CN103874943A - Method for manufacturing polarizer - Google Patents

Method for manufacturing polarizer Download PDF

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Publication number
CN103874943A
CN103874943A CN201280049409.1A CN201280049409A CN103874943A CN 103874943 A CN103874943 A CN 103874943A CN 201280049409 A CN201280049409 A CN 201280049409A CN 103874943 A CN103874943 A CN 103874943A
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active energy
energy beam
tackifier
polarization plates
beam irradiation
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CN201280049409.1A
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CN103874943B (en
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古川淳
广岩梓
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1284—Application of adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/42—Polarizing, birefringent, filtering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2310/00—Treatment by energy or chemical effects
    • B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
    • B32B2310/0806—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2310/00—Treatment by energy or chemical effects
    • B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
    • B32B2310/0806—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation
    • B32B2310/0831—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation using UV radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/16—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating
    • B32B37/20—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of continuous webs only
    • B32B37/203—One or more of the layers being plastic
    • B32B37/206—Laminating a continuous layer between two continuous plastic layers
    • 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

Abstract

This method for manufacturing a polarizer is provided with the following steps, in this order: an adhesive application step in which an active-energy-ray-curable adhesive is applied to one surface of a transparent film or transparent films or one or both surfaces of a polarizing film; a bonding step in which a layered body comprising the transparent film(s) layered to one or both surfaces of the polarizing film with the aforementioned adhesive interposed therebetween is subjected to pressure so as to bond the transparent film(s) to the polarizing film; and a first active-energy-ray exposure step in which the adhesive is cured by exposing the aforementioned layered body to active-energy rays while said layered body is being conveyed in close contact with a roll rotating in the conveyance direction. The cumulative amount of ultraviolet-ray (UVB) exposure in the first active-energy-ray exposure step is between 10 and 185 mJ/cm2, inclusive.

Description

The manufacture method of polarization plates
Technical field
The present invention relates to as the manufacture method of polarization plates that forms one of useful optical component such as liquid crystal display.
Background technology
Polarizing coating is widely used as making dichroism pigment be adsorbed in polyvinyl alcohol resin film and being orientated the material forming, known have using iodine as the iodine of dichromatism pigment be polarizing coating or be polarizing coating etc. using dichromatism direct dyes as the dyestuff of dichromatism pigment.These polarizing coatings generally form polarization plates at its single or double via hyaline membranes such as tackifier laminating tri acetyl cellulose membranes.
As the method for the stacked hyaline membrane of single or double at polarizing coating, have in advance after the surface-coated active energy ray curable resin of hyaline membrane, clamp polarizing coating and hyaline membrane with a pair of niproll (doubling roller), fit thus, then, irradiate active energy beam and make its bonding curing side (patent documentation 1: TOHKEMY 2004-245925 communique, patent documentation 2: TOHKEMY 2009-134190 communique, patent documentation 3: TOHKEMY 2011-95560 communique).
The polarization plates of like this manufacturing, if active energy ray curable resin is not suitably cured, exists polarization plates entirety as played wave, to produce the curling situations such as wave volume (ウ ェ ー Block カ ー Le).When polarization plates produces wave when volume, not only bad order, and while being fitted in liquid crystal cells, thus also easily at the residual bubble of bonding plane, workability is reduced, also can become the reason that the display quality of liquid crystal display declines simultaneously.
In patent documentation 3, record irradiating active energy beam while making active energy ray curable resin solidification, made the closely sealed outer peripheral face at roller of duplexer while make it curing, thereby can suppress the generation of wave volume etc.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2004-245925 communique
Patent documentation 2: TOHKEMY 2009-134190 communique
Patent documentation 3: TOHKEMY 2011-95560 communique
Summary of the invention
Invent problem to be solved
Have by irradiate active energy beam make in the manufacture method of polarization plates of the operation of active energy ray curable resin solidification, the surface of duplexer has produced the such fluctuating of wave (hereinafter referred to as " wavy spot ") sometimes.In the time producing wavy spot in polarization plates, roll up similarly with wave, can become because of bad order the reason of the quality reduction of liquid crystal display.The object of the invention is to suppress the generation of above-mentioned wavy spot.
For the method for dealing with problems
The present invention is the manufacture method of the polarization plates that forms at the single or double laminating hyaline membrane of polarizing coating, described manufacture method possesses successively: tackifier painting process, at the tackifier of the one side of above-mentioned hyaline membrane or the single or double of above-mentioned polarizing coating coating active energy ray curable; Bonding process, exerts pressure to the duplexer forming at the stacked above-mentioned hyaline membrane of single or double of above-mentioned polarizing coating via above-mentioned tackifier, thereby makes above-mentioned hyaline membrane and the laminating of above-mentioned polarizing coating; And the 1st active energy beam irradiation process, above-mentioned duplexer is sealed in during the above-mentioned duplexer of conveyance under the state of the roller of conveyance direction rotation, above-mentioned duplexer is irradiated to active energy beam, make above-mentioned adhesive solidification; Wherein, in above-mentioned the 1st active energy beam irradiation process, the accumulated light of ultraviolet ray (UVB) is 10mJ/cm 2above and 185mJ/cm 2below.
In the invention described above, in the time that at least one party of above-mentioned hyaline membrane is acetate fiber prime system resin, effect is better.
With regard to the invention described above, after the 1st active energy beam irradiation process, also possesses the 2nd active energy beam irradiation process that above-mentioned duplexer irradiation active energy beam is made to above-mentioned adhesive solidification.
In an embodiment of the invention described above, in the 1st active energy beam irradiation process, the irradiation of above-mentioned active energy beam utilizes multiple light sources to carry out.
Invention effect
According to the present invention, can make the good polarization plates of the outward appearance being suppressed of wavy spot and wave volume.Therefore,, while using the polarization plates obtaining by manufacture method of the present invention, can provide and prevent that the workability that liquid crystal cells is fitted from reducing and the liquid crystal display of high-quality.
Accompanying drawing explanation
Fig. 1 is the diagrammatic side view that represents an embodiment of the manufacturing installation of polarization plates involved in the present invention.
Fig. 2 is the diagrammatic side view that represents an embodiment of the manufacturing installation of polarization plates involved in the present invention.
Embodiment
The present invention is the manufacture method that forms polarization plates at the single or double laminating hyaline membrane of polarizing coating, described manufacture method possesses successively: tackifier painting process, at the tackifier of the one side of hyaline membrane or the single or double of polarizing coating coating active energy ray curable; Bonding process, exerts pressure to the duplexer forming at the stacked hyaline membrane of single or double of polarizing coating via tackifier, thereby makes hyaline membrane and polarizing coating laminating; And the 1st active energy beam irradiation process, duplexer is sealed in during conveyance duplexer under the state of the roller of conveyance direction rotation, duplexer is irradiated to active energy beam, make above-mentioned adhesive solidification.In the 1st active energy beam irradiation process, the accumulated light of ultraviolet ray (UVB) is 10mJ/cm 2above and 185mJ/cm 2below.
First, the every key element using in manufacture method of the present invention is elaborated.
(polarizing coating)
The polarizing coating using in the manufacture method of polarization plates of the present invention particularly, is to make dichroism pigment be adsorbed in the polyvinyl alcohol resin film of uniaxial tension and be orientated the film forming.Polyvinyl alcohol resin film can be that resin saponification obtains by making polyvinyl acetate.Be resin as polyvinyl acetate, except the polyvinyl acetate of the homopolymer as vinyl acetate, also can enumerate the multipolymer (such as vinyl-vinyl acetate copolymer) of other monomers of vinyl acetate and energy and its copolymerization etc.As can with other monomers of vinyl acetate copolymerization, also can enumerate insatiable hunger and close carboxylic acids, olefines, vinyl ethers, unsaturated sulfonic acid class, there is the acrylic amide of ammonium etc.The saponification degree of polyvinyl alcohol resin be 85 % by mole above, preferably more than 90 % by mole, more preferably 98～100 % by mole.The average degree of polymerization of polyvinyl alcohol resin is generally 1000～10000, and preferably 1500～5000.These polyvinyl alcohol resins can carry out modification, for example, can use through the polyvinyl formal of aldehydes modification, polyvinyl acetal, polyvinyl butyral etc.
The material that such polyvinyl alcohol resin masking is formed, the former material film that can be used as polarizing coating uses.The method of polyvinyl alcohol resin masking is not particularly limited, can passes through known proper method masking in the past.The thickness of the former material film being made up of polyvinyl alcohol resin is not particularly limited, for example, be 10～150 μ m left and right.Generally can supply with by roller shape, thickness is in the scope of 20～100 μ m, be preferably in the scope of 30～80 μ m, in addition, in the scope that the width of industrial practicality is 1500～6000mm.
With regard to commercially available polyvinyl alcohol mesentery, the former material thickness of (Vinylon VF-PS#7500, Kuraray system/OPL film, M-7500, the synthetic system of Japan) is 75 μ m, the former material thickness of (Vinylon VF-PS#6000, Kuraray system, Vinylon VF-PE#6000, Kuraray system) is 60 μ m.
Polarizing coating is generally manufactured through following operation: make polyvinyl alcohol resin film dyeing and the operation (dyeing treatment process) of absorption dichromatism pigment, the operation (washing treatment process) that has the polyvinyl alcohol resin film of dichromatism pigment to wash with the operation of boric acid aqueous solution processing (boric acid treatment process) and after this boric acid aqueous solution is processed absorption with dichromatism pigment.
In addition, when the manufacture of polarizing coating, general polyvinyl alcohol resin film is by uniaxial tension, and this uniaxial tension can carry out before dyeing treatment process, also can in dyeing treatment process, carry out, and also can after dyeing treatment process, carry out.Carry out uniaxial tension after dyeing treatment process time, this uniaxial tension can carry out before boric acid treatment process, also can in boric acid treatment process, carry out.Certainly, also can in above-mentioned multiple stages, carry out uniaxial tension.
Uniaxial tension can be between the different roller of peripheral speed uniaxial tension, also can carry out uniaxial tension with hot-rolling.In addition, can be the dry type stretching stretching in atmosphere, also can be the wet type stretching and stretch under the state of solvent swell.Stretching ratio is generally 3～8 times of left and right.
In dyeing treatment process, the dyeing that utilizes dichromatism pigment of polyvinyl alcohol resin film for example by carrying out polyvinyl alcohol resin film immersion in the aqueous solution that contains dichromatism pigment.As dichromatism pigment, can use such as iodine, dichroic dye etc.Dichroic dye comprises: the dichromatism direct dyes that for example contains the bis-azo compounds such as C.I.DIRECT RED39; The dichromatism direct dyes that contains the compound such as trisazo-, four azos.It should be noted that, polyvinyl alcohol resin film is preferably implemented in advance the dip treating in water before dyeing is processed.
While using iodine as dichromatism pigment, generally adopt the method for flooding polyvinyl alcohol resin film and dye in the aqueous solution that contains iodine and potassium iodide.The content of the iodine in this aqueous solution is generally 0.01～1 weight portion with respect to every 100 weight parts waters, and the content of potassium iodide is generally 0.5～20 weight portion with respect to every 100 weight parts waters.Use iodine during as dichromatism pigment, be generally 20～40 ℃ for the temperature of the aqueous solution that dyes, the dip time (dyeing time) in this aqueous solution is generally 20～1800 seconds.
On the other hand, while using dichroic dye as dichromatism pigment, generally can adopt the method for flooding polyvinyl alcohol resin film and dye in the aqueous solution that contains dichroic dye.The content of the dichroic dye in this aqueous solution is generally 1 × 10 with respect to every 100 weight parts waters -4～10 weight portions, are preferably 1 × 10 -3～1 weight portion, is particularly preferably 1 × 10 -3～1 × 10 -2weight portion.This aqueous solution also can contain the inorganic salts such as sodium sulphate as dyeing assistant.Use dichroic dye during as dichromatism pigment, be generally 20～80 ℃ for the temperature of the aqueous dye solutions that dyes, in addition, the dip time (dyeing time) in this aqueous solution is generally 10～1800 seconds.
Boric acid treatment process is carried out in containing boron aqueous acid through the polyvinyl alcohol resin film immersion of dichromatism pigment dyeing by making.The amount of the boric acid in borated aqueous solution is generally 2～15 weight portions with respect to every 100 weight parts waters, is preferably 5～12 weight portions.While using iodine as dichromatism pigment in above-mentioned dyeing treatment process, preferably contain potassium iodide for the borated aqueous solution of this boric acid treatment process.Now, the amount of the potassium iodide in borated aqueous solution, with respect to every 100 weight parts waters, is generally 0.1～15 weight portion, preferably 5～12 weight portions.Dip time in borated aqueous solution is generally 60～1200 seconds, and preferably 150～600 seconds, further preferably 200～400 seconds.The temperature of borated aqueous solution is generally more than 40 ℃, is preferably 50～85 ℃, more preferably 55～75 ℃.
Then,, in washing treatment process, by for example being impregnated in, above-mentioned boric acid polyvinyl alcohol resin film after treatment in water, washes processing.The temperature of the water in washing processing is generally 4～40 ℃, and dip time is generally 1～120 second.After washing is processed, general enforcement is dry to be processed, and can obtain polarizing coating.Dry suitable use such as air drier, the far infra-red heater etc. processed carries out.The dry temperature of processing is generally 30～100 ℃, is preferably 50～80 ℃.The dry time of processing is generally 60～600 seconds, is preferably 120～600 seconds.
Like this, implement uniaxial tension, the dyeing that utilizes dichromatism pigment, boric acid processing and washing for polyvinyl alcohol resin film and process, can obtain polarizing coating.The thickness of this polarizing coating is generally in the scope of 5～50 μ m.
(hyaline membrane)
In the present invention, hyaline membrane is fitted in the single or double of above-mentioned polarizing coating.As forming the material of hyaline membrane, for example, can enumerate the polyester based resin of cyclic olefine resin, acetate fiber prime system resin, polyethylene terephthalate or PEN, polybutylene terephthalate and so on, polycarbonate-based resin, as the acrylic resin of polymethylmethacrylate (PMMA) and so on, as the widely used membrane material in the past in this field such as the ethylene series resin of polypropylene and so on.While making hyaline membrane be fitted in polarizing coating two-sided, each hyaline membrane can be the film of identical type, can be also different types of film, but at least one party while being cellulose acetate resin film effect better.In the time using cellulose acetate resin film, during as hyaline membrane, easily produce wavy spot, therefore apply the manufacture method of polarization plates of the present invention, the inhibition that wavy spot occurs becomes remarkable.
Cyclic olefine resin is for example to have the thermoplastic resin (being also referred to as thermoplasticity cyclic olefine resin) of the monomeric unit of the cyclic olefin (cycloolefin) that comprises norborene, polycyclic system norbornene monomer and so on.Cyclic olefine resin also can be the ring-opening polymerization polymer of above-mentioned cycloolefin or uses the hydride of the ring opening copolymer thing of two or more cycloolefin, also can be cycloolefin and chain alkene, has the addition polymer of aromatics of vinyl etc.In addition, the cyclic olefine resin of importing polar group is also effective.
When using cycloolefin and chain alkene and/or thering is the multipolymer of aromatics of vinyl, as chain alkene, can enumerate ethene, propylene etc., in addition, as the aromatics with vinyl, can enumerate styrene, α-methyl styrene, core alkyl-substituted styrene etc.In such multipolymer, the monomeric unit that comprises cycloolefin can be 50 % by mole following (preferably 15～50 % by mole).Especially,, when using cycloolefin and chain alkene and having the terpolymer of aromatics of vinyl, the monomeric unit that comprises cycloolefin, can be fewer amount as described above.In such terpolymer, the monomeric unit that comprises chain alkene is generally 5～80 % by mole, and the monomeric unit that comprises the aromatics with vinyl is generally 5～80 % by mole.
Cyclic olefine resin can the suitable commercially available product of suitable use, such as Topas(Ticona company system), Arton(JSR(strain) company's system), ZEONOR(Japan ZEON(strain) system), ZEONEX(Japan ZEON(strain) system), Apel(Mitsui Chemicals (strain) system), OXIS( great Cang industrial group system) etc.When such cyclic olefine resin masking is formed to film, can suitable use solvent casting method, the known method such as extrusion by melting.In addition, such as also can use Escena(ponding chemical industry (strain) system), SCA40(ponding chemical industry (strain) system), ZeonorFilm(Optes(strain) system) etc. the commercially available product of the resinous film of cyclic olefine of masking in advance.
Cyclic olefine resin molding also can be through uniaxial tension or biaxial stretch-formed material.Can give phase difference value arbitrarily to cyclic olefine resin molding by stretching.Stretch and generally unreel on one side and carry out continuously from film roller on one side, utilize heating furnace, stretch towards the direct of travel (length direction of film) of roller, direction (Width of film) or its both sides vertical with its direct of travel.The temperature of heating furnace is general to be adopted near the scope to the glass transition temperature+100 ℃ glass transition temperature of cyclic olefine resin.The multiplying power stretching is generally 1.1～6 times, preferably 1.1～3.5 times.
If cyclic olefine resin molding is in roller reeling condition, film is bonded to each other and has the tendency of easy generation adhesion, thus generally fit after diaphragm, then form roller volume.In addition, because of the general surfactivity of cyclic olefine resin molding poor, therefore preferably carry out the surface modification treatment such as Cement Composite Treated by Plasma, corona treatment, ultraviolet treatment with irradiation, flame (fire is scorching) processing, saponification processing with the bonding surface of polarizing coating.Wherein, be preferably and can, than the Cement Composite Treated by Plasma that is easier to implement, be particularly preferably atmospheric plasma treatment, corona treatment.
Acetate fiber prime system resin refers to cellulosic partially or completely carboxylate, for example, can enumerate and comprise cellulosic acetic acid esters, propionic ester, butyric ester, their film of mixed ester etc.More specifically, can enumerate tri acetyl cellulose membrane, diacetyl cellulose film, cellulose ethanoate propionic ester film, cellulose acetate butyrate film etc.As such cellulose esters resin film, can preferably use suitable commercially available product, for example: Fujitac TD80(Fujiphoto (strain) system), Fujitac TD80UF(Fujiphoto (strain) system), Fujitac TD80UZ(Fujiphoto (strain) system), KC8UX2M(Konica Minolta Opto(strain) system), KC8UY(Konica Minolta Opto(strain) system), Fujitac TD60UL(Fujiphoto (strain) system), KC2UAW(Konica Minolta Opto(strain) system), KC4UYW(Konica Minolta Opto(strain) system), KC6UAW(Konica Minolta Opto (strain) system) etc.
In addition, as hyaline membrane, also can suitable use give the cellulose acetate resin film of phase difference characteristics.As the commercially available product of such cellulose acetate resin film of having given phase difference characteristics, can enumerate WV BZ438(Fujiphoto (strain) system), KC4FR-1(Konica Minolta Opto(strain) system), KC4CR-1(Konica Minolta Opto(strain) system), KC4AR-1(Konica Minolta Opto(strain) system) etc.Cellulose acetate is also referred to as acetyl group cellulose, or is also referred to as cellulose ethanoate.
These cellulose acetate resin films easily absorb water, and exist the moisture rate of polarization plates to bring the situation of the lax impact in the end of polarization plates.It is more preferred that moisture rate when polarization plates is manufactured more approaches equilibrium moisture rate in manufacturing line or the roller volume custodial warehouse of keeping environment, for example dust free room of polarization plates, although also depend on the formation of stacked film, but be for example 2.0～3.5% left and right, more preferably 2.5～3.0%.The numerical value of the moisture rate of this polarization plates is measured with dry weight method, is the weight change after 105 ℃/120 minutes.
The thickness of the hyaline membrane using in the manufacture method of polarization plates of the present invention, although be preferably thin thickness, if too thin, intensity will reduce, and makes processability deteriorated.On the other hand, if too thickly can produce the problems such as the transparency reduces or stacked rear required set time is elongated.So the suitable thickness of hyaline membrane is for example 5～200 μ m, and be preferably 10～150 μ m, and 10～100 μ m more preferably.
For improving the cementability of tackifier and polarizing coating and/or hyaline membrane, also can implement the surface modification treatment such as corona treatment, flame treatment, Cement Composite Treated by Plasma, UV treatment, primary coat (primer) coating processing, saponification processing to polarizing coating and/or hyaline membrane.
In addition, can be respectively implement non-glare treated, antireflection processing, be firmly coated with the surface treatments such as processing, antistatic treatment, antifouling processing for hyaline membrane separately, or also above-mentioned processing of more than two kinds capable of being combined being implemented.In addition, hyaline membrane and/or hyaline membrane sealer also can contain the ultraviolet light absorber such as benzophenone based compound, benzotriazole based compound, or the plastifier such as phenyl phosphate based compound, phthalate compound.
In addition, hyaline membrane can have as the function of phase retardation film, as the function of brightness enhancement film, as the function of reflectance coating, as the function of semi-transparent anti-film, as the function of diffusion barrier, as optical functions such as the functions of optical compensation films.Now, for example pass through at optical functional films such as the stacked phase retardation film in the surface of hyaline membrane, brightness enhancement film, reflectance coating, semi-transparent anti-film, diffusion barrier, optical compensation films, thereby there is such function, in addition, also can give such function to hyaline membrane itself.In addition, also can, as thering is the diffusion barrier etc. of function of brightness enhancement film, make hyaline membrane there are multiple functions.
For example, the stretch processing that can record by No. 2841377 communique of the hyaline membrane date of execution this patent to above-mentioned, No. 3094113 communique of Jap.P. etc., or the processing that No. 3168850 communique is recorded of date of execution this patent, thereby give the function as phase retardation film.The phase difference characteristics of phase retardation film, can suitably select such as front phase difference value is 5～100nm, thickness direction phase difference value scope that is 40～300nm etc.In addition, for above-mentioned hyaline membrane, by adopting the method that TOHKEMY 2002-169025 communique or TOHKEMY 2003-29030 communique are recorded to form minute aperture, or by stacked different the centre wavelength of selecting reflection 2 layers above cholesteric liquid crystal layer, thereby can give the function as brightness enhancement film.
If above-mentioned hyaline membrane is formed to metal film by evaporation or sputter etc., can give the function as reflectance coating or semi-transparent anti-film.Containing fine-grained resin solution, can give the function as diffusion barrier by coating on above-mentioned hyaline membrane.In addition, by being coated with the liquid crystal compounds such as plate-like liquid crystal compounds and making its orientation on above-mentioned hyaline membrane, thereby can give the function as optical compensation films.In addition, also can make hyaline membrane contain the compound that manifests phase differential.Further, also can use suitable tackifier, make various optical functional films directly fit in polarizing coating.As the commercially available product of optical functional film, for example, can enumerate: DBEF(3M company system, can be from Sumitomo 3M(strain in Japan) obtain) etc. brightness enhancement film; The visual angle improvement films such as WV film (Fujiphoto (strain) system); ArtonFilm(JSR(strain) system), ZeonorFilm((strain) Optes system), Escena(ponding chemical industry (strain) system), VA-TAC(Konica Minolta Opto(strain) system), Sumikalight(Sumitomo Chemical (strain) system) the poor film of equiphase etc.
(active energy ray curable tackifier)
Polarizing coating and hyaline membrane are fitted via the tackifier of active energy ray curable.As active energy ray curable tackifier, from viewpoints such as weatherability, refractive index, cationically polymerizables, can enumerate by irradiating active energy beam tackifier that be cured, that comprise the epoxy based resin composition that contains epoxy resin.But, be not limited thereto, the various active energy ray curable tackifier (organic solvent is that tackifier, hot melt are tackifier, solventless adhesive etc.) that in the past used can be adopted in the manufacture of polarization plates, for example, the tackifier of the acrylic resin compositions such as acrylamide, acrylate, urethane acrylate, epoxy acrylate etc. can be comprised.
Epoxy resin refers to the compound in molecule with more than 2 epoxy radicals.From viewpoints such as weatherability, refractive index, cationically polymerizables, epoxy resin contained in the curable epoxy resin composition as tackifier is preferably, and does not contain the epoxy resin (reference example is as patent documentation 1) of aromatic rings in molecule.Can illustrate hydrogenated epoxy resin, alicyclic epoxy resin, aliphatic epoxy resin etc. as such epoxy resin.
Hydrogenated epoxy resin can be by making polyol as the raw material of aromatic epoxy resin under the existence of catalyzer, under pressurized conditions, selectivity obtains core hydrogenation polyol through core hydrogenation, then the method that this core hydrogenation polyol is carried out to glycidyl ether obtains.As aromatic epoxy resin, for example, can enumerate: the bisphenol-type epoxy resins such as the diglycidyl ether of the diglycidyl ether of bisphenol-A, the diglycidyl ether of Bisphenol F and bisphenol S; The epoxy resin of the phenol aldehyde types such as phenol novolac epoxy resins, cresol novolak epoxy and hydroxy benzaldehyde phenol novolac epoxy resins; The epoxy resin of the multifunctional types such as the glycidol ether of tetrahydroxy benzene methylmethane, the glycidol ether of tetrahydroxybenzophenone and epoxidation polyvinyl phenol etc.In hydrogenated epoxy resin, be preferably the glycidol ether of the bisphenol-A of hydrogenation.
Alicyclic epoxy resin refers to the epoxy resin in molecule with the epoxy radicals that 1 above and ester ring type ring key closes." epoxy radicals of closing with ester ring type ring key " refers to the oxygen atom-O-of the bridging structure in the structure shown in following formula.In following formula, m is 2～5 integer.
［ changing 1 ］
Figure BDA0000487966640000101
By (the CH in above-mentioned formula 2) min one or more hydrogen atoms remove and the group that obtains and other chemical constitution bondings and compound, can become alicyclic epoxy resin.(CH 2) min one or more hydrogen atoms, can also suitably replace with the straight chain-like alkyl such as methyl, ethyl.In alicyclic epoxy resin, there is the epoxy resin of oxabicyclo hexane ring (compound of m=3 in above-mentioned formula), oxabicyclo heptane ring (compound of m=4 in above-mentioned formula), demonstrate excellent cementability, so preferably use.Below, exemplified with the alicyclic epoxy resin of preferred use, be still not limited to these compounds particularly.
(a) the epoxycyclohexyl methyl epoxycyclohexane carboxylate class shown in following formula (I):
［ changing 2 ］
Figure BDA0000487966640000102
(in formula, R 1and R 2represent independently of each other the straight chain-like alkyl of hydrogen atom or carbon number 1～5.）
(b) the epoxycyclohexane carboxylate class of the alkane diol shown in following formula (II):
［ changing 3 ］
Figure BDA0000487966640000103
(in formula, R 3and R 4the straight chain-like alkyl that represents independently of each other hydrogen atom or carbon number 1～5, n represents 2～20 integer.）
(c) the epoxycyclohexyl methyl ester class of the dicarboxylic acid shown in following formula (III):
［ changing 4 ］
Figure BDA0000487966640000111
(in formula, R 5and R 6the straight chain-like alkyl that represents independently of each other hydrogen atom or carbon number 1～5, p represents 2～20 integer.）
(d) the epoxycyclohexyl methyl ethers of the polyglycol shown in following formula (IV):
［ changing 5 ］
Figure BDA0000487966640000112
(in formula, R 7and R 8the straight chain-like alkyl that represents independently of each other hydrogen atom or carbon number 1～5, q represents 2～10 integer.）
(e) the epoxycyclohexyl methyl ethers of the alkane diol shown in following formula (V):
［ changing 6 ］
Figure BDA0000487966640000113
(in formula, R 9and R 10the straight chain-like alkyl that represents independently of each other hydrogen atom or carbon number 1～5, r represents 2～20 integer.）
(f) bicyclic oxygen three spiro-compounds shown in following formula (VI):
［ changing 7 ］
Figure BDA0000487966640000114
(in formula, R 11and R 12represent independently of each other the straight chain-like alkyl of hydrogen atom or carbon number 1～5.）
(g) the bicyclic oxygen single-spiro compound shown in following formula (VII):
［ changing 8 ］
Figure BDA0000487966640000121
(in formula, R 13and R 14represent independently of each other the straight chain-like alkyl of hydrogen atom or carbon number 1～5.）
(h) the vinyl cyclohexene diepoxide class shown in following formula (VIII):
［ changing 9 ］
Figure BDA0000487966640000122
(in formula, R 15represent the straight chain-like alkyl of hydrogen atom or carbon number 1～5.）
(i) the epoxide ring amyl group ethers shown in following formula (IX):
［ changing 10 ］
(in formula, R 16and R 17represent independently of each other the straight chain-like alkyl of hydrogen atom or carbon number 1～5.）
(j) the bicyclic oxygen tristane shown in following formula (X) (ジ エ Port キ シ ト リ シ Network ロ デ カ Application) class:
［ changing 11 ］
Figure BDA0000487966640000124
(in formula, R 18represent the straight chain-like alkyl of hydrogen atom or carbon number 1～5.）
In above-mentioned illustrative alicyclic epoxy resin, from there being the reasons such as commercially available or its analog ratio is easier to obtain, more preferably use alicyclic epoxy resin below.
(A) carboxylate of 7-oxabicyclo ［ 4.1.0 ］ heptane-3-carboxylic acid and (7-oxa--bis-ring ［ 4.1.0 ］ heptan-3-yl) methyl alcohol in formula (I), R 1=R 2the compound of=H ］
(B) carboxylate of 4-methyl-7-oxabicyclo ［ 4.1.0 ］ heptane-3-carboxylic acid and (4-methyl-7-oxa--bis-ring ［ 4.1.0 ］ heptan-3-yl) methyl alcohol in formula (I), R 1=4-CH 3, R 2=4-CH 3compound
(C) carboxylate of 7-oxabicyclo ［ 4.1.0 ］ heptane-3-carboxylic acid and 1,2-ethylene glycol in formula (II), R 3=R 4the compound of=H, n=2 ］
(D) carboxylate of (7-oxabicyclo ［ 4.1.0 ］ heptan-3-yl) methyl alcohol and hexane diacid in formula (III), R 5=R 6the compound of=H, p=4 ］
(E) carboxylate of (4-methyl-7-oxabicyclo ［ 4.1.0 ］ heptan-3-yl) methyl alcohol and hexane diacid in formula (III), R 5=4-CH 3, R 6=4-CH 3, p=4 compound
(F) etherate of (7-oxabicyclo ［ 4.1.0 ］ heptan-3-yl) methyl alcohol and 1,2-ethylene glycol in formula (V), R 9=R 10the compound of=H, r=2 ］
In addition, as aliphatic epoxy resin, can enumerate the polyglycidyl ether of aliphatic polyol or its alkylene oxide addition product.More specifically, can enumerate: the diglycidyl ether of BDO; The diglycidyl ether of 1,6-hexanediol; The triglycidyl ether of glycerine; The triglycidyl ether of trimethylolpropane; The diglycidyl ether of polyglycol; The diglycidyl ether of propylene glycol; Polyglycidyl ether of the one kind or two or more alkylene oxide (oxirane, epoxypropane) of addition on the aliphatic polyols such as ethylene glycol, propylene glycol, glycerine and the polyether glycol that obtains etc.
Form the epoxy resin of tackifier that comprises epoxy based resin composition and can use separately a kind or and use two or more.The epoxide equivalent of the epoxy resin using in said composition is 30～3000g/ equivalent, the preferred scope of 50～1500g/ equivalent normally.When epoxide equivalent is during lower than 30g/ equivalent, there is the flexible reduction of the composite polarizing plate after solidifying, or the possibility that reduces of bonding strength.On the other hand, in the time exceeding 3000g/ equivalent, the possibility that in existence and tackifier, the compatibility of other contained compositions reduces.
In this tackifier, from reactive viewpoint, as the curing reaction of epoxy resin, preferably use cationic polymerization.For this reason, preferably in the curable epoxy resin composition as active energy ray curable tackifier, coordinate cationic polymerization initiators.Cationic polymerization initiators produces kation kind or lewis acid by the irradiation of luminous ray, ultraviolet ray, X ray, electron ray isoreactivity energy-ray, causes the polyreaction of epoxy radicals.Below, irradiation by active energy beam is produced to the cationic polymerization initiators that kation kind or lewis acid start the polyreaction of epoxy radicals and be called " light cationic polymerization initiators ".
Carry out for the curing method of tackifier with light cationic polymerization initiators and by irradiating active energy beam with regard to making, can solidify at normal temperatures, consider like this thermotolerance of polarizing coating or expand due to the necessity of strain reduce, from making intermembranous bonding viewpoint well very favourable.In addition, light cationic polymerization initiators produces catalytic action by light, so even if be mixed in epoxy resin, also have excellent storage stability, workability.
As light cationic polymerization initiators, for example, can enumerate: aromatic series diazo salt; The salt such as aromatic series salt compounded of iodine, aromatic series sulfonium salt; Iron-arene complex etc.
As aromatic series diazo salt, for example, can enumerate diazobenzene hexafluoro antimonate, diazobenzene hexafluorophosphate and diazobenzene hexafluoro borate etc.In addition, as aromatic series salt compounded of iodine, for example, can enumerate diphenyl iodine four (pentafluorophenyl group) borate, diphenyl iodine hexafluorophosphate, diphenyl iodine hexafluoro antimonate and two (4-nonyl phenyl) iodine hexafluorophosphate etc.
As aromatic series sulfonium salt, for example can enumerate: triphenylsulfonium hexafluorophosphate, triphenylsulfonium hexafluoro antimonate, triphenylsulfonium four (pentafluorophenyl group) borate, 4, 4 '-bis-(diphenyl sulfonium) diphenylsulfide two (hexafluorophosphate), 4, 4 '-bis-［ two (beta-hydroxy ethoxy) phenyl sulfonium ］ diphenylsulfide two (hexafluoro antimonate), 4, 4 '-bis-［ two (beta-hydroxy ethoxy) phenyl sulfonium ］ diphenylsulfide two (hexafluorophosphate), 7-［ two (p-methylphenyl) sulfonium ］-ITX hexafluoro antimonate, 7-［ two (p-methylphenyl) sulfonium ］-ITX four (pentafluorophenyl group) borate, 4-phenylcarbonyl group-4 '-diphenyl sulfonium-diphenylsulfide hexafluorophosphate, 4-(is to tert-butyl-phenyl carbonyl)-4 '-diphenyl sulfonium-diphenylsulfide hexafluoro antimonate, and 4-(is to tert-butyl-phenyl carbonyl)-4 '-bis-(p-methylphenyl) sulfonium-diphenylsulfide four (pentafluorophenyl group) borate etc.
In addition; as iron-arene complex, for example, can enumerate dimethylbenzene-cyclopentadienyl group iron (II) hexafluoro antimonate, cumene-cyclopentadienyl group iron (II) hexafluorophosphate and dimethylbenzene-cyclopentadienyl group iron (II)-tri-(trifluoromethyl sulfonyl) methanides etc.
These light cationic polymerization initiators can easily obtain commercially available product, for example, if name by trade name respectively, can enumerate " Kayarad PCI-220 ", " Kayarad PCI-620 " (above by Japanese chemical drug (strain) system), " UVI-6990 " (associating carbonide (Union Carbide) company's system), " Adeka Optomer SP-150 ", " Adeka Optomer SP-170 " (above by (strain) ADEKA system), " CI-5102 ", " CIT-1370 ", " CIT-1682 ", " CIP-1866S ", " CIP-2048S " and " CIP-2064S " (above by Japanese Cao Da (strain) system), " DPI-101 ", " DPI-102 ", " DPI-103 ", " DPI-105 ", " MPI-103 ", " MPI-105 ", " BBI-101 ", " BBI-102 ", " BBI-103 ", " BBI-105 ", " TPS-101 ", " TPS-102 ", " TPS-103 ", " TPS-105 ", " MDS-103 ", " MDS-105 ", " DTS-102 ", " DTS-103 " (learning (strain) system by greening above), " PI-2074 " (Luo Diya (Rhodia) company system), Deng.
These light cationic polymerization initiators can use separately a kind, also can be mixed with two or more.Wherein, even if the wavelength region may of aromatic series sulfonium salt more than 300nm also has UVA characteristic, therefore curability excellence, can provide the solidfied material with good mechanical strength and bonding strength, therefore preferably uses.
About the use level of light cationic polymerization initiators, with respect to epoxy resin 100 weight portions, normally 0.5～20 weight portion, preferably more than 1 weight portion, also preferably below 15 weight portions.In the use level of light cationic polymerization initiators with respect to epoxy resin 100 weight portions during lower than 0.5 weight portion, solidify insufficient, the trend that exists physical strength, bonding strength to reduce.In addition, in the time that the use level of light cationic polymerization initiators exceedes 20 weight portion with respect to epoxy resin 100 weight portions, the ionic substance in solidfied material increases, and therefore the hydroscopicity of solidfied material improves, the possibility that exists endurance quality to reduce.
In the situation that making with light cationic polymerization initiators, curable epoxy resin composition can also contain photosensitizer as required.By using photosensitizer, the reactivity of cationic polymerization improves, and can make the physical strength of solidfied material, bonding strength improve.As photosensitizer, for example, can enumerate carbonyls, organosulfur compound, persulfide, redox based compound, azo and diazo-compounds, halogenide, photo-reduction pigment etc.
For example, if enumerate the example more specifically of photosensitizer, can enumerate: benzoin methylether, benzoin iso-propylether and α, the benzoin derivatives such as alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone; Benzophenone, 2,4-dichloro benzophenone, o-benzoyl yl benzoic acid methyl esters, 4,4 '-bis-(dimethylamino) benzophenone and 4,4 '-benzophenone derivates such as bis-(diethylamino) benzophenone; The thioxanthone derivates such as CTX and ITX; The anthraquinone derivatives such as 2-chloroanthraquinone and 2-methylanthraquinone; The acridone derivativeses such as N-methylacridine ketone and N-butyl acridone; And α, α-diethoxy acetophenone, benzil, Fluorenone, xanthone, uranyl compound and halogenide etc.Photosensitizer can only use separately a kind, can also and use two or more.The photosensitizer preferably content in curable epoxy resin composition 100 weight portions is the scope of 0.1～20 weight portion.
The contained epoxy resin of tackifier solidifies by light cationic polymerization, but also can by light cationic polymerization and hot cationic polymerization, the two is cured.In the latter case, preferably also with light cationic polymerization initiators and hot cationic polymerization initiators.
As hot cationic polymerization initiators, can enumerate benzil sulfonium salt, thiophene (チ オ Off ェ ニ ウ system) salt, thiophane salt (チ オ ラ ニ ウ ム salt), benzil ammonium, pyridiniujm, hydrazine (ヒ De ラ ジ ニ ウ system) salt, carboxylate, sulphonic acid ester and amine acid imide etc.These hot cationic polymerization initiators can be used as commercially available product and easily obtain, for example, if name by trade name respectively, can enumerate " Adekaopton CP77 ", " Adekaopton CP66 " (above for Asahi Denka Co., Ltd.'s system), " CI-2639 ", " CI-2624 " (being Tso Tat Co., Ltd., Japan's system above), " Sun-aid SI-60L ", " Sun-aid SI-80L ", " Sun-aid SI-100L " (being three new chemical industry Co., Ltd. systems above) etc.
The tackifier of active energy ray curable can further contain the compound of the promotion cationic polymerizations such as oxetanes (オ キ セ タ Application) class, polyalcohols.
Oxetanes class is the compound in molecule with quaternary cyclic ethers, for example can enumerate 3-ethyl-3-hydroxymethyl oxetanes, Isosorbide-5-Nitrae-bis-［ (3-ethyl-3-oxetanyl) methoxy ］ benzene, 3-ethyl-3-(phenoxymethyl) oxetanes, two ［ (3-ethyl-3-oxetanyl) methyl ］ ether, 3-ethyl-3-(2-ethyl hexyl oxy methyl) oxetanes and phenol phenolic aldehyde oxetanes etc.These oxetanes classes can easily obtain commercially available product, for example, all name with trade name, can enumerate " ARON OXETANE OXT-101 ", " ARON OXETANE OXT-121 ", " ARON OXETANE OXT-211 ", " ARON OXETANE OXT-221 ", " ARON OXETANE OXT-212 " (being East Asia synthetic (strain) system) etc.These oxetanes classes in curable epoxy resin composition containing being proportionally generally 5～95 % by weight, being preferably 30～70 % by weight.
As polyalcohols, preferably there is not the polyvalent alcohol of the acidic-group beyond phenol hydroxyl, for example can enumerate do not have the functional group beyond hydroxyl polyol compound, polyester polyols alcoholic compound, polycaprolactone polyol compound, there is polyol compound and the polycarbonate polyol etc. of phenol hydroxyl.The molecular weight of these polyalcohols is generally more than 48, is preferably more than 62, more preferably more than 100, but also is preferably below 1000.These polyalcohols in curable epoxy resin composition containing proportional conventionally below 50 % by weight, preferably below 30 % by weight.
In the tackifier of active energy ray curable, can further coordinate the adjuvants such as ion trap agent, antioxidant, chain-transferring agent, tackifier, thermoplastic resin, filling agent, flow modifier, levelling agent, plastifier, defoamer.As ion trap agent, can enumerate the mineral compound of pulverous bismuth system, antimony system, magnesium system, aluminium system, calcium system, titanium system and their mixed stocker etc., as antioxidant, can enumerate hindered phenol is antioxidant etc.
The tackifier of active energy ray curable can use with the form of the solventless adhesive that do not contain in fact solvent composition, but each coating method has respectively optimum range of viscosities, therefore for viscosity adjustment, also can contain solvent.As solvent, the material that preferably use does not reduce the optical property of polarizing coating and well composition epoxy resin etc. dissolved, can enumerate the organic solvents such as the hydro carbons take toluene as representative, the ester class take ethyl acetate as representative.The viscosity of the tackifier of active energy ray curable used in the present invention is for example the scope of 5～1000mPas left and right, is preferably 10～200mPas, more preferably 20～100mPas.
The manufacture method > of < polarization plates
Next, manufacturing installation and the manufacture method of polarization plates of the present invention are described with reference to accompanying drawing on one side on one side.Fig. 1 is the schematic diagram of an embodiment of the manufacturing installation that represents that the manufacture method of polarization plates of the present invention uses.
The manufacturing installation of the polarization plates shown in Fig. 1 is disposed with along conveyance direction: for the tackifier apparatus for coating 11,12 of the one side coating binder at hyaline membrane 2,3; Obtain the doubling roller (niproll) 51,52 of duplexer 4 for fitting hyaline membrane 2,3 and polarizing coating 1; Make the closely sealed roller of duplexer 4 13; Be arranged on relative with the outer peripheral face of this roller 13 to the 1st active energy beam irradiation unit 31,32 of position; Be arranged at the 2nd active energy beam irradiation unit 16～18 that more leans on conveyance direction downstream than it; And niproll 19 for conveyance.
First,, at the one side of the hyaline membrane 2,3 of emitting continuously from the state that is wound into roller shape, utilize the tackifier (tackifier painting process) of tackifier apparatus for coating 11,12 coating active energy ray curables.
Then, two-sided at the polarizing coating 1 of emitting continuously from the state that is wound into roller shape, come to be stackedly coated with the hyaline membrane 2,3 of tackifier and to obtain duplexer via tackifier, this duplexer is being seized on both sides by the arms under the state between a pair of doubling roller 51,52 to conveyance direction rotation, so that the mode that at least one party's doubling roller is pressed to the direction of another doubling roller and exerting pressure, by polarizing coating 1 and hyaline membrane 2,3 laminatings, form duplexer 4(bonding process thus).
Then, make this duplexer 4 be sealed in the process of outer peripheral face limit conveyance duplexer 4 of roller 13 on limit, irradiate active energy beam from the 1st active energy beam irradiation unit 31,32 outer peripheral faces towards roller 13, make tackifier polymerizing curable (the 1st active energy beam irradiation process).
It should be noted that, be configured in the 2nd active energy beam irradiation unit 16～18th in conveyance direction downstream, for making the device of the complete polymerizing curable of tackifier (the 2nd active energy beam irradiation process), can append or omit as required, because making fully polymerizing curable of tackifier by the 2nd active energy beam irradiation process, therefore in the 1st active energy beam irradiation process, needn't make tackifier polymerizing curable completely, and then easily control the accumulated light of active energy beam so that being inhibited of wave volume, therefore preferably there is the 2nd active energy beam irradiation process.Finally make duplexer 4 by conveyance niproll 19, batch in winding roller 20 as polarization plates.Below, describe each operation in detail.
(tackifier painting process)
The coating process of tackifier on hyaline membrane 2,3 is not particularly limited, for example, can utilize scraper, line rod, mould to be coated with the various coating methods such as machine, comma coating machine, intaglio plate coating machine.Wherein, if consideration and film coated, transport circuit (パ ス ラ イ Application) degree of freedom, fabric width etc. corresponding, tackifier apparatus for coating 11,12 is preferably gravure roll (グ ラ PVC ア ロ ー Le).
While using gravure roll to carry out the coating of tackifier as tackifier apparatus for coating 11,12, the thickness (coating thickness) of the tackifier being coated with is preferably approximately 0.1～10 μ m, more preferably 0.2～4 μ m.The coating thickness of tackifier is recently adjusted with respect to the stretching than of linear velocity of hyaline membrane according to the speed of gravure roll.Generally speaking,, by making draw ratio (speed/linear velocity of gravure roll) be adjusted to 0.5～10, can make the coating thickness of tackifier be adjusted to approximately 0.1～10 μ m.More specifically, the linear velocity that makes hyaline membrane 2,3 is 10～100m/ minute, gravure roll is towards the reverse direction rotation of the conveyance direction of hyaline membrane 2,3, and the speed that makes gravure roll is 5～1000m/ minute, can make thus the coating thickness of tackifier be adjusted to approximately 0.1～10 μ m.
Tackifier, after preparation, for example, is coated with under the environment of general set point of temperature ± 5 in the scope that is adjusted into 15～40 ℃ ℃ (, when set point of temperature is 30 ℃, 30 ℃ ± 5 ℃), preferably ± 3 ℃, more preferably ± 1 ℃.
(bonding process)
In this operation, two-sided at the polarizing coating 1 of emitting continuously from the state that is wound into roller shape, carrys out the stacked hyaline membrane 11,12 that is coated with tackifier by above-mentioned operation via tackifier.This duplexer is being seized on both sides by the arms under the state between a pair of doubling roller 51,52 to conveyance direction rotation, for example, by doubling roller 51 is pressed to the direction of doubling roller 52, thereby by polarizing coating 1 and hyaline membrane 2,3 laminatings, forming duplexer 4.Now, with with respect to becoming with the vertical face of direction of pressing of doubling roller ± mode of angle in the scope of the mode of angle within the scope of 3 °, be preferably ± 1 °, particularly preferably in the mode overlapping with face perpendicular to pressing direction, make polarizing coating to conveyance between doubling roller.Like this, polarizing coating can not produce bubble nearby contacting of doubling roller with hyaline membrane.
It should be noted that, in Fig. 1, show the one side coating binder equably at hyaline membrane 2,3, make the face that is coated with tackifier of hyaline membrane 2,3 and polarizing coating 1 is overlapping and the method for utilizing doubling roller 51,52 to fit, but also can, at the two-sided coating binder equably of polarizing coating 1, fit in the overlapping hyaline membrane 2,3 of the face that is coated with tackifier the utilization laminating 51,52 of polarizing coating 1.
As the material of doubling roller 51,52, can enumerate metallic roll, rubber rollers.A side who preferably makes a pair of doubling roller 51,52 is metallic roll, and the opposing party is rubber rollers.As the mother metal of metallic roll, can use various known materials, but be preferably SUS304, more preferably implement chromium plating processing on its surface.In addition, there is no particular limitation for the material of rubber doubling roller, can enumerate EPDM, NBR, carbamate, Titan(タ イ タ Application), silicone etc.The hardness of rubber rollers there is no special restriction, normally 60～100 °, is preferably 85～95 °.It should be noted that, the hardness of rubber rollers can utilize the sclerometer based on JISK6253 to measure.As commercially available sclerometer, use the durometer " Type-A " of such as Aska company system etc.Specifically, while using the type objects compressive surface of rod grade, measure the skin resistance of rubber rollers with sclerometer.
With regard to the squeeze pressure of metallic roll and rubber rollers, be preferably Fujiphoto biplate type processed Prescale(ultralow pressure with) instantaneous pressure be 0.5～3.0MPa, more preferably 0.7～2.3MPa.There is no particular limitation for the diameter of doubling roller 51,52, normally 50～400mm.In addition, the diameter of two (a pair of) doubling rollers 51,52 can be identical, also can be different.
(the 1st active energy beam irradiation process)
Roller 13 forms outer peripheral face through the accurately machined convex surface of minute surface, make duplexer 4 be sealed at its surface while conveyance duplexer 4 makes tackifier polymerizing curable by active energy beam irradiation unit 31,32 in this process.Make tackifier polymerizing curable, and making the abundant closely sealed aspect of duplexer 4, the diameter of roller 13 is not particularly limited.Roller 13 is to be driven in rotation corresponding to the rotational speed of line speed.In addition, in the time that polymerizing curable is carried out in the irradiation that utilizes active energy beam, the chill roll that roller 13 also can be used as for making the heat heat radiation that duplexer 4 produces works.Now, the surface temperature of chill roll is preferably set to 4～30 ℃.
The light source using while carrying out the polymerizing curable of tackifier by the irradiation of active energy beam is not particularly limited, and sends out light source photodistributed but be preferably to have below wavelength 400nm.For example can enumerate 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 halid lamp as such light source.The irradiation of the active energy beam in the 1st active energy beam irradiation process is preferably divided into repeatedly to be carried out.Figure 1 illustrates: the situation that the sub irradiation of active energy beam carries out for 2 times, that is, configure the situation of 2 light sources (active energy beam irradiation unit 31 and 32) along the conveyance direction of duplexer, but be not limited to 2 times, for example also can be divided into and carrying out for 3 times.
Fig. 2 represents that the light source using in the 1st active energy beam irradiation process has been configured manufacturing installations 3, polarization plates along the conveyance direction of duplexer.In manufacturing installation shown in Fig. 2, compared with the manufacturing installation shown in Fig. 1, distinctive points is only, as using light source in the 1st active energy beam irradiation process, except active energy beam irradiation unit 31,32, also dispose active energy beam irradiation unit 33, other inscape that therefore description thereof is omitted.
In the 1st active energy beam irradiation process, take the accumulated light of the ultraviolet ray (UVB) by 13, roller as 10mJ/cm 2above and 185mJ/cm 2following mode, irradiates active energy beam to duplexer 4.Preferably take ultraviolet ray (UVB) accumulated light as 60mJ/cm 2above and 175mJ/cm 2following mode is irradiated active energy beam.When accumulated light exceedes 185mJ/cm 2time, will become the generation reason of the wavy spot in polarization plates.In addition, when accumulated light is less than 10mJ/cm 2time, irradiating in the operation (the 2nd active energy beam irradiation process) of active energy beam with horizontality thereafter, changes produced greatly and easily cure shrinkage by the accumulated light of active energy beam, therefore easily produces wave and roll up.
Each irradiation intensity to active energy ray curable tackifier determines according to the composition of each tackifier, is not particularly limited, but is preferably 10～5000mW/cm 2.If the irradiation intensity to resin combination is less than 10mW/cm 2, the reaction time long, if exceed 5000mW/cm 2, the heating during due to the heat of light source institute radiation and the polymerization of composition, therefore likely produce the deteriorated of xanthochromia that the constituent material of tackifier is composition epoxy resin etc. or polarizing coating.It should be noted that, exposure intensity is preferably the intensity for the effective wavelength region may of activation of light cationic polymerization initiators, the more preferably intensity of the wavelength region may below wavelength 400nm, the further intensity of the wavelength region may of optimal wavelength 280～320nm.
In the time that active energy beam is ultraviolet ray, long-pending body layer 4 is irradiated in the operation of active energy beam, preferably limit applies the tension force of 100～800N/m at length direction (conveyance direction) to duplexer 4, and limit reaches 0.1 second above linear velocity conveyance duplexer 4 with irradiation time.
(the 2nd active energy beam irradiation process)
In the time that the accumulated light of the active energy beam being produced by active energy beam irradiation unit 31,32 is insufficient, the 2nd later active energy beam irradiation unit 16～18 is preferably set, thereby boost active energy beam, promote duplexer 4 tackifier solidify.The accumulated light of the ultraviolet ray (UVB) in the whole operations including the 1st active energy beam irradiation process is 10mJ/cm 2above, particularly preferably so that accumulated light reaches 60～5000mJ/cm 2mode set.When the accumulated light to above-mentioned tackifier is less than 10mJ/cm 2time, the generation of spike that is derived from initiating agent is insufficient, tackifier curing insufficient.On the other hand, when this accumulated light exceedes 5000mJ/cm 2time, it is very long that irradiation time becomes, and it is unfavorable that throughput rate is improved.Now, according to combination of used film or tackifier kind etc., which kind of wavelength region may (UVA(320～390nm) or UVB(280～320nm) etc.) in required accumulated light will there are differences.
For carry out reliably the solidifying of tackifier of polarization plates (duplexer) end, for example, can enumerate and make electrodeless D bulb (バ Le Block ラ Application プ) be FUSION system " Light Hammer10 " take move with respect to film as across the mode method of arranging etc.
There is curing ratio, i.e. reaction rate in active energy ray curable resin, is preferably more than 90%, more preferably more than 95%.
(polarization plates coiling process)
The tension force that batches duplexer (polarization plates) 4 is made as to 30N/cm 2～150N/cm 2scope in.Be preferably 30N/cm 2～120N/cm 2scope in.When to be less than 30N/cm 2tension force transfer roller when volume of strip, because meeting causes the dislocation of reeling, therefore not preferred, when tension force is greater than 150N/cm 2time, roll tightly stretch tight (volume I Parties ま り) stronger, easily produce lax.
It should be noted that, batch length longer, in the time of same tension force, more easily cause and roll tightly stretch tight (phenomenon that is difficult for reverting to smooth state while unreeling), therefore can make polarization coiled sheet in volume core, make tension force on one side continuously or interim reduction on one side.Reduce in the method for tension force even if state on the implementation this so-called gradual change, tension force now also will be set to 150N/cm 2below.
Batch in the length of the polarization plates of rolling up core and be not particularly limited, but more than being preferably 100m and below 4000m.
The diameter of volume core cylindraceous is preferably 6 inches～12 inches.The diameter of volume core is the bigger the better, and more preferably 11 inches, 12 inches etc., but in the time that diameter is excessive, have the tendency that is difficult for handover or keeping.
Because the material of cylindric volume core is used at dust free room, therefore, as long as itself be difficult for producing dust and guaranteeing that suitable intensity, with the wider polarization plates of reeling width, is not particularly limited, can select FRP(fiberglass-reinforced plastic) etc.
Embodiment
Below, enumerate embodiment to be described in more detail the present invention, but the present invention is not limited to these embodiment.
［ embodiment 1 ］
(making of polarizing coating)
As the former material film of polyvinyl alcohol (PVA), the rectangular polyvinyl alcohol film of the use degree of polymerization 2400,99.9 % by mole of saponification degrees, thickness 75 μ m, width 3000mm " the synthetic system of OPL film M-7500(Japan) ".Stretching is that peripheral speed is poor to carry out by the driving niproll for the treatment of trough front and back is added.
First, not make the lax mode of former material film keep the tense situation of film, in the swelling groove of pure water that is equipped with 30 ℃, flood 80 seconds, make film fully swelling.With the swelling entrance accompanying in swelling groove and the roller velocity ratio of outlet be 1.2.Utilize after the dewatering of niproll, in the water retting groove of pure water that is equipped with 30 ℃, flood 160 seconds.The stretching ratio that makes the operating direction in this groove is 1.09 times.
Then, in the staining trough of aqueous solution that iodine/potassium iodide/water is housed counts with weight ratio 0.02/2.0/100, flood, carry out uniaxial tension with the stretching ratio of approximately 1.5 times simultaneously.Then, in the boric acid groove that potassium iodide/boric acid/water is housed counts with weight ratio 12/3.7/100 aqueous solution, at 55.5 ℃, flood 130 seconds, carry out uniaxial tension until the accumulation stretching ratio from former material reaches 5.7 times simultaneously.Then, in the boric acid groove that potassium iodide/boric acid/water is housed counts with weight ratio 9/2.4/100 aqueous solution, at 40 ℃, flood 60 seconds.
Then, in rinsing bowl, wash approximately 16 seconds with the pure water of 8 ℃, then, by the drying oven of approximately 60 ℃, the drying oven of approximately 85 ℃, the mode that adds up to 160 seconds with the residence time in these drying ovens is dried successively.Like this, obtaining absorption has iodine and makes it carry out the polarizing coating of the thickness 28 μ m of orientation.
(making of polarization plates)
As hyaline membrane, prepare the cellulose acetate resin film of having given phase difference characteristics " KC4CR-1(Konica Minolta Opto(strain) system) " of thickness 40 μ m and the tri acetyl cellulose membrane " KC8UX2MW " (Konica Minolta company system) of thickness 80 μ m.
Then, at the one side of the above-mentioned cellulose acetate resin film " KC4CR-1 " of having given phase difference characteristics, use the tackifier of tackifier apparatus for coating (Micro Chamber Doctor: Mechanology Inc. of Fuji system) coating ultraviolet ray (UVB) curing type, i.e. composition epoxy resin " KR series " (ADEKA company system, cation polymerization initiator).In addition, at the one side of above-mentioned tri acetyl cellulose membrane " KC8UX2MW ", use the tackifier of identical tackifier apparatus for coating coating ultraviolet ray (UVB) curing type, i.e. composition epoxy resin " KR series " (ADEKA company system, cation polymerization initiator).Now, the linear velocity of the stacked body of polarizing coating of tackifier apparatus for coating is made as to 25m/ minute, make the reverse rotation of gravure roll towards the conveyance direction of stacking material, make the thickness of the adhesive layer on cellulose acetate resin film " KC4CR-1 " be about 4.0 μ m, make the thickness of the adhesive layer on tri acetyl cellulose membrane " KC8UX2MW " be about 3.3 μ m(and add up to approximately 7.3 μ m).
Then, two-sided at above-mentioned polarizing coating, via above-mentioned composition epoxy resin (ultraviolet hardening tackifier), utilize niproll to make above-mentioned cellulose acetate resin film " KC4CR-1 " and tri acetyl cellulose membrane " KC8UX2MW " laminating (laminate pressure 1.5MPa).
For the polarizing coating that is fitted with above-mentioned 2 kinds of hyaline membranes, limit length direction apply the tension force of 600N/m and make it and chill roll closely sealed, limit is transferred with linear velocity 25m/ minute, it is passed through by metal halide lamp 2 lamps (GS-YUASA company system, the electric energy 130W/cm of 1 lamp) irradiate ultraviolet ray in, carry out the 1st active energy beam irradiation process, make again it pass through by electrodeless D bulb 3 lamps (the Fusion company system " Light Hammer10 " arranging afterwards, the electric energy 216W/cm of 1 lamp) irradiate ultraviolet ray in, carry out the 2nd active energy beam irradiation process, be made into thus polarization plates.
Above-mentioned electrodeless D bulb 3 lamps refer to: Width at film is arranged to unit that 6 electrodeless D bulbs form, is listed as in the length direction configuration 3 of film the device forming.
During by metal halide lamp, tri acetyl cellulose membrane " KC8UX2MW " contact that makes to fit in above-mentioned polarizing coating is set in the outer peripheral face of the chill roll of 23 ℃, from cellulose acetate resin film " KC4CR-1 " side irradiation ultraviolet radiation.Thus, can suppress the deteriorated of tackifier due to the hot impact in the 1st active energy beam irradiation process or polarizing coating.
In the 1st active energy beam irradiation process in the present embodiment, it is 172mJ/cm that metal halide lamp adds up to the total amount of the ultraviolet accumulated light of 2 lamps 2.In addition, in the 2nd active energy beam irradiation process arranging thereafter, it is 296mJ/cm that electrodeless D bulb adds up to the total amount of the ultraviolet accumulated light of 3 lamps 2.From the above, the total amount of the ultraviolet accumulated light in whole operations (the 1st and the 2nd active energy beam irradiation process) of irradiation active energy beam is 468mJ/cm 2.With regard to accumulated light herein, it is according to being, the measured value obtaining in the wavelength region may (UVB) of wavelength 280～320nm, by the analyzer (the UV Power processed Puck of Fusion UV company II) of irradiation intensity.The adaptation aspect of the polarization plates of more than making is no problem.
(ocular estimate)
For the polarization plates of as above making, utilize the reflex that irradiates fluorescent light to evaluate the situation occurred of wavy spot and wave volume.Particularly, while confirming that there is fluctuating on the surface of polarization plates, be evaluated as " having " wavy spot, unconfirmed during to fluctuating, be evaluated as " nothing " wavy spot.In addition, while confirming that polarization plates entirety has had wave, be evaluated as " having " wave volume, unconfirmed during to wave, be evaluated as " nothing " wave and roll up.Result is as shown in table 1.
［ embodiment 2 ］
Make polarizing coating pass through metal halide lamp 3 lamps (GS-YUASA company system, the electric energy 60W/cm of 1 lamp) carry out the 1st active energy beam irradiation process, make again to carry out the 2nd active energy beam irradiation process in its ultraviolet ray of passing through to be irradiated by electrodeless D bulb 1 lamp arranging afterwards (Fusion company system " Light Hammer10 ", the electric energy 180W/cm of 1 lamp).In addition, operation, is made into polarization plates similarly to Example 1.
In the 1st active energy beam irradiation process of the present embodiment, it is 173mJ/cm that metal halide lamp adds up to the total amount of the ultraviolet accumulated light of 3 lamps 2.In addition, in the 2nd active energy beam irradiation process arranging thereafter, it is 63mJ/cm that electrodeless D bulb adds up to the total amount of the ultraviolet accumulated light of 1 lamp 2.From the above, the total amount of the ultraviolet accumulated light in whole operations (the 1st and the 2nd active energy beam irradiation process) of irradiation active energy beam is 236mJ/cm 2.With regard to accumulated light herein, it is according to being, the measured value of the analyzer (the UV Power processed Puck of Fusion UV company II) of the irradiation intensity of the wavelength region may (UVB) of wavelength 280～320nm.The adaptation aspect of the polarization plates of more than making is no problem.
For the polarization plates of embodiment 2, carry out similarly to Example 1 ocular estimate.Result is as shown in table 1.
［ embodiment 3 ］
Make polarizing coating pass through metal halide lamp 1 lamp (GS-YUASA company system, the electric energy 60W/cm of 1 lamp, with 50% dim light optical filter) and carry out the 1st active energy beam irradiation process, in addition, operation, is made into polarization plates similarly to Example 1.
In the 1st active energy beam irradiation process in the present embodiment, it is 20mJ/cm that metal halide lamp adds up to the total amount of the ultraviolet accumulated light of 1 lamp 2.In addition, in the 2nd active energy beam irradiation process arranging thereafter, it is 296mJ/cm that electrodeless D bulb adds up to the total amount of the ultraviolet accumulated light of 3 lamps 2.From the above, the total amount of the ultraviolet accumulated light in whole operations (the 1st and the 2nd active energy beam irradiation process) of irradiation active energy beam is 316mJ/cm 2.With regard to accumulated light herein, it is according to being, the measured value of the analyzer (the UV Power processed Puck of Fusion UV company II) of the irradiation intensity of the wavelength region may (UVB) of wavelength 280～320nm.The adaptation aspect of the polarization plates of more than making is no problem.
For the polarization plates of embodiment 3, carry out similarly to Example 1 ocular estimate.Result is as shown in table 1.
［ comparative example 1 ］
Make polarizing coating pass through metal halide lamp 2 lamps (GS-YUASA company system, the electric energy 140W/cm of 1 lamp) and carry out the 1st active energy beam irradiation process.In addition, operation, is made into polarization plates similarly to Example 1.
In the 1st active energy beam irradiation process in this comparative example, it is 191mJ/cm that metal halide lamp adds up to the total amount of the ultraviolet accumulated light of 2 lamps 2.In addition, in the 2nd active energy beam irradiation process arranging thereafter, it is 296mJ/cm that electrodeless D bulb adds up to the total amount of the ultraviolet accumulated light of 3 lamps 2.From the above, the total amount of the ultraviolet accumulated light in whole operations (the 1st and the 2nd active energy beam irradiation process) of irradiation active energy beam is 487mJ/cm 2.With regard to accumulated light herein, it is according to being, the measured value obtaining in the wavelength region may (UVB) of wavelength 280～320nm, by the analyzer (the UV Power processed Puck of Fusion UV company II) of irradiation intensity.The adaptation aspect of the polarization plates of more than making is no problem.
For the polarization plates of comparative example 1, carry out similarly to Example 1 ocular estimate.Result is as shown in table 1.
［ comparative example 2 ］
Make polarizing coating pass through metal halide lamp 3 lamps (GS-YUASA company system, the electric energy 100W/cm of 1 lamp) and carry out the 1st active energy beam irradiation process.In addition, operation, is made into polarization plates similarly to Example 2.
In the 1st active energy beam irradiation process in this comparative example, it is 289mJ/cm that metal halide lamp adds up to the total amount of the ultraviolet accumulated light of 3 lamps 2.In addition, in the 2nd active energy beam irradiation process arranging thereafter, it is 63mJ/cm that electrodeless D bulb adds up to the total amount of the ultraviolet accumulated light of 1 lamp 2.From the above, the total amount of the ultraviolet accumulated light in whole operations (the 1st and the 2nd active energy beam irradiation process) of irradiation active energy beam is 352mJ/cm 2.With regard to accumulated light herein, it is according to being, the measured value obtaining in the wavelength region may (UVB) of wavelength 280～320nm, by the analyzer (the UV Power processed Puck of Fusion UV company II) of irradiation intensity.The adaptation aspect of the polarization plates of more than making is no problem.
For the polarization plates of comparative example 2, carry out similarly to Example 1 ocular estimate.Result is as shown in table 1.
［ comparative example 3 ］
Do not carry out the 1st active energy beam irradiation process, and make polarizing coating pass through, in the ultraviolet ray by electrodeless D bulb 3 lamps (Fusion company system " Light Hammer10 ", the electric energy 216W/cm of 1 lamp) irradiation, to carry out the 2nd active energy beam irradiation process.In addition, operation, is made into polarization plates similarly to Example 1.
In the 2nd active energy beam irradiation process in this comparative example, it is 296mJ/cm that electrodeless D bulb adds up to the total amount of the ultraviolet accumulated light of 3 lamps 2, the total amount of the ultraviolet accumulated light in whole operations (the 1st and the 2nd active energy beam irradiation process) of irradiation active energy beam is also 296mJ/cm 2.With regard to accumulated light herein, it is according to being, the measured value obtaining in the wavelength region may (UVB) of wavelength 280～320nm, by the analyzer (the UV Power processed Puck of Fusion UV company II) of irradiation intensity.The adaptation aspect of the polarization plates of more than making is no problem.
For the polarization plates of comparative example 3, carry out similarly to Example 1 ocular estimate.Result is as shown in table 1.
[table 1]
Figure BDA0000487966640000271
In table 1, empty hurdle ("-") represents not exist this.As shown in table 1, for the polarization plates of embodiment 1～3, all, without the problem of adaptation, also confirm the generation without wavy spot and wave volume simultaneously.On the other hand, for comparative example 1,2, the generation of wavy spot can be confirmed to have, for comparative example 3, the generation of wave volume can be confirmed to have.From above result, be 10mJ/cm by making the accumulated light in the 1st active energy beam irradiation process 2above and 185mJ/cm 2below, can prevent the generation of wavy spot and wave volume.
Utilizability in industry
Polarization plates of the present invention, can effectively be applied on the various displays take liquid crystal display as representative.
Symbol description
1 polarizing coating
2,3 hyaline membranes
4 duplexers (polarization plates)
11,12 tackifier apparatus for coating
13 rollers (chill roll)
16,17,18,31,32,33 active energy beam irradiation units
19 conveyance niprolls
20 winding rollers

Claims (5)

1. a manufacture method for polarization plates, is the manufacture method of the polarization plates that forms at the single or double laminating hyaline membrane of polarizing coating, and described manufacture method possesses successively:
Tackifier painting process, at the tackifier of the one side of described hyaline membrane or the single or double of described polarizing coating coating active energy ray curable;
Bonding process, exerts pressure to the duplexer forming at the stacked described hyaline membrane of single or double of described polarizing coating via described tackifier, thereby makes described hyaline membrane and the laminating of described polarizing coating; And
The 1st active energy beam irradiation process, described duplexer is sealed in during duplexer described in conveyance under the state of the roller of conveyance direction rotation, irradiates active energy beam to described duplexer, makes described adhesive solidification,
Wherein, in described the 1st active energy beam irradiation process, the accumulated light of ultraviolet ray (UVB) is 10mJ/cm 2above and 185mJ/cm 2below.
2. the manufacture method of polarization plates as claimed in claim 1, wherein, described roller is chill roll.
3. the manufacture method of polarization plates as claimed in claim 1 or 2, wherein, at least one party of described hyaline membrane is cellulose acetate resin film.
4. the manufacture method of the polarization plates as described in any one in claim 1～3, wherein, after described the 1st active energy beam irradiation process, also possesses the 2nd active energy beam irradiation process that described duplexer irradiation active energy beam is made to described adhesive solidification.
5. the manufacture method of the polarization plates as described in any one in claim 1～4, wherein, in described the 1st active energy beam irradiation process, the irradiation of described active energy beam utilizes multiple light sources to carry out.
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