CN103201656A - Methods for producing polarizing laminate film and polarizing plate - Google Patents
Methods for producing polarizing laminate film and polarizing plate Download PDFInfo
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- CN103201656A CN103201656A CN2011800537213A CN201180053721A CN103201656A CN 103201656 A CN103201656 A CN 103201656A CN 2011800537213 A CN2011800537213 A CN 2011800537213A CN 201180053721 A CN201180053721 A CN 201180053721A CN 103201656 A CN103201656 A CN 103201656A
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- Prior art keywords
- film
- resin
- base material
- polyvinyl alcohol
- layer
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- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
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- 210000002858 crystal cell Anatomy 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- DJTHARKDQLFDST-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate;methyl 2-methylprop-2-enoate Chemical compound COC(=O)C(C)=C.CC(=C)C(=O)OC1CCCCC1 DJTHARKDQLFDST-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 229920005994 diacetyl cellulose Polymers 0.000 description 1
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- 229920001971 elastomer Polymers 0.000 description 1
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- 150000002513 isocyanates Chemical class 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
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- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical class C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 235000012736 patent blue V Nutrition 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical group CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
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- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical compound CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NZYOAGBNMCVQIV-UHFFFAOYSA-N sodium;chloro-(4-methylphenyl)sulfonylazanide;trihydrate Chemical compound O.O.O.[Na+].CC1=CC=C(S(=O)(=O)[N-]Cl)C=C1 NZYOAGBNMCVQIV-UHFFFAOYSA-N 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 238000007811 spectroscopic assay Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- OLSOUGWNONTDCK-UHFFFAOYSA-J tetrasodium 5-amino-3-[[4-[4-[(8-amino-1-hydroxy-3,6-disulfonatonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-4-hydroxynaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].C1=C(S([O-])(=O)=O)C=C2C=C(S([O-])(=O)=O)C(N=NC3=CC=C(C=C3OC)C=3C=C(C(=CC=3)N=NC=3C(=CC4=CC(=CC(N)=C4C=3O)S([O-])(=O)=O)S([O-])(=O)=O)OC)=C(O)C2=C1N OLSOUGWNONTDCK-UHFFFAOYSA-J 0.000 description 1
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Images
Classifications
-
- 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
- B29C55/023—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets using multilayered plates or sheets
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- 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
- 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
- B29C55/065—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 in several stretching steps
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2029/00—Use of polyvinylalcohols, polyvinylethers, polyvinylaldehydes, polyvinylketones or polyvinylketals or derivatives thereof as moulding material
- B29K2029/04—PVOH, i.e. polyvinyl alcohol
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0018—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular optical properties, e.g. fluorescent or phosphorescent
- B29K2995/0034—Polarising
Abstract
A method for producing a polarizing laminate film including a base film and a polarizer layer formed on one surface of the base film involves, in the following order: a resin film laminating step of laminating a resin film made of a polyvinyl alcohol resin and having a thickness of 50 [mu]m or less onto one surface of a base film, to thereby obtain a laminate film; a stretching step of uniaxially stretching the laminate film; and a dyeing step of dyeing the resin film of the uniaxially stretched laminate film with a dichroic dye, to thereby form a polarizer layer. The present invention can provide a method for producing a polarizing laminate film having a thin polarizer layer without giving rise to the problem that the ends of the base film are folded inside.
Description
Technical field
The present invention relates to the manufacture method of a kind of polarizability stacked film and polarization plates.
Background technology
Polarization plates is widely used as feed element of the polarized light in the display device of liquid crystal indicator etc. etc.As described polarization plates, all the time, use the stacked polarization plates that forms of diaphragm that the layer of polarizer that is made of polyvinyl alcohol resin and triacetyl cellulose etc. are arranged.In the layer of polarizer (polarizing coating), not only be required high optical property, and in recent years along with development in mobile devices such as the subnotebook PC of liquid crystal indicator, mobile phone etc., be required thin-wall light-weighted.
Example as the manufacture method of polarization plates; known have a following method: by after the film that is made of polyvinyl alcohol resin that stretches separately; perhaps the limit stretches, and the dyeing processing is implemented on the limit, crosslinking Treatment is made polarizing coating; and it is laminated in diaphragm etc., make polarization plates (for example with reference to JPH11-49878-A) thus.
Other a example as the manufacture method of polarization plates, proposition has following method: the solution that contains polyvinyl alcohol resin in the coating of the surface of base material film, after resin bed is set, the stacked film that is constituted by stretching base material film and resin bed, then dye, form layer of polarizer by resin bed, obtain having the method (for example with reference to JP2000-33829-A) of the polarizability stacked film of layer of polarizer.Disclose it is directly utilized and make polarization plates or behind this film applying diaphragm, make the method for polarization plates with peeling off product utilization behind the base material film.
Other a example as the manufacture method of polarization plates; diaphragm is carried out coextrusion and makes stacked film with resin and polyvinyl alcohol resin; this stacked film stretches; then dye, obtain the method (for example with reference to JP2009-25821-A) of the polarization plates that constituted by layer of polarizer and diaphragm thus.
Yet, the film that is made of polyvinyl alcohol resin is being implemented independent stretching, dyeing, crosslinking Treatment and made in the method for polarizing coating, owing to be easy to generate fracture, fold etc., so it is difficult to handle the following slim film of 50 μ m, therefore be difficult to realize the slimming of polarizing coating.
Contain the solution of polyvinyl alcohol resin and arrange in the method for resin bed in the coating of the surface of base material film, shrink because of the drying of the solution that contains polyvinyl alcohol resin resin bed is shunk easily, consequently produce the two ends of base material film sometimes to the phenomenon of resin bed side warpage, if keeping making the base material film continuous flow with resin bed under this state, the end that then can cause base material film in drying oven or the drying oven outlet undesirable condition of bending takes place.
Come out to make in the method for stacked film making diaphragm carry out co-extrusion with resin and polyvinyl alcohol resin; usually make polyvinyl alcohol resin with the solvent fusion; extrude, therefore with above-mentioned same, shrink the undesirable condition that bending takes place in the end that causes base material film because of drying sometimes.
Therefore, the object of the present invention is to provide manufacturing can not cause the end of base material film the undesirable condition of bending to take place and have the polarizability stacked film of slim layer of polarizer and the method for polarization plates.
Summary of the invention
The present invention comprises following proposal.
[1] a kind of manufacture method of polarizability stacked film, described polarizability stacked film has base material film and is formed at the layer of polarizer of a face of this base material film, and described method comprises following operation successively: be the resin molding bonding process that the resin molding that contains polyvinyl alcohol resin below the 50 μ m obtains stacked film at a face coating thickness of base material film;
Above-mentioned stacked film is carried out the stretching process of uniaxial tension; And
Dye with the described resin molding of dichromatism pigment to above-mentioned uniaxial tension stacked film, and the dyeing process of formation layer of polarizer.
[2] according to [1] described method, wherein, in the above-mentioned resin molding bonding process, described resin molding is fitted in a face of described base material film by bonding agent (adhesion drug) layer or bonding agent (then drug) layer.
[3] according to [1] or [2] described method, wherein, in the above-mentioned resin molding bonding process, above-mentioned thickness of resin film is more than the 15 μ m.
[4] according to each described method in [1]～[3], wherein, the above-mentioned resin molding that uses in the above-mentioned resin molding bonding process is the resin molding that utilizes the manufacture method manufacturing that comprises following operation successively to form,
The resin bed that forms the resin bed that contains polyvinyl alcohol resin at supporter forms operation,
This resin bed is carried out the 1st dry drying process, peel off this resin bed and obtain the resin bed separation circuit of this resin bed from this supporter, and
This resin bed is carried out the 2nd dry drying process under than the high baking temperature of the temperature in the 1st drying process.
[5] a kind of manufacture method of polarization plates, described polarization plates have layer of polarizer and are formed at the diaphragm of a face of this layer of polarizer, and described manufacture method comprises following operation successively after utilizing [1] described method to make the polarizability stacked film:
The diaphragm bonding process of the face applying diaphragm of the above-mentioned layer of polarizer in this polarizability stacked film and face opposition side above-mentioned base material film side; And
Peel off the base material film stripping process of above-mentioned base material film from this polarizability stacked film.
According to the present invention, can make and to make that the end of base material film bends in the manufacturing process, and have polarizability stacked film and the polarization plates of slim layer of polarizer.
Description of drawings
Fig. 1 is the process flow diagram of an embodiment of the manufacture method of expression polarizability stacked film of the present invention.
Fig. 2 is the process flow diagram of an embodiment of the manufacture method of expression polarization plates of the present invention.
Fig. 3 is the process flow diagram of an embodiment of the manufacture method of expression polyvinyl alcohol resin film.
Embodiment
Below, be elaborated with reference to the preferred implementation of accompanying drawing limit to the manufacture method of the manufacture method of polarizability stacked film of the present invention and polarization plates.
(manufacture method of polarizability stacked film)
Fig. 1 is the process flow diagram of an embodiment of the manufacture method of expression polarizability stacked film of the present invention.Have base material film and be formed at the layer of polarizer of a face of base material film with the polarizability stacked film of present embodiment manufacturing.In the manufacture method of the polarizability stacked film of present embodiment, usually a face that is implemented in base material film is successively fitted and is comprised the resin molding of polyvinyl alcohol resin and obtain the resin molding bonding process (S10) of stacked film, this stacked film is carried out the stretching process (S20) of uniaxial tension and dyes with the resin molding of dichromatism pigment to this stacked film, forms the dyeing process (S30) of layer of polarizer.
In this instructions, the duplexer that will be fitted with the resin molding that contains polyvinyl alcohol resin (below be also referred to as " polyvinyl alcohol resin film ") at a face of base material film is called " stacked film ", the polyvinyl alcohol resin film that will have as the function of polaroid is called " layer of polarizer ", will have the duplexer of layer of polarizer to be called " polarizability stacked film " at a mask of base material film.In addition, will there be the duplexer of diaphragm to be called " polarization plates " at a mask of layer of polarizer.
By above-mentioned manufacture method, can obtain possessing the polarizability stacked film with layer of polarizer sufficient polarization property, below for example thickness 25 μ m at base material film.The thickness of the layer of polarizer of the polarizability stacked film that obtains by above-mentioned manufacture method is preferably below the 25 μ m, more preferably below the 20 μ m.As described later, this polarizability stacked film also can be used as for the intermediate product that layer of polarizer is transferred to diaphragm and uses, and in addition, has at base material film under the situation of function of diaphragm, also can be with this polarizability stacked film directly as polarization plates.
(manufacture method of polarization plates)
Fig. 2 is the process flow diagram of an embodiment of the manufacture method of expression polarization plates of the present invention.Have layer of polarizer and be formed at the diaphragm of a face of layer of polarizer with the polarization plates of present embodiment manufacturing.Manufacture method about the polarization plates of present embodiment; usually implementing following operation successively: the resin molding bonding process (S10) that obtains stacked film at a face applying polyvinyl alcohol resin film of base material film; this stacked film is carried out the stretching process (S20) of uniaxial tension; and with the dichromatism pigment polyvinyl alcohol resin film of this stacked film is dyeed and form the dyeing process (S30) of layer of polarizer; thereby after obtaining the polarizability stacked film, usually has the diaphragm bonding process (S40) at the face applying diaphragm of layer of polarizer and the face opposition side base material film side of polarizability stacked film successively; and the base material film stripping process (S50) of peeling off base material film from the polarizability stacked film.
Utilize above-mentioned manufacture method can obtain possessing the polarization plates with layer of polarizer sufficient polarization property, below for example thickness 25 μ m at diaphragm.Utilize the thickness of the layer of polarizer of the polarization plates that above-mentioned manufacture method obtains to be preferably below the 25 μ m, more preferably below the 20 μ m.This polarization plates can be as the blooming, liquid crystal cells etc. that for example fit in other by the pressure sensitive bonding agent.
Below each operation of the S10～S50 among Fig. 1 and Fig. 2 is elaborated.Need to prove that each operation of S10～S30 of Fig. 1 and Fig. 2 is same operation.
＜resin molding bonding process (S10) 〉
A face applying polyvinyl alcohol resin film at base material film.The applying method of base material film and polyvinyl alcohol resin film is so long as through the stretching process (S20) of back, the method that dyeing process (S30) also can not be peeled off, then be not particularly limited.For example, form adhesive phase or bond layer at the binding face of polyvinyl alcohol resin film and/or base material film, and by adhesive phase or bond layer both are fitted.
(polyvinyl alcohol resin film)
The thickness of the polyvinyl alcohol resin film that uses in the resin molding bonding process is made as below the 50 μ m.Though the polyvinyl alcohol resin film can form layer of polarizer through stretching process and the dyeing process of back, but the polyvinyl alcohol resin film in the resin molding bonding process (S10), the thickness of the polyvinyl alcohol resin film before namely stretching surpasses under the situation of 50 μ m, also can not carry out the operation of stretching process and dyeing process even if do not fit with base material film as described herein, therefore the advantage of being brought by the present invention is few.In addition, the thickness of polyvinyl alcohol resin film surpasses under the situation of 50 μ m, and the thickness that is difficult to form layer of polarizer sometimes is the following films of 25 μ m.And then the thickness of polyvinyl alcohol resin film (before stretching) preferably is made as more than the 10 μ m, more preferably is made as more than the 15 μ m.Under the situation of the thickness less than 10 μ m of polyvinyl alcohol resin film, be difficult to obtain separately the polyvinyl alcohol resin film.The thickness of polyvinyl alcohol resin film is 15～45 μ m more preferably.
As the polyvinyl alcohol resin that forms the polyvinyl alcohol resin film, can use polyvinyl acetate (PVA) is the material that the resin saponification forms.Be resin as polyvinyl acetate (PVA), except the polyvinyl acetate (PVA) as the homopolymer of vinyl acetate, but illustration with can be with the multipolymer of the monomer of vinyl acetate copolymerized other etc.As can with the monomer of vinyl acetate copolymerized other, for example can enumerate unsaturated carboxylic acid class, olefines, ethene ethers, unsaturated sulfonic acid class, have the acrylic amide of ammonium etc.
The preferred fully saponified thing of polyvinyl alcohol resin.The scope of saponification degree is preferably 80 moles of %～100 mole %, the scope of 90 moles of %～100 mole % more preferably, and then most preferably be the scope of 94 moles of %～100 mole %.If 80 moles of % of saponification degree less than, the water tolerance that forms after the layer of polarizer and the undesirable condition of the obvious deterioration of humidity resistance are arranged then.
Here said saponification degree refers to that be that in resin contained acetoxy group utilize saponifying process be changed to the value of ratio hydroxyl after than (mole %) expression as the polyvinyl acetate (PVA) of the raw material of polyvinyl alcohol resin with the unit, is the numerical value of following formula definition.Can obtain with the method for JIS K6726 (1994) regulation.
Saponification degree (mole %)=(hydroxyl value) ÷ (hydroxyl value+acetic acid radix) * 100
Saponification degree is more high, and the ratio of expression hydroxyl is more high, i.e. the ratio of the acetoxy group of expression obstruction crystallization is low.
In addition, polyvinyl alcohol resin can be the modified polyvinylalcohol that a part is modified.Can enumerate for example with alkene such as ethene, propylene; Unsaturated carboxylic acids such as acrylic acid, methacrylic acid, crotonic acid; The material that modification forms to polyvinyl alcohol resin such as the Arrcostab of unsaturated carboxylic acid, acrylic acid amides etc.The ratio of modification is preferably 30 moles of % of less than, and more preferably less than 10%.Implemented to surpass under the situation of modification of 30 moles of %, to become be difficult to adsorb the dichromatism pigment, produces the undesirable condition of polarization property step-down.
The average degree of polymerization of polyvinyl alcohol resin also is not particularly limited, but is preferably 100～10000, and more preferably 1500～8000, and then be preferably 2000～5000 especially.Here said average degree of polymerization also is the numerical value that utilizes the method for JIS K6726 (1994) regulation to obtain.
98.0～99.0 moles of %), PVA117 (saponification degree: 98.0～99.0 moles of %), PVA624 (saponification degree: 95.0～96.0 moles of %) and PVA617 (saponification degree: 94.5～95.5 moles of %) as the polyvinyl alcohol resin with this specific character, for example can enumerate the PVA124 (saponification degree: of (strain) Kuraray system; 97.0～98.8 moles of %), AH-22 (saponification degree: 97.5～98.5 moles of %), NH-18 (saponification degree: 98.0～99.0 moles of %), and N-300 (saponification degree: 98.0～99.0 moles of %) AH-26 of Japanese synthetic chemical industry (strain) system (saponification degree: for example; JAPAN VAM﹠amp for example; The JC-33 of OVAL CO.LTD (strain) (saponification degree: 99.0 moles more than the %), JM-33 (saponification degree: 93.5～95.5 moles of %), JM-26 (saponification degree: 95.5～97.5 moles of %), JP-45 (saponification degree: 86.5～89.5 moles of %), JF-17 (saponification degree: 98.0～99.0 moles of %), JF-17L (saponification degree: 98.0～99.0 moles of %), and, JF-20 (saponification degree: 98.0～99.0 moles of %) etc., these can in the formation of polyvinyl alcohol resin film of the present invention, be fit to the use.
By to aforesaid polyvinyl alcohol resin film processed, form the polyvinyl alcohol resin film.As the method for the film processed of polyvinyl alcohol resin film, limit especially.For example can enumerate that pva coating is that resin solution makes its dry solvent cast method on supporter; The polyvinyl alcohol resin melting mixing that perhaps will contain water is expressed into extrusion by melting on the supporter with extruder; And then, the polyvinyl alcohol resin aqueous solution is ejected into gel embrane method processed in the poor solvent (low-solubility solvent) etc.Wherein, owing to obtain more transparent film, so preferred casting or extrusion by melting.
Below preferred embodiment describing the manufacture method of polyvinyl alcohol resin film.Fig. 3 represents the process flow diagram of manufacture method of the polyvinyl alcohol resin film of present embodiment.In the present embodiment, usually be implemented in successively the resin bed that forms the resin bed that contains polyvinyl alcohol resin on the supporter form operation (S110), make this resin bed drying the 1st drying process (S120), peel off described resin bed and obtain the resin bed separation circuit (S130) of described resin bed from described supporter, and this resin bed is carried out dry the 2nd drying process (S140) under than the high temperature of the temperature in the 1st drying process.
As said supporter here, can enumerate for example mold release film, stainless steel band, chill bundle roller.As the method at supporter formation resin bed in the resin bed formation operation (S110), but above-mentioned solvent cast method, the extrusion by melting of illustration.For example preferably at the polyvinyl alcohol resin solution that the surface coating makes the powder dissolution of polyvinyl alcohol resin obtain in good solvent (highly dissoluble solvent) of supporter, solvent evaporates by making, the dry solvent cast method that forms.By forming the polyvinyl alcohol resin layer in this wise, can form thickness is the polyvinyl alcohol resin layer of 10～50 μ m.
As the method at supporter coating polyvinyl alcohol resin solution, can suitably select to adopt known method such as rolling method, mould rubbing method, comma rubbing method, lip formula rubbing method, spin-coating method, silk screen rubbing method, spray formula rubbing method (fountain coating method), infusion process, gunite such as line rod rubbing method, reverse rubbing method and intaglio plate coating.
The polyvinyl alcohol resin solution that uses in these methods can by for example in being warming up to 80～90 ℃ water dissolve polyvinyl alcohol be that resin obtains.
The solid component concentration of polyvinyl alcohol resin is preferably the scope of 6wt%～50wt%.When the concentration of solid constituent was lower than 6wt%, it is low that viscosity became, and the flowability when resin bed forms becomes too high, is difficult to obtain uniform film.On the other hand, if the concentration of solid constituent surpasses 50wt%, then viscosity becomes too high, and the flowability when resin bed forms became low, thereby film processed becomes difficult.
Can in polyvinyl alcohol resin solution, add plastifier.Wherein preferably use polyvalent alcohol, for example can enumerate, ethylene glycol, glycerine, propylene glycol, diethylene glycol, triethylene glycol, TEG, trimethylolpropane etc.Can also make up a plurality of.Especially preferably make spent glycol, glycerine.In addition, can also be as required and with antiblocking agents such as surfactant etc.
Form operation (S110) afterwards at resin bed, in the 1st drying process (S120), at low temperature, be generally under the baking temperature below 60 ℃, it is dried to peels off the degree that is formed at the resin bed on the supporter from supporter.Can refer to such state that coating fluid becomes solid shape to a certain degree and can peel off as film from the degree that supporter is peeled off.As long as the common moisture rate that is dried to is the following state of 30wt%, just can stably peel off whole film.If be dried to below the 20wt%, then can more easily peel off, so preferred.Here said moisture rate is represented the amount of moisture obtained with the dry weight method, can obtain with following method.
After (about 25 ℃ of 55%RH) place more than 30 minutes at normal temperatures with the PVA film after peeling off, film weight is measured.
Then, 105 ℃ dry handle 60 minutes after after the taking-up, place and be back to normal temperature until film temperature in several minutes.
Place after several minutes, the weight of film is measured again.
The following formula of value substitution that obtains.
Moisture rate=(weight-dried weight before dry)/dry preceding weight * 100 (wt/wt%)
As making it be dried to the concrete way that to peel off the degree that is formed at the resin bed on the supporter from supporter, for example preferably in reality is made, research is able to the drying condition of this state of peeling off in preliminary experiment in advance, and carries out under this condition.For example preferably make its drying 1～30 minute 40 ℃～60 ℃ temperature range, more preferably 50 ℃ of dryings about 3～20 minutes.
In the 1st drying process (S120), by in low temperature drying, and by being dried to the degree that resin bed is not exclusively peeled off from supporter dryly, the drying that is difficult to thus take place in the resin bed is shunk, and can prevent that the end in the supporter from taking place to curl.
Then, in resin bed separation circuit (S130), peel off the 1st drying process dried resin layer from supporter, obtain resin bed.In addition, in the 2nd drying process (S140), make the resin bed drying of having peeled off from supporter.In the 2nd drying process (S140), make resin bed fully dry.Therefore, compare with the 1st drying process, under the baking temperature of high temperature, make its drying.Here said high temperature is generally below 150 ℃, is preferably below 120 ℃, more preferably below 100 ℃, is preferably more than 60 ℃, more preferably more than 70 ℃.Though drying means has the method that blows hot blast, the method that contacts with hot-rolling, uses the whole bag of tricks such as method of IR well heater heating, can all suitably use.Need to prove, said baking temperature is under the situation of such drying equipment that drying oven is set such as the method that blows hot blast or IR well heater in the 1st drying process and the 2nd drying process, refer to the atmosphere temperature in the drying oven, under the situation of the drying equipment of the such contact-type of hot-rolling, refer to the surface temperature of hot-rolling.Through above operation, make the polyvinyl alcohol resin film.
The polyvinyl alcohol resin film of making of the method for present embodiment becomes the good film that curls and be suppressed.
(base material film)
Resin as being used for base material film can use for example thermoplastic resin excellent such as the transparency, physical strength, thermal stability, stretchability, can select suitable resin according to their glass transition temperature Tg or fusing point Tm.Such base material film that base material film preferably uses the temperature range of the stretching that can be suitable for thereon stacked polyvinyl alcohol resin film to stretch.
As the concrete example of thermoplastic resin, can enumerate polyolefin-based resins, polyester based resin, cyclic polyolefin hydrocarbon system resin (norbornene resin), (methyl) acrylic resin, cellulose esters and be resin, polycarbonate-based resin, polyvinyl alcohol resin, vinyl acetate and be resin, polyarylate and be resin, polystyrene resin, polyethersulfone and be resin, polysulfones and be resin, polyamide-based resin, polyimide is resin; And their potpourri, multipolymer etc.
Base material film can be the film that only is made of a kind of above-mentioned resin, also can be the film that the mixed with resin more than 2 kinds is formed.This base material film can be monofilm, also can be multilayer film.
As polyolefin-based resins, can enumerate tygon, polypropylene etc., preferably high magnification ground stretching stably easily.In addition, also can use ethene and copolymerization of propylene and propylene-ethylene copolymers of obtaining etc.Copolymerization also can be the monomer of other kinds, as can with the monomer of other kinds of copolymerization of propylene, can enumerate for example ethene, alpha-olefin.As alpha-olefin, preferably use the alpha-olefin of carbon number more than 4, more preferably the alpha-olefin of carbon number 4～10.The concrete example of the alpha-olefin of carbon number 4～10 comprises straight chain shape monoene hydro carbons such as 1-butylene, 1-amylene, 1-hexene, 1-heptene, 1-octene, 1-decene; Branch-like monoene hydro carbons such as 3-methyl-1-butene, 3-Methyl-1-pentene, 4-methyl-1-pentene; Vinyl cyclohexane etc.Propylene and can be random copolymers with other the multipolymer of monomer of its copolymerization also can be segmented copolymer.About the containing ratio from the formation unit of these other monomers in the multipolymer, can obtain by carrying out infrared ray (IR) spectroscopic assay based on the method for the 616th page of record of " macromolecule analyze Ha Application De Block Star Network (macromolecule analysis handbook) " (nineteen ninety-five, the distribution of Kinokuniya bookstore).
In above-mentioned, as the propylene resin that constitutes the propylene resin film, preferably use homopolymer, propylene-ethylene random copolymers, propylene-1-butene random copolymer, and the propylene-ethylene-1-butene random copolymer of propylene.
In addition, constitute the stereoregularity of the propylene resin of propylene resin film, be preferably isotactic or syndiotactic in fact.About the propylene resin film that is made of the propylene resin with isotactic or syndiotactic stereoregularity in fact, its property handled is better, and the physical strength excellence under hot environment.
Polyester based resin is the polymkeric substance with ester bond, mainly is the condensed polymer of polybasic carboxylic acid and polyvalent alcohol.As polybasic carboxylic acid, mainly use the dicarboxylic acid of binary, m-phthalic acid, terephthalic acid (TPA), dimethyl terephthalate (DMT), naphthalene dicarboxylic acids dimethyl ester etc. are for example arranged.In addition, employed polyvalent alcohol also mainly uses 2 yuan glycol, can enumerate propane diol, butanediol, neopentyl glycol, cyclohexanedimethanol etc.As concrete resin, can enumerate polyethylene terephthalate, polybutylene terephthalate, PEN, PBN, PTT, poly-naphthalenedicarboxylic acid propylene glycol ester, poly terephthalic acid cyclohexane dimethyl esters, poly-naphthalenedicarboxylic acid cyclohexane dimethyl esters etc.Also preferably use their hybrid resin, multipolymer.
As cyclic polyolefin hydrocarbon system resin, preferably use norbornene resin.Cyclic polyolefin hydrocarbon system resin is for being the general name that polymerized unit carries out the resin of polymerization with the cyclic olefin, can enumerate the resin that for example JPH01-240517-A, JPH03-14882-A, JPH03-122137-A etc. put down in writing.As concrete example, can enumerate open loop (being total to) polymkeric substance of cyclic olefin; The addition polymer of cyclic olefin; The multipolymer (representational is random copolymers) of alpha-olefins such as cyclic olefin and ethene, propylene; Reach the graft polymer that above-mentioned substance is formed with the modification of unsaturated carboxylic acid or derivatives thereof; And their hydride etc.As the concrete example of cyclic olefin, can enumerate the norborneol alkene monomer.
As cyclic polyolefin hydrocarbon system resin, commercially available have various products.As concrete example, can enumerate Topas (registered trademark) (Ticona corporate system), ARTON (registered trademark) (JSR (strain) system), ZEONOR (registered trademark) (Japanese ZEON (strain) system), ZEONEX (registered trademark) (Japanese ZEON (strain) system), APEL (registered trademark) (Mitsui Chemicals (strain) system) etc.
As (methyl) acrylic resin, can adopt arbitrarily suitable (methyl) acrylic resin.For example can enumerate, poly-(methyl) acrylate, methyl methacrylate-(methyl) acrylic copolymer, methyl methacrylate-(methyl) acrylate copolymer, methyl methacrylate-acrylate-(methyl) acrylic copolymer, (methyl) methyl acrylate-styrol copolymer (MS resin etc.) of polymethylmethacrylate etc., have the polymkeric substance (for example methyl methacrylate-cyclohexyl methacrylate multipolymer, methyl methacrylate-(methyl) acrylic acid norborneol ester copolymer etc.) of alicyclic alkyl etc.
Preferably can enumerate poly-(methyl) acrylic acid C1-6 Arrcostabs such as poly-(methyl) methyl acrylate.As (methyl) acrylic resin, more preferably using methyl methacrylate is resin as the methyl methacrylate of principal ingredient (50～100 weight %, be preferably 70～100 weight %).
Cellulose esters is that resin is the ester of cellulose and fatty acid.Be the concrete example of resin as cellulose esters, can enumerate cellulosic triacetate, cellulose diacetate, cellulose tripropionate, cellulose dipropionate etc.
In addition, also can enumerate substituting group with other kinds etc. and the part of these multipolymers or hydroxyl be modified material that forms etc.Wherein, special preferred cellulose triacetate.Cellulosic triacetate is commercially available a multiple product, even if from obtain easiness, the cost aspect also is favourable.As the example of the commercially available product of cellulosic triacetate, can enumerate FUJITAC (registered trademark) TD80 (Fujiphoto (strain) system), FUJITAC (registered trademark) TD80UF (Fujiphoto (strain) system), FUJITAC (registered trademark) TD80UZ (Fujiphoto (strain) system), FUJITAC (registered trademark) TD40UZ (Fujiphoto (strain) system), KC8UX2M (KONICA MINOLTA OPTO (strain) system), KC4UY (KONICA MINOLTA OPTO (strain) system) etc.
Polycarbonate-based resin be by by the carbonate group bonding engineering plastics that constitute of the polymkeric substance of monomeric unit, be the resin with high resistance to impact, thermotolerance, anti-flammability.In addition, owing to have the high transparency, so also go in the optical applications.In order to reduce photoelastic coefficient polymer backbone has been carried out the resin of modifying that is called as modified polycarbonate, the copolymerization polycarbonate of having improved the wavelength reliability etc. also by commercially available, and can be applicable in the optical applications.Such polycarbonate resin for example can be enumerated Panlite (registered trademark) (Supreme Being people changes into (strain)), Iupilon (registered trademark) (Mitsubishi's engineering plastics (strain)), SD POLYCA (registered trademark) (Sumitomo Tao Shi (strain)), CALIBER (registered trademark) (DOW Chemical (strain)) etc. by extensively commercially available.
In the base material film, except above-mentioned thermoplastic resin, can be added with proper additive arbitrarily.As such adjuvant, can enumerate for example ultraviolet light absorber, antioxidant, lubricant, plastifier, release agent, anti-coloring agent, fire retardant, nucleator, antistatic agent, pigment, colorant etc.The content with above-mentioned illustrative thermoplastic resin in the base material film is preferably 50～100 weight %, 50～99 weight % more preferably, more preferably 60～98 weight %, be preferably 70～97 weight % especially.Reason be in the base material film thermoplastic resin contain quantity not sufficient 50 weight % the time, the high transparent that thermoplastic resin has originally etc. can not be demonstrated fully out sometimes.
The thickness of the base material film before though stretch can suitably determine, usually from the viewpoint of operability such as intensity, the property handled, be preferably 1～500 μ m, more preferably 1～300 μ m, more preferably 5～200 μ m, be preferably 5～150 μ m especially.
About base material film, in order to improve the adaptation with the polyvinyl alcohol resin film, can carry out corona treatment, plasma treatment, flame treatment etc. to the surface of the side that is fitted with the polyvinyl alcohol resin film at least.In addition in order to improve adaptation, can also form thin layers such as undercoat on the surface of the side that is formed with the polyvinyl alcohol resin film of base material film.
(undercoat)
Can form undercoat on the surface of the side that is fitted with the polyvinyl alcohol resin film of base material film.As undercoat, so long as in base material film and polyvinyl alcohol resin film, bring into play the material of stronger closing force to a certain degree, then be not particularly limited.Can use for example thermoplastic resin excellent such as the transparency, thermal stability, stretchability.Particularly, can enumerate acrylic resin, polyvinyl alcohol resin, but be not limited to these.Wherein, preferably use the good polyvinyl alcohol resin of adaptation.
As the polyvinyl alcohol resin as undercoat, can enumerate for example polyvinyl alcohol resin and derivant thereof.As the derivant of polyvinyl alcohol resin, except polyvinyl formal, polyvinyl acetal etc., also can enumerate with alkene such as ethene, propylene; Unsaturated carboxylic acids such as acrylic acid, methacrylic acid, crotonic acid; The Arrcostab of unsaturated carboxylic acid; Acrylic acid amides etc. carry out modification to polyvinyl alcohol resin and the material that obtains.In the above-mentioned polyvinyl alcohol resin material, preferably use polyvinyl alcohol resin.
In order to improve the intensity of undercoat, can also in above-mentioned thermoplastic resin, add crosslinking chemical.The crosslinking chemical that adds in the thermoplastic resin can use known crosslinking chemicals such as organic system, inorganic system.For the thermoplastic resin that uses, as long as suitably select more suitably crosslinking chemical.For example, except epoxy is crosslinking chemical, isocyanate-based crosslinking chemical, the crosslinking chemical of dialdehyde system, the crosslinking chemical of metal-chelating system etc. hang down molecule crosslinked dose, can also use the crosslinking chemical of macromolecules systems such as methylolation melamine resin, daiamid epoxy resin etc.Use under the situation of polyvinyl alcohol resin as thermoplastic resin, especially preferably use daiamid epoxy resin, methylolation melamine, dialdehyde, metallo-chelate crosslinking chemical etc. as crosslinking chemical.
The thickness of undercoat is preferably 0.05～1 μ m, 0.1～0.4 μ m more preferably.If be thinner than 0.05 μ m, then the closing force of base material film and polyvinyl alcohol film can descend, if be thicker than 1 μ m, then the polarization plates thickening is therefore not preferred.
(adhesive phase)
The bonding agent that constitutes adhesive phase is called as pressure adhesive, usually comprising with acrylic resin, phenylethylene resin series, silicone-based resin etc. is base polymer, and the composition that forms to crosslinking chemicals such as wherein adding isocyanate compound, epoxy compound, aziridine cpd.And then can also in bonding agent, cooperate particulate, form the adhesive phase of display light scattering.
The thickness of adhesive phase is preferably 1～40 μ m, in the scope of the characteristic of not loss processability, permanance, is preferably coating, more preferably 3～25 μ m thinly.If 3～25 μ m then have good processability, and on the change in size of control polarizing coating, also be suitable thickness.If adhesive phase less than 1 μ m, then cohesive reduces, if surpass 40 μ m, and the undesirable condition that then takes place that bonding agent overflows easily etc.
The method that forms adhesive phase at base material film, polyvinyl alcohol resin film is not particularly limited, can contain with above-mentioned base polymer in the coating of base material face or polyvinyl alcohol resin face is the solution of each composition of representative, carry out drying and after forming adhesive phase, fit with the film of distance piece, other kinds; Also can after forming adhesive phase, distance piece be attached at base material face or polyvinyl alcohol resin face and stacked.In addition, can also when form adhesive phase, base material film or polyvinyl alcohol resin face as required the one or both in base material face or polyvinyl alcohol resin face or the adhesive phase be implemented driving fit and handle, for example corona treatment etc.
(bond layer)
As the bonding agent that constitutes bond layer, can enumerate and for example use polyvinyl alcohol resin aqueous solution, water system two-liquid type carbamate is the water system bonding agent of latex binder etc.Wherein, preferably use the polyvinyl alcohol resin aqueous solution.For the polyvinyl alcohol resin as bonding agent, the vinyl alcohol homopolymer that obtains except the polyvinyl acetate (PVA) as the homopolymer of vinyl acetate being carried out saponification handle, also have the Dichlorodiphenyl Acetate vinyl acetate and can carry out saponification to handle with other the multipolymer of monomer of its copolymerization and the ethenol system copolymer that obtains and then the hydroxyl of above-mentioned substance carried out the partially modified modified polyvinylalcohol based polymer that forms etc.Can also add polyaldehyde, soluble epoxide compound, melamine based compound, zirconium dioxide compound, zinc compound etc. in the water system bonding agent as adjuvant.Use under the situation of bonding agent of such water system, bond layer therefrom far is thinner than 1 μ m usually, even if with common observation by light microscope cross section, in fact also do not observe this bond layer.
Used the applying method of the film of water system bonding agent to be not particularly limited, the surface that can be set forth in base material film or polyvinyl alcohol resin film is coated with or pours into a mould bonding agent equably, and at overlapping another film of coated face, utilize that roller etc. is fitted, dry method etc.Usually bonding agent is coated with under 15～40 ℃ temperature after its preparation, and binding temperature is generally 15～30 ℃ scope.
Use under the situation of water system bonding agent, behind the applying film, carry out drying in order to remove water contained in the water system bonding agent.Preferred 30 ℃～90 ℃ of the temperature of drying oven.If 30 ℃ of less thaies, the tendency that then exists bonding plane to become and peel off easily.If more than 90 ℃, then deterioration might take place owing to heat in the optical property of polaroid etc.Can be made as drying time 10～1000 seconds.
After the drying, can also be in room temperature or the temperature higher slightly than room temperature, for example cultivate about 12～600 hours under the temperature about 20～45 ℃.The temperature that temperature during cultivation adopts when setting than drying usually is low.
In addition, as the bonding agent of non-water system, can also use Photocurable adhesive agent.As Photocurable adhesive agent, can enumerate potpourri of photo-curable photoreactive epoxy resin cationic polymerization initiators for example etc.
As carry out the method that film is fitted with Photocurable adhesive agent, can use known method in the past, can enumerate for example by The tape casting, line rod rubbing method, intaglio plate rubbing method, comma rubbing method, scraper plate method, mould rubbing method, dip coated method, spray-on process etc., in the bonding plane coating adhesive of film, the method for overlapping 2 films.The tape casting is 2 films as applied thing to be moved on one side to approximate vertical direction, general horizontal direction or vergence direction between the two, to its surface flow down method that bonding agent make its diffusion profile on one side.
Behind the surperficial coating adhesive of film, with clamping such as niproll and film is fitted, carry out bonding thus.In addition, can also preferably use and with roller etc. this duplexer is pressurizeed and make the method for its uniform spreading.At this moment, can use metal, rubber etc. as the material of roller.And then also preferred the employing makes this duplexer by between roller and the roller, pressurizes and method that it is sprawled.At this moment, these rollers both can be identical materials, also can be unlike materials.Use bond layer after the applying such as above-mentioned niproll, dry or solidify before thickness to be preferably 5 μ m following and more than the 0.01 μ m.
In order to improve cementability, can suitably implement surface treatments such as plasma treatment, corona treatment, ultraviolet treatment with irradiation, flame (flame) processing, saponification processing to the gluing of surfaces of film.
Handle as saponification, can enumerate the method in the aqueous solution of the alkali that impregnated in NaOH, potassium hydroxide and so on.
Using under the situation of light-cured resin as bonding agent, behind stacked film, by the irradiation active energy beam Photocurable adhesive agent is solidified.The light source of active energy beam is not particularly limited, be preferably the active energy beam that below wavelength 400nm, has luminous distribution, particularly, preferably use low pressure mercury lamp, medium pressure mercury lamp, high-pressure sodium lamp, ultrahigh pressure mercury lamp, chemical lamp, black lamp, microwave-excitation mercury lamp, metal halide lamp etc.
Intensity is penetrated in the illumination of Photocurable adhesive agent can suitably be determined according to the composition of Photocurable adhesive agent, is not particularly limited, but the exposure intensity of the effective wavelength region may of activation of polymerization initiator is preferably 0.1～6000mW/cm
2Be 0.1mW/cm in exposure intensity
2Under the above situation, the reaction time can be not long, is being 6000mW/cm
2Under the following situation, the xanthochromia of the epoxy resin due to the heating the when curing from the heat of radiation of light source and Photocurable adhesive agent seldom can take place, the deterioration of polarizing coating.The light application time of time for using according to the Photocurable adhesive agent that will solidify penetrated in the illumination of Photocurable adhesive agent, be not particularly limited, but preferably reach 10～10000mJ/cm according to the long-pending represented accumulation light quantity of form with above-mentioned exposure intensity and irradiation time
2Mode set.Be 10mJ/cm in the accumulation light quantity to Photocurable adhesive agent
2Can make it produce the spike from polymerization initiator of q.s under the above situation, curing reaction is carried out more reliably, be 10000mJ/cm
2Under the following situation, irradiation time can be not long, can keep good throughput rate.Need to prove that the thickness of the postradiation bond layer of active energy beam is generally about 0.001～5 μ m, it is above and be that 2 μ m are following, more preferably 0.01 μ m is above and be below the 1 μ m to be preferably 0.01 μ m.
Make under the situation that the Photocurable adhesive agent on base material film, the polyvinyl alcohol resin film solidifies in the irradiation that utilizes active energy beam, preferably under the transmissivity that does not reduce these films, form and aspect, the transparency etc., condition through each function of the polarization plates after whole operations, be cured.
＜stretching process (S20) 〉
Here, to carrying out uniaxial tension by base material film and the film formed stacked film of polyvinyl alcohol resin.The stretching ratio that is preferably to surpass below 5 times and 17 times carries out uniaxial tension.More preferably the stretching ratio that surpasses below 5 times and 8 times carries out uniaxial tension.If stretching ratio is below 5 times, the polyvinyl alcohol resin film can fully not be orientated, and therefore as a result of, the undesirable condition that the degree of polarization of layer of polarizer can fully not improve takes place sometimes.On the other hand, stretching ratio surpasses under 17 times the situation because the fracture of the stacked film when taking place to stretch easily, so may the back processability, operability during operation can reduce.Stretch processing in the stretching process (S20) is not limited to one section and stretches, and also can carry out with multistage.Under the situation of carrying out with multistage, preferably add up to the complete cross section of stretch processing to carry out stretch processing with the stretching ratio above 5 times.
Horizontal stretch processing that in the stretching process among the present invention (S20), can implement vertical stretch processing that the length direction to stacked film carries out, width of cloth direction is stretched etc.As vertical stretching mode, can enumerate drawing process between roller, compression stretching method etc., can enumerate stenter method etc. as horizontal stretching mode.
＜dyeing process (S30) 〉
Here, dye with the resin bed of dichromatism pigment to stacked film.As the dichromatism pigment, can enumerate for example iodine, organic dyestuff.As organic dyestuff, can use and for example can use red BR, red LR, red R, pink LB, ruby red BL, purplish red (Bordeaux) GS, sky blue LG, lemon yellow, blue BR, blue 2R, purplish blue (Navy) RY, green LG, purple LB, purple B, black H, black B, black GSP, yellow 3G, yellow R, orange LR, orange 3R, scarlet GL, scarlet KGL, Congo red, blue GL, the Si Pula orange of the blue G of brilliant violet BK, Si Pula (Supra), Si Pula GL, direct sky blue, chlorazol fast orange d S, fast black etc.These dichroic substance can be a kind of, also can be also with using more than two kinds.
About dyeing process, for example undertaken by the whole stretched film of dipping in the aqueous solution that contains the dichromatism pigment (staining solution).As staining solution, can use in dissolution with solvents the solution of above-mentioned dichromatism pigment.As the solvent of staining solution, make water usually, but also can further add the organic solvent that intermiscibility is arranged with glassware for drinking water.The concentration of dichromatism pigment is preferably 0.01～10 weight %, and more preferably 0.02～7 weight % is preferably 0.025～5 weight % especially.
Using under the situation of iodine as the dichromatism pigment, owing to can further improve dyeing efficient, so the preferred iodide that further add.As these iodide, for example can enumerate, potassium iodide, lithium iodide, sodium iodide, zinc iodide, silver iodide, lead iodide, cupric iodide, barium iodide, calcium iodide, stannic iodide, titanium iodide etc.In staining solution, the adding proportion of these iodide is preferably 0.01～20 weight %.In the iodide, preferably add potassium iodide.Add under the situation of potassium iodide, the ratio of iodine and potassium iodide is in weight ratio, is preferably 1: 5～1: 100 scope, and more preferably 1: 6～1: 80 scope is preferably 1: 7～1: 70 scope especially.
The dip time of stretched film in staining solution is not particularly limited, and is preferably 15 seconds usually～15 minutes scope, more preferably 1 minute～3 minutes.In addition, the temperature of staining solution is preferably 10～60 ℃ scope, more preferably 20～40 ℃ scope.
＜crosslinked operation 〉
Can carry out bonding crosslinking Treatment in the dyeing process.Crosslinking Treatment can be undertaken by for example flood stretched film in containing the solution of crosslinking chemical (crosslinker solution).As crosslinking chemical, can use known material in the past.For example, can enumerate boron compounds such as boric acid, borax, glyoxal, glutaraldehyde etc.These can be a kind of, also can be and with more than two kinds.
As crosslinker solution, can use the solution that in solvent, has dissolved crosslinking chemical.As solvent, can use for example water, but also can further contain the organic solvent that intermiscibility is arranged with glassware for drinking water.The concentration of the crosslinking chemical in the crosslinker solution is not limited thereto, and is preferably the scope of 1～20 weight %, more preferably 6～15 weight %.
In crosslinker solution, can add iodide.By the interpolation of iodide, can make the polarization characteristic homogenising more in the face of resin bed.As iodide, can enumerate for example potassium iodide, lithium iodide, sodium iodide, zinc iodide, silver iodide, lead iodide, cupric iodide, barium iodide, calcium iodide, stannic iodide, titanium iodide.The content of iodide is 0.05～15 weight %, 0.5～8 weight % more preferably.
The dip time of stacked film in crosslinker solution be preferably 15 seconds usually～and 20 minutes, more preferably 30 seconds～15 minutes.In addition, the temperature of crosslinker solution is preferably 10～80 ℃ scope.
＜washing procedure 〉
After crosslinked operation, preferably carry out washing procedure.As washing procedure, can implement water washing and handle.Water washing is handled usually and can be undertaken by dipping stacked film in pure water such as ion exchange water, distilled water.The water washing temperature is common 3～50 ℃, be preferably 4 ℃～20 ℃ scope.Dip time was generally for 2～300 seconds, was preferably for 3 seconds～240 seconds.
About washing procedure, can make up the carrying out washing treatment and the water washing that utilize iodide solution and handle, also can suitably use the solution of liquid alcohols such as being combined with methyl alcohol, ethanol, isopropyl alcohol, butanols, propyl alcohol.
＜drying process 〉
Also can behind washing procedure, implement drying process.As drying process, can adopt suitable arbitrarily method (for example air dry, dry, the heat drying of air-supply).For example, the baking temperature during heat drying is generally 20～95 ℃, is generally drying time about 1～15 minute.
By above operation, the polyvinyl alcohol resin film has the function as layer of polarizer, and a mask that can be manufactured on base material film has the polarizability stacked film of layer of polarizer.
(layer of polarizer)
Particularly, layer of polarizer is the layer of polarizer that forms at the polyvinyl alcohol resin film absorption orientation dichromatism pigment through uniaxial tension.Stretching ratio is preferably and surpasses 5 times, more preferably surpasses below 5 times and 17 times.
The thickness of layer of polarizer (thickness of the polyvinyl alcohol resin film after the stretching) is preferably below the 25 μ m, more preferably below the 20 μ m, is preferably more than the 2 μ m.Be made as below the 25 μ m by the thickness with layer of polarizer, can constitute slim polarizability stacked film.
＜diaphragm bonding process (S40) 〉
The face applying diaphragm of the layer of polarizer in the polarizability stacked film and the face opposition side base material film side.The applying method of layer of polarizer and diaphragm is not particularly limited.For example the binding face at layer of polarizer and/or diaphragm forms adhesive phase or bond layer, by adhesive phase or bond layer both is fitted.Be used as the material of adhesive phase, bond layer with identical at adhesive phase, the bond layer described in above-mentioned resin molding bonding process (S10) hurdle.
(diaphragm)
Diaphragm can be the simple diaphragm that does not have optical function, also can be that phase retardation film or brightness improve the diaphragm that film has optical function such the time.
Material as diaphragm is not particularly limited, and can enumerate for example cyclic polyolefin resin film; The cellulose acetate resin film that is formed by triacetyl cellulose, the such resin of diacetyl cellulose; The polyester based resin film that is formed by polyethylene terephthalate, PEN, the such resin of polybutylene terephthalate; The polycarbonate resin film; The acrylic resin film; Polypropylene-based resin film etc., the film that in this field, all the time is widely used.
As cyclic polyolefin hydrocarbon system resin, can preferably use suitable commercially available product, for example Topas (registered trademark) (Ticona corporate system), ARTON (registered trademark) (JSR (strain) system), ZEONOR (registered trademark) (Japanese ZEON (strain) system), ZEONEX (registered trademark) (Japanese ZEON (strain) system), APEL (registered trademark) (Mitsui Chemicals (strain) system) etc.To such cyclic polyolefin hydrocarbon system resin film processed and during film forming, can suitably use known methods such as solvent cast method, extrusion by melting.In addition, can also use the commercially available product of the resinous film of cyclic polyolefin hydrocarbon system of film processed in advance such as ESCENA (registered trademark) (ponding chemical industry (strain) system), SCA40 (ponding chemical industry (strain) system), ZEONOR (registered trademark) film ((strain) OPTES system).
The cyclic polyolefin resin film can be uniaxial tension or biaxial stretch-formed after film.By stretching, can give phase difference value arbitrarily to the cyclic polyolefin resin film.Usually can stretch continuously while rolling the film roller, stretch to the direct of travel of roller, direction or this two direction vertical with its direct of travel with heating furnace.The temperature of heating furnace is generally near the scope to the glass transition temperature+100 ℃ glass transition temperature of cyclic polyolefin hydrocarbon system resin.The multiplying power that stretches is generally 1.1～6 times in each direction, is preferably 1.1～3.5 times.
Therefore the common surfactivity of cyclic polyolefin resin film is poor, preferably can be to implementing surface treatments such as plasma treatment, corona treatment, ultraviolet treatment with irradiation, flame (flame) processing, saponification processing with the bonding surface of layer of polarizer.Wherein, preferably can be than the plasma treatment that is easier to implement, corona treatment.
As the cellulose acetate resin film, can preliminary election use suitable commercially available product, for example FUJITAC (registered trademark) TD80 (Fujiphoto (strain) system), FUJITAC (registered trademark) TD80UF (Fujiphoto (strain) system), FUJITAC (registered trademark) TD80UZ (Fujiphoto (strain) system), FUJITAC (registered trademark) TD40UZ (Fujiphoto (strain) system), KC8UX2M (KONICA MINOLTA OPTO (strain) system), KC4UY (KONICA MINOLTA OPTO (strain) system) etc.
In order to improve viewing angle characteristic, can form liquid crystal layer etc. on the surface of cellulose acetate resin film.In addition, also can stretch by the cellulose-based resin molding of Dichlorodiphenyl Acetate in order to give phase differential.In order to improve the cementability with polarizing coating, the cellulose-based resin molding of Dichlorodiphenyl Acetate is implemented saponification and is handled usually.Handle as saponification, can adopt the method for in the aqueous solution of the alkali of NaOH, potassium hydroxide and so on, flooding.
Can also form optical layers such as hard conating, antiglare layer, anti-reflection layer on the surface of aforesaid diaphragm.The method that forms these optical layers on the diaphragm surface is not particularly limited, and can use known method.
About the thickness of diaphragm, from the requirement of slimming, the thin thickness of preferably trying one's best is preferably below the 90 μ m, more preferably below the 50 μ m.On the contrary, if thin excessively, therefore then intensity decline, poor in processability are preferably more than the 5 μ m.
＜base material film stripping process (S50) 〉
In the manufacture method of the polarization plates of present embodiment, as shown in Figure 2, after diaphragm being fitted in the diaphragm bonding process (S40) of layer of polarizer, carry out base material film stripping process (S50).In the base material film stripping process (S50), peel off base material film from the polarizability stacked film.The stripping means of base material film is not particularly limited, and can adopt the method same with the stripping process of the common stripping film that carries out in the polarization plates of band bonding agent.Behind diaphragm bonding process (S40), can directly peel off at once, also can temporarily be wound into the stripping process that other are set behind roller shape in addition and peel off.By above operation, a mask that can be manufactured on layer of polarizer has the polarization plates of diaphragm.
(other optical layers)
In practicality, above-mentioned polarization plates can be as stacked other the polarization plates of optical layers.
In addition, said protection film also can have the function of these optical layers.
As other the example of optical layers, can enumerate certain polarized light of transmission, and reflection shows that reflective polarizing film, the surface of the polarized light of the character opposite with it have the film of the film with anti-dazzle function of concaveconvex shape, belt surface anti-reflective function, reflectance coating that the surface has reflection function, have a Transflective film, compensation film for angular field of view etc. of reflection function and transmission function simultaneously.
Show commercially available product with the reflective polarizing film of the polarized light of its opposite nature as being equivalent to certain polarized light of transmission and reflection, for example can enumerate DBEF (3M corporate system, can obtain from Sumitomo 3M (strain)), APF (3M corporate system, can from Sumitomo 3M strain) and obtain) etc.As compensation film for angular field of view, can be set forth in substrate surface coating fluid crystallinity compound and the optical compensation films of orientation has taken place, the phase retardation film that formed by polycarbonate-based resin, by the phase retardation film of cyclic polyolefin hydrocarbon system resin-shaped one-tenth etc.As the commercially available product of the optical compensation films that is equivalent at substrate surface coating fluid crystallinity compound and has taken place to be orientated, can enumerate WV film (Fujiphoto (strain) system), NH film (Nippon Oil(Nippon Mitsubishi Oil) (strain) system), NR film (Nippon Oil(Nippon Mitsubishi Oil) (strain) system) etc.In addition, as the commercially available product of the phase retardation film that is equivalent to be become by cyclic polyolefin hydrocarbon system resin-shaped, can enumerate ARTON (registered trademark) film (JSR (strain) system), ESCENA (registered trademark) (ponding chemical industry (strain) system), ZEONOR (registered trademark) film ((strain) OPTES system) etc.
Embodiment
(embodiment 1)
The making of＜polyvinyl alcohol resin film 〉
(trade name: PVA124) powder dissolution is made the polyvinyl alcohol resin aqueous solution of solid component concentration 10wt% in 90 ℃ warm water to make the fully saponified polyvinyl alcohol resin of being sold by Kuraray (strain).Utilize lip formula rubbing method to be coated with the polyvinyl alcohol resin aqueous solution that obtains with about 400 μ m thickness at the PET base material of having implemented demoulding processing.After 10 minutes, peel polyvinyl alcohol resin film from the PET base material 50 ℃ of dryings, and then 80 ℃ of dryings 5 minutes, obtain not having the polyvinyl alcohol resin film that curls.Dried thickness is 41 μ m.
＜resin molding bonding process 〉
Dissolve polyvinyl alcohol powder and crosslinking chemical in hot water, the bonding agent aqueous solution of the composition below preparing.In addition, to implementing Corona discharge Treatment on the thick base material film of the 110 μ m that formed by acrylic resin (trade name: FLX80E4, Sumitomo Chemical (strain) system), use intaglio plate coating machine is that mode about 0.2 μ m is coated with above-mentioned bonding agent aqueous solution with dried thickness.Then, behind the above-mentioned polyvinyl alcohol resin film of fitting, make its dry 3 minutes at 50 ℃, obtained stacked film.The stacked film that obtains is smooth and processing ease.
(bonding agent aqueous solution)
Water: 100 weight portions, polyvinyl alcohol resin powder ((strain) Kuraray system, average degree of polymerization 18000, trade name: KL-318): 3 weight portions, daiamid epoxy resin (crosslinking chemical, firmly change CHEMTEX (strain) system, trade name: SR650 (30)): 1.5 weight portions.
＜stretching process 〉
Use tenter frame apparatus to the free end uniaxial tensions of above-mentioned stacked film 5.8 times of 160 ℃ of enforcements.The thickness of the polyvinyl alcohol resin film after the stretching is 18 μ m.
＜dyeing process 〉
Then, with stacked film 30 ℃ as the staining solution of the mixed aqueous solution of iodine and potassium iodide in dipping about 180 seconds, make the dyeing of polyvinyl alcohol resin film after, with the unnecessary iodine liquid of 10 ℃ pure water rinsing.Then 76 ℃ as the crosslinker solution of the mixed aqueous solution of borax and potassium iodide in dipping 300 seconds.Washed for 4 seconds with 10 ℃ pure water then, remove the redundant moisture on surface at last with niproll.The cooperation ratio of the soup of each layer is as follows.Make stacked film after the dyeing 80 ℃ of dryings 5 minutes, obtained the polarizability stacked film.
(staining solution)
Water: 100 weight portions, iodine: 0.6 weight portion, potassium iodide: 10 weight portions.
(crosslinker solution)
Water: 100 weight portions, boric acid: 9.5 weight portions, potassium iodide: 5 weight portions.
＜diaphragm bonding process 〉
The bonding agent aqueous solution that preparation is same with the resin molding bonding process.After the above-mentioned bonding agent aqueous solution of the face coating of layer of polarizer and the face opposition side base material film side of above-mentioned polarizability stacked film; applying diaphragm (TAC:KC4UY of KONICA MINOLTA OPTO (strain) system) has obtained by base material film, bond layer, layer of polarizer, bond layer, these 5 layers of polarization plates that forms of diaphragm.
＜base material film stripping process 〉
Make above-mentioned polarization plates after 5 minutes, obtain polarization plates 80 ℃ of dryings.Peel off base material film from the polarization plates that obtains.Base material film is stripped from easily, has obtained by bond layer, layer of polarizer, bond layer, these 4 layers of polarization plates that forms of diaphragm.The thickness of layer of polarizer is 18 μ m.Measure the polarization property of the polarization plates that obtains with the spectrophotometer (V7100) of Japanese light splitting (strain) system.The incident direction of light is from the layer of polarizer side.Visibility compensation monomer transmissivity is 41.8%, visibility compensating polarizing degree is 99.997%, and polarization property is very excellent, be can be fully as the performance of polarization plates use.
(comparative example 1)
With embodiment 1 in the same manner to after having implemented Corona discharge Treatment on the base material film, utilize slit (gap) rubbing method directly to be coated with among the embodiment 1 the polyvinyl alcohol resin aqueous solution that is used for making the polyvinyl alcohol resin film.Then, though be implemented in 50 ℃, 10 minutes drying continuously, 80 ℃, 5 minutes dryings, take place significantly to curl because the drying of polyvinyl alcohol resin layer is shunk, in the outlet of drying oven the end bending has taken place.The dried thickness of the polyvinyl alcohol resin layer that obtains is about 39 μ m.
Claims (5)
1. the manufacture method of a polarizability stacked film, described polarizability stacked film has base material film and is formed at the layer of polarizer of a face of described base material film, and described method comprises following operation successively:
The resin molding bonding process is that the resin molding that contains polyvinyl alcohol resin below the 50 μ m obtains stacked film at a face coating thickness of base material film;
Stretching process carries out uniaxial tension to described stacked film; And
Dyeing process dyes to the described resin molding of described uniaxial tension stacked film and forms layer of polarizer with the dichromatism pigment.
2. method according to claim 1, wherein,
In the described resin molding bonding process, described resin molding is fitted in a face of described base material film by adhesive phase or bond layer.
3. method according to claim 1 and 2, wherein,
In the described resin molding bonding process, described thickness of resin film is more than the 15 μ m.
4. according to each described method in the claim 1～3, wherein,
The described resin molding that uses in the described resin molding bonding process is the resin molding that utilizes the method manufacturing that comprises following operation successively to form,
Resin bed forms operation, forms the resin bed that contains polyvinyl alcohol resin at supporter,
The 1st drying process makes the resin bed drying that is formed on the supporter,
The resin bed separation circuit is peeled off dried resin layer from described supporter, obtains described resin bed, and
The 2nd drying process makes the resin bed of having peeled off dry under than the high baking temperature of the temperature in described the 1st drying process.
5. the manufacture method of a polarization plates, described polarization plates has layer of polarizer and is formed at the diaphragm of a face of described layer of polarizer,
Described method comprises following operation successively after utilizing the described manufacture method of claim 1 to make the polarizability stacked film:
The diaphragm bonding process, the face applying diaphragm of the described layer of polarizer in described polarizability stacked film and face opposition side described base material film side; And
The base material film stripping process is peeled off described base material film from described polarizability stacked film.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2010251647 | 2010-11-10 | ||
| JP2010-251647 | 2010-11-10 | ||
| PCT/JP2011/076130 WO2012063954A1 (en) | 2010-11-10 | 2011-11-08 | Methods for producing polarizing laminate film and polarizing plate |
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| CN103201656A true CN103201656A (en) | 2013-07-10 |
| CN103201656B CN103201656B (en) | 2015-05-27 |
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| JP (2) | JP5921855B2 (en) |
| KR (2) | KR101967078B1 (en) |
| CN (1) | CN103201656B (en) |
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| WO (1) | WO2012063954A1 (en) |
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Also Published As
| Publication number | Publication date |
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| JP2012118521A (en) | 2012-06-21 |
| KR101740763B1 (en) | 2017-05-26 |
| JP2016136281A (en) | 2016-07-28 |
| JP5921855B2 (en) | 2016-05-24 |
| TW201704027A (en) | 2017-02-01 |
| TW201226189A (en) | 2012-07-01 |
| JP6339621B2 (en) | 2018-06-06 |
| TWI566937B (en) | 2017-01-21 |
| KR20170058441A (en) | 2017-05-26 |
| TWI592305B (en) | 2017-07-21 |
| WO2012063954A1 (en) | 2012-05-18 |
| CN103201656B (en) | 2015-05-27 |
| KR20140006800A (en) | 2014-01-16 |
| KR101967078B1 (en) | 2019-04-08 |
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