed was stretched 1.4 times in the width direction (TD direction) at 120 ° C. using a stretching machine, and then transported with a fixed width of 2.4 m (equivalent to 1.2 times stretching). Otherwise, a polyvinyl alcohol film (width 2.4 m, thickness 50 ⁇ m, length 2 km) was obtained in the same manner as in Example 1. The dimensional change rate in the flow direction (MD direction) before and after stretching in the width direction (TD direction) was 0.96. The properties of the obtained polyvinyl alcohol film were as shown in Tables 1 and 2. Further, using the polyvinyl alcohol film, a polarizing film and a polarizing plate were obtained in the same manner as in Example 1. No fracture occurred during such production. The properties of the obtained polarizing film were as shown in Table 2.
  • Example 3 In Example 1, the ejection speed during film formation was 0.8 m / min, and a film having a water content of 5% by weight (width 2 m, thickness 20 ⁇ m) was stretched 1.4 times in the width direction (TD direction) and then fixed. A polyvinyl alcohol film (width 2.6 m, thickness 15 ⁇ m, length 2 km) was obtained in the same manner as in Example 1 except that the film was transported at a width of 2.6 m (equivalent to 1.3 times stretching). The dimensional change rate in the flow direction (MD direction) before and after stretching in the width direction (TD direction) was 0.98. The properties of the obtained polyvinyl alcohol film were as shown in Tables 1 and 2.
  • a polarizing film and a polarizing plate were obtained in the same manner as in Example 1. Despite the thinness of the original polyvinyl alcohol film, no breakage occurred in the stretching process during the production of the polarizing film. The properties of the obtained polarizing film were as shown in Table 3.
  • Example 1 A polyvinyl alcohol film (width 2 m, thickness 60 ⁇ m) was obtained in the same manner as in Example 1 except that the film formed in Example 1 was not stretched in the width direction (TD direction) using a stretching machine. , 2 km long).
  • the properties of the obtained polyvinyl alcohol film were as shown in Tables 1 and 2. Further, using the polyvinyl alcohol film, a polarizing film and a polarizing plate were obtained in the same manner as in Example 1. The properties of the obtained polarizing film were as shown in Table 3.
  • Example 3 a polyvinyl alcohol film (width 2 m, thickness 20 ⁇ m) was formed in the same manner as in Example 3 except that the film formed was not stretched in the width direction (TD direction) using a stretching machine. , 2 km long).
  • the properties of the obtained polyvinyl alcohol film were as shown in Tables 1 and 2. Further, using the polyvinyl alcohol film, a polarizing film and a polarizing plate were obtained in the same manner as in Example 1. The properties of the obtained polarizing film were as shown in Table 3.
  • the ratio of the swelling degree X (%) in the width direction (TD direction) to the swelling degree Y (%) in the flow direction (MD direction) indicates that the conditions (1) and (2)
  • the polarizing films of Examples 1 to 3 obtained from the polyvinyl alcohol film satisfying the range specified in (1) had a high degree of polarization and no color unevenness.
  • the ratio between the swelling degree X (%) in the width direction (TD direction) and the swelling degree Y (%) in the flow direction (MD direction) is outside the range specified by the conditions (1) and (2). It can be seen that the polarizing films of Comparative Examples 1 and 2 obtained from a certain polyvinyl alcohol film are inferior in the degree of polarization and color unevenness is observed.
  • the in-plane phase difference (Rxy) and the crossing angle ⁇ (°) between the orientation axis (slow axis) and the width direction (TD direction) satisfy the range specified by the conditions (4) and (5).
  • the polarizing films of Examples 1 to 3 obtained from the alcohol film had a high degree of polarization and no color unevenness.
  • the in-plane retardation (Rxy) and the crossing angle ⁇ (°) between the orientation axis (slow axis) and the width direction (TD direction) are outside the range specified by the conditions (4) and (5). It can be seen that the polarizing films of Comparative Examples 1 and 2 obtained from a certain polyvinyl alcohol film are inferior in the degree of polarization and color unevenness is observed.
  • the polarizing film and polarizing plate using the polyvinyl alcohol film of the present invention are excellent in polarizing performance, and are portable information terminals, personal computers, televisions, projectors, signage, electronic desk calculators, electronic watches, word processors, electronic papers, game machines. , Video, camera, photo album, thermometer, audio, liquid crystal display devices such as automobiles and machinery instruments, sunglasses, anti-glare glasses, stereoscopic glasses, wearable display, display elements (CRT, LCD, organic EL, electronic paper) Etc.) for antireflection layers, optical communication equipment, medical equipment, building materials, toys and the like.

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Abstract

L'invention concerne un film à base d'alcool polyvinylique dont l'épaisseur est comprise entre ５ et ６０μｍ, la largeur est supérieure ou égale à 2m, et la longueur est supérieure ou égale à 2km. Plus précisément, l'invention concerne un film à base d'alcool polyvinylique pour fabrication de pellicule polarisante qui est caractéristique en ce que lorsque ce film à base d'alcool polyvinylique est immergé pendant 15 minutes dans une eau à 30°C, le degré de gonflement X (%) dans la direction de la largeur (direction TD) et le degré de gonflement Y (%) dans la direction de la longueur (direction MD) satisfont les conditions suivantes (1) et (2). （１）１１０≦Ｙ≦１４０ （２）１,０１≦Ｙ／Ｘ≦１,２
PCT/JP2016/081793 2015-10-27 2016-10-27 Film à base d'alcool polyvinylique pour fabrication de pellicule polarisante ainsi que pellicule polarisante mettant en œuvre celui-ci, plaque de polarisation, et procédé de fabrication de film à base d'alcool polyvinylique pour fabrication de pellicule polarisante WO2017073639A1 (fr)

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KR1020187009707A KR102629982B1 (ko) 2015-10-27 2016-10-27 편광막 제조용 폴리비닐 알코올계 필름 및 이를 사용한 편광막, 편광판, 및 편광막 제조용 폴리비닐 알코올계 필름의 제조
CN201680058384.XA CN108139528B (zh) 2015-10-27 2016-10-27 偏光膜制造用聚乙烯醇系薄膜、及使用了其的偏光膜、偏光板、以及偏光膜制造用聚乙烯醇系薄膜的制造方法

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