CN106842403A - The manufacture method of polarizer - Google Patents
The manufacture method of polarizer Download PDFInfo
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- CN106842403A CN106842403A CN201611052849.9A CN201611052849A CN106842403A CN 106842403 A CN106842403 A CN 106842403A CN 201611052849 A CN201611052849 A CN 201611052849A CN 106842403 A CN106842403 A CN 106842403A
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
-
- 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
- G02B5/3041—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 comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—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 comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67316—Acids
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
- D06P1/67358—Halides or oxyhalides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Engineering & Computer Science (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polarising Elements (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The present invention provides a kind of manufacture method of polarizer, and it passes through to remove the PVA being dissolved in dyeing liquor can further improve productivity ratio.The manufacture method includes dyeing process, in the dyeing process, polyvinyl alcohol (PVA) resin film is immersed in the dyeing liquor containing dichroism pigment (iodine), thus PVA resin films are dyeed, dyeing liquor contains crosslinking agent (boric acid), and above-mentioned dyeing liquor is filtered using filter material.
Description
Technical field
The present invention relates to the manufacture method of polarizer.
Background technology
Since in the past, as the feed element of the polarised light in the display devices such as liquid crystal display device, and as polarization
The detecting element of light, widely uses polarization plates.Polarization plates are usually the one side or double in polarizing coating (polarizer) using bonding agent
The element of the composition of face laminating diaphragm.
Polarizer is by implementing to non-stretched polyvinyl alcohol (PVA) resin film (reel film) swelling treatment, at dyeing
It is dried to manufacture after reason, stretch processing, crosslinking Treatment, carrying out washing treatment etc..
In recent years, along with the high performance of liquid crystal display device, slimming, slimming is also required that for polarizer.Example
Such as, thickness be less than 10 μm polarizer by thermoplastic resin base material be coated with PVA system's resin solutions and make its drying and
To be formed the layered product after the layered product with PVA resins and implement above-mentioned reason everywhere as reel film this is manufactured.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2008-292935 publications
The content of the invention
Invent problem to be solved
But, in the above-mentioned dyeing process for dyeing PVA resin films (PVA resins), enter to be about to reel
In the dyeing liquor containing iodine (dichroism pigment) of the film immersion in dye bath.Now, sometimes a part of PVA from PVA systems tree
Adipose membrane is dissolved in dyeing liquor.Particularly filming to thickness is the dissolubility of less than 10 μm of polarizer (PVA resin films)
It is high.
In this case, if carrying out the continuous production of polarizer, the PVA for dissolving is accumulated in dye bath, dyeing liquor
In PVA concentration raise so that the PVA of precipitation is attached on PVA resin films, causes the dyeing of polarizer unequal.In addition,
When taking out reel film from dye bath, the de- liquid (dehydration) of dyeing liquor is deteriorated.The result is that producing the yield drop for causing polarizer
Low such problem.Additionally, in addition to the above problems, because the PVA concentration in dyeing liquor is raised, can also produce iodine in PVA
Adsorption rate (dyeing kinetics) reduction on resin film, problem as infringement productivity ratio.
As its countermeasure, disclose contacted with activated carbon by the foreign matter comprising PVA for making to be produced in bath is crosslinked so that
Adsorb the method (referring to above-mentioned patent document 1) for removing.But, activated carbon also adsorbs iodine, therefore, for needing to protect iodine concentration
Hold not preferred for constant dye bath.
It is thus impossible to the PVA being dissolved in dyeing liquor is removed, thus, as elevated for the PVA concentration in dye bath
Countermeasure, was typically updated periodically (replacing) treatment fluid before above mentioned problem is produced.But, it is many in existing dyeing process
Using iodine, KI etc. as dyeing liquor.Therefore, the problems such as environmental problem, high cost caused by the discharge from halogen,
Also the renewal (replacing) of dyeing liquor is not preferably carried out continually.
The present invention be in view of above-mentioned present situation and propose, its object is to provide a kind of manufacture method of polarizer, its lead to
Cross and remove the PVA that is dissolved in dyeing liquor and can further improve productivity ratio.
The means used to solve the problem
As the means for solving the above problems, mode of the invention, there is provided a kind of manufacture method of polarizer,
It includes dyeing process, in the dyeing process, polyvinyl alcohol (PVA) resin film is immersed in into the dyeing comprising dichroism pigment
In liquid, thus above-mentioned PVA resin films are dyeed, above-mentioned dyeing liquor contains crosslinking agent, using filter material to above-mentioned dyeing liquor
Filtered.
In addition, the manufacture method of the polarizer of aforesaid way can be following manufacture method：Make above-mentioned dyeing liquor via upper
State filter material circulation.
In addition, the manufacture method of the polarizer of aforesaid way can be following manufacture method：Above-mentioned dyeing liquor is stirred
Mix.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned crosslinking agent is boron
Compound.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned boron compound is
Boric acid.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned PVA systems resin
Its thickness of film is less than 10 μm, is formed on thermoplastic resin base material.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned crosslinking agent it is dense
It is 0.01~0.1 weight portion to spend.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned dichroism pigment
It is iodine.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned dichroism pigment
Concentration be 0.01~10 weight portion.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way：Above-mentioned dyeing liquor contains
KI.
Invention effect
As described above, mode of the invention, using the teaching of the invention it is possible to provide a kind of manufacture method of polarizer, it passes through to remove dissolving
PVA in dyeing liquor can further improve productivity ratio.
Specific embodiment
In the present embodiment, as the manufacture method for applying polarizer of the invention, enumerate as a example by following situations
Row explanation：PVA system's resin solutions are coated with thermoplastic resin base material and it is dried, so as to be formed with PVA resins
The layered product of (film), then implements each treatment using the layered product as reel film, thus manufactures the polarizer below 10 μm of thickness.
<Thermoplastic resin base material>
First, the thermoplastic resin base material used in the manufacture method for applying polarizer of the invention is illustrated.
As thermoplastic resin base material, the thermoplastic resin base material of the transparent protective film of polarizer is used as since can using in the past.
As the material for constituting thermoplastic resin base material, for example, can use the transparency, mechanical strength, heat endurance, water
Divide the excellent thermoplastic resins such as block, isotropism, draftability.As the concrete example of such thermoplastic resin, can be with
Enumerate：The celluosic resins such as tri acetyl cellulose；The polyester such as polyethylene terephthalate, PEN
Resin；Polyethersulfone resin；Polysulfone resin；Polycarbonate resin；The polyamides such as nylon, aromatic polyamide；Polyimides
Resin；The vistanexes such as polyethylene, polypropylene, ethylene-propylene copolymer；Ring with ring system structure or ENB structure
Shape vistanex (norbornene resin)；(methyl) acrylic resin；Polyarylate resin；Polystyrene resin；Poly- second
Enol resin；And their mixture.
In addition, in order to improve the adaptation with PVA resins, thermoplastic resin base material can be implemented to be surface-treated (example
Such as sided corona treatment), it is also possible to form the thin layers such as priming coat (prime coat).
Thermoplastic resin can be roughly divided into：Macromolecule is in the thermoplastic resin and height of the crystalline state of ordered arrangement
Molecule is in without ordered arrangement or only few amorphous or noncrystalline state thermoplastic of the part with ordered arrangement
Property resin.The former is referred to as crystalline state, the latter is referred to as amorphous or noncrystalline state.Correspondingly, crystalloid is formed
The thermoplastic resin of the property of state is referred to as crystalline resin, and the thermoplastic resin without such property is referred to as amorphism tree
Fat.
On the other hand, either crystalline resin or amorphous resin, will be not at the resin of crystalline state or do not reach
Resin referred to as amorphous (ァ モ Le Off ァ ス) or amorphous (non-Jing Quality to crystalline state) resin.Here, amorphous or amorphous
Resin is used with the amorphous resin difference of the property for not forming crystalline state.
As crystalline resin, for example, there are：Olefin-based resin including polyethylene (PE), polypropylene (PP)；Including
The ester system resin of polyethylene terephthalate (PET), polybutylene terephthalate (PBT) (PBT).The spy of crystalline resin
It is the general property for having and being caused macromolecule arrangement and crystallized by heating, stretching orientation one of to levy.The physical property of resin
Various change is occurred according to the degree for crystallizing.
On the other hand, for example for polypropylene (PP), crystalline resin as polyethylene terephthalate (PET)
For, the high molecular arrangement by heating, stretching is orientated and causes can be also hindered, crystallization can be suppressed.To suppress
Such polypropylene (PP) of crystallization, polyethylene terephthalate (PET) are referred to as amorphism polypropylene, amorphism and gather
Ethylene glycol terephthalate, they are referred to as amorphism olefin-based resin, amorphism ester system resin respectively.
For example in the case of polypropylene (PP), by forming atactic (the ァ sunset Network チ Star Network Agencies without stereoregularity
Make), the amorphism polypropylene (PP) for inhibiting crystallization can be produced.In addition, for example, polyethylene terephthalate
(PET) in the case of, polymerized monomer is used as by modified group as copolymerization M-phthalic acid, 1,4-CHDM,
The molecule of the crystallization of polyethylene terephthalate (PET) is hindered by copolymerization, can be made and be inhibited crystallization
Amorphism polyethylene terephthalate (PET).
The thickness of thermoplastic resin base material (before stretching) can suitably determine, but general workability from intensity, operability etc.,
The viewpoints such as thin layer are set out, and are 10~500 μm.In particular it is preferred that being 20~300 μm, more preferably 30~200 μm.Thermoplasticity
The thickness of resin base material is particularly preferred in the case of 50~150 μm.
<Polyvinyl alcohol (PVA) resin (film)>
In the manufacture method for applying polarizer of the invention, formed on above-mentioned thermoplastic resin base material and included
The layered product of PVA resins (film).Used as PVA systems resin, can use without particular limitation has thoroughly in visible region
The scattered adsorption of photosensitiveness has the PVA systems resin of the dichroic substances such as iodine, dichroic dye.
As PVA systems resin, the PVA systems resin of polarizer is used as since preferably using in the past.As PVA systems resin,
PVA or derivatives thereof can be enumerated.As the derivative of PVA, polyvinyl formal, polyvinyl acetal can be enumerated
Deng.In addition, can also enumerate：The alkene such as ethene, propylene；The unsaturated carboxylic acids such as acrylic acid, methacrylic acid, crotonic acid and
Its Arrcostab；Material after being modified using acrylamide etc..
The degree of polymerization of PVA is preferably 100~10000, more preferably 1000~10000.On saponification degree, soap is generally used
Change degree is 80~100 moles of PVA of %.
The additives such as plasticizer, surfactant can also be contained in PVA systems resin.As plasticizer, can enumerate
Polyalcohol and its condensation product etc..Specifically, can for example enumerate：It is glycerine, two glycerine, triglycerin, ethylene glycol, propane diols, poly-
Ethylene glycol etc..The usage amount of plasticizer etc. is not particularly limited, in preferably every 100 weight portion PVA systems resin for 20 weight portions with
Under.
<Layered product (reel film)>
Layered product as reel film can be by being coated with the aqueous solution containing PVA systems resin on thermoplastic resin base material
After be dried so as to form PVA resins and to obtain.In addition, layered product can be thermoplastic resin base material and PVA systems tree
The structure that lipid layer builds up across base coat layer.In addition, layered product can also be that thermoplastic resin base material and PVA resins are direct
The structure that is laminated into or be substrate layer and hydrophilic macromolecule layer integration state layered product.
The aqueous solution for example can be after being dissolved in appropriate heating by the powder or crushed material of PVA systems resin, cut-out thing etc.
Water (hot water) in prepare.The concentration of the aqueous solution is preferably set to 2~20 weight portions relative to the weight portion of water 100, more preferably
It is 4~10 weight portions.
Painting solution can suitably select to use such as bar rubbing method, reversion coating on thermoplastic resin base material
The rolling methods such as method, intaglio plate coating, spin-coating method, silk screen rubbing method, jetting type rubbing method, dip coating, spraying process, die coating method, comma
Coating (ト of カ Application マ Us one) method, lip rubbing method, spin-coating method etc..
In the case where thermoplastic resin base material has priming coat, the direct painting solution on the priming coat.The opposing party
Face, in the case where thermoplastic resin base material does not have priming coat, the direct painting solution on substrate layer.Need explanation
It is that drying temperature is preferably set to 50~200 DEG C, more preferably 60~150 DEG C.Drying time is preferably set to 5~30 minutes.
According to obtaining in the case of the stretching ratio of PVA resins in the stretch processing for considering to implement layered product
The thickness of polarizer is that less than 10 μm of thickness is formed.The thickness of non-stretched PVA resins is preferably set to 3~20 μ
M, more preferably 5~15 μm.
<Treatment process>
In the manufacture method for applying polarizer of the invention, to layered product (reel film) at least implement dyeing treatment and
Stretch processing.In addition, in the manufacture method for applying polarizer of the invention, it is possible to implement crosslinking Treatment.Dyeing process,
Bath is respectively processed in crosslinking Treatment and stretch processing using dye bath, crosslinking bath and stretch bath respectively.In the situation using treatment bath
Under, it is possible to use the treatment fluid (aqueous solution etc.) corresponding with each treatment.
<Dyeing process>
In dyeing process, by the PVA resins that make iodine or dichroic dye be adsorbed in layered product and be orientated come
Carry out dyeing treatment.In dyeing process, dyeing treatment can be carried out together with stretch processing.
Dyeing treatment is carried out by the way that layered product is immersed in the dyeing liquor in dye bath into (dye bath).As dyeing
Liquid, generally iodine solution.Iodine aqueous solution as iodine solution can be used by the use of iodine and contained as the iodide of dissolution aids
There is aqueous solution of iodide ion etc..
As iodide, it is possible to use for example：KI, lithium iodide, sodium iodide, zinc iodide, silver iodide, lead iodide, iodine
Change copper, barium iodide, calcium iodide, stannic iodide, titanium iodide etc..As iodide, preferably KI.In addition, in the present embodiment
The iodide for using are also same with above-mentioned iodide in the case of being used in other operations.
Iodine concentration in iodine solution is preferably set to 0.01~10 weight portion relative to the weight portion of solvent 100, more preferably
0.02~5 weight portion, more preferably 0.1~1.0 weight portion.Iodide concentration preferably sets relative to the weight portion of solvent 100
It is set to 0.1~10 weight portion, more preferably 0.2~8 weight portion.During iodine staining, the temperature of iodine solution is preferably set to 20~50
DEG C, more preferably 25~40 DEG C.Dip time is preferably set to 10~300 seconds, more preferably 20~240 seconds.Need explanation
, dyeing time can be soaked according to the mode that can reach the degree of polarization or transmissivity specified within the optional time
Stain.
<Stretching process>
In stretching process, dry type stretching treatment and wet tensile treatment can be used.In stretching process, by layer
Stack implements uniaxial tension to carry out stretch processing.Uniaxial tension can be the longitudinal direction carried out relative to the length direction of layered product
Any one in stretching and the cross directional stretch that is carried out relative to the width of layered product.
In cross directional stretch, it is also possible to while carrying out stretching in width while being shunk in length direction.As transverse direction
Stretching mode, can enumerate for example：The fixing end monoaxial stretching method of one end is fixed via stenter, do not fix the freedom of one end
End monoaxial stretching method etc..
On the other hand, in longitudinal stretching, it is possible to use for example：Drawing process, compression stretching method between roller, use tentering
Drawing process of machine etc..In addition, stretch processing can also be carried out with multistage.Additionally, stretch processing can be drawn by using twin shaft
Stretch, oblique extension etc. is carried out.
Dry type stretching treatment can widely set temperature range during stretching layered product, in this respect preferably.In dry type
In stretch processing, preferably by layered product be heated to 50~200 DEG C, more preferably 80~180 DEG C, more preferably 100~
Stretch processing is carried out in the state of 160 DEG C.In stretching process, including in the case of dry type stretching treatment, preferably in dyeing process
Preceding implementation dry type stretching treatment.
In the treatment fluid used in wet tensile treatment, iodide can be contained.Contain iodide in treatment fluid
In the case of, iodide concentration is preferably set to 0.1~10 weight portion, more preferably 0.2~5 weight relative to the weight portion of solvent 100
Amount part.Treatment temperature in wet tensile method is preferably set to more than 25 DEG C, more preferably 30~85 DEG C, further for 50~
70℃.Dip time is preferably set to 10~800 seconds, more preferably 30~500 seconds.Furthermore it is possible to dyeing treatment, crosslinking at
Reason implements stretch processing together.
In stretching process, relative to layered product the original length, in the way of being calculated as 4~8 times by total stretching ratio
Carry out stretch processing.Total stretching ratio is preferably 5~7 times.It should be noted that total stretching ratio refers to beyond stretching process
Operation etc. in stretching in the case of include the accumulation stretching ratio of stretching in other operations.Total stretching ratio is being examined
Suitably determined in the case of considering the stretching ratio in other operations etc..
When always stretching ratio is low, orientation is not enough, it is difficult to obtain the polarizer of optical characteristics high (degree of polarization).On the other hand,
When always stretching ratio is too high, tension failure is susceptible to.In addition, polarizer becomes too thin, the processability in subsequent handling has can
Can reduce.
In stretching process, such as " No. 4751481 publications of Japanese Patent No. " it is described, auxiliary that can be in atmosphere
Implement wet tensile treatment after stretch processing.The draft temperature in assisting tension treatment in atmosphere preferably presets
For 60~180 DEG C, further be 95~150 DEG C of temperature so high.In addition, in atmosphere assisting tension treatment in drawing
Stretch multiplying power and be preferably set to 1.3~4 times, be more preferably set as 1.5~3 times.In addition, the assisting tension in atmosphere processes it
Treatment temperature in the wet tensile treatment implemented afterwards is preferably set to 50~80 DEG C, more preferably 60~70 DEG C.Dip time
It is preferably set to 5~120 seconds, more preferably 10~60 seconds.In addition, the stretching ratio preferably always stretching times in wet tensile treatment
Rate is set as 4~7 times, more preferably 5~6 times.
In stretching process, including in atmosphere assisting tension treatment and wet tensile process in the case of, preferably
Assisting tension treatment in implementing atmosphere before dyeing treatment, the implementation wet tensile treatment after dyeing treatment.It is this
In the case of, the treatment bath for wet tensile treatment is also used as crosslinking bath, preferably implements at crosslinking together with wet tensile treatment
Reason.
<Cross-linking process step>
In cross-linking process step, crosslinking Treatment is carried out using boron compound as crosslinking agent.Crosslinking Treatment can with dyeing at
Reason, stretch processing are carried out together.In addition, crosslinking Treatment can be divided into repeatedly carrying out.As boron compound, it is possible to use such as boron
Acid, borax etc..The general form with the aqueous solution or water-organic solvent mixed solution of boron compound is used.
In the case of using boric acid aqueous solution, heat resistance is assigned by the degree of cross linking, therefore, the boric acid concentration of boric acid aqueous solution
1~10 weight portion, more preferably 2~7 weight portions are preferably set to relative to the weight portion of solvent 100.In boric acid aqueous solution etc.
The iodide such as KI can be contained.In the case of containing iodide in boric acid aqueous solution, iodide concentration is relative to water 100
Weight portion is preferably set to 0.1~10 weight portion, more preferably 0.5~8 weight portion.
Crosslinking Treatment can be carried out by the way that layered product is immersed in boric acid aqueous solution etc..Treatment temperature in crosslinking Treatment
Degree is preferably set to more than 25 DEG C, and more preferably 30~85 DEG C, be further 30~60 DEG C.Process time is preferably set to 5~
800 seconds, more preferably 8~500 seconds.
<Insoluble operation>
In the manufacture method for applying polarizer of the invention, to layered product implement dyeing treatment or crosslinking Treatment it
Before can implement insoluble treatment.The purpose of insoluble operation is to implement for making PVA resins undissolved insoluble
Treatment.
In insoluble operation, can be by making the PVA resins in layered product be immersed in such as boric acid or containing boron
Insoluble treatment is carried out in the solution of the boron compounds such as sand.Solution is general with the aqueous solution or the shape of water-organic solvent mixed solution
State is used.
In the case of using boric acid aqueous solution, the boric acid concentration of boric acid aqueous solution preferably sets relative to the weight portion of solvent 100
It is set to 1~4 weight portion.Treatment temperature in insoluble operation is preferably set to more than 25 DEG C, more preferably 30~85 DEG C, enters one
Walk is 30~60 DEG C.Process time is preferably set to 5~800 seconds, more preferably 8~500 seconds.
<Washing procedure>
In the manufacture method for applying polarizer of the invention, dyeing treatment, stretch processing can be implemented to layered product
And further implement crosslinking Treatment, but carrying out washing treatment can be implemented after these treatment are implemented.
In washing procedure, it is possible to use liquor kalii iodide carries out carrying out washing treatment.Iodate potassium concn in liquor kalii iodide
0.5~10 weight portion, more preferably 0.5~8 weight portion, more preferably 1 are preferably set to relative to the weight portion of solvent 100
~6 weight portions.
In the carrying out washing treatment using liquor kalii iodide, its treatment temperature is preferably set to 5~60 DEG C, more preferably 10~
40℃.Dip time is preferably set to 1~120 second, more preferably 3~90 seconds.Using the rank of the carrying out washing treatment of liquor kalii iodide
As long as just it is not particularly limited before section dried process.
In addition, as carrying out washing treatment, it is possible to implement water washing.Water washing is immersed in by by PVA systems resin
Carried out in the pure water such as ion exchange water, distilled water.Water washing temperature is preferably set to 5~50 DEG C, more preferably 10~45 DEG C,
More preferably 15~40 DEG C.Dip time is preferably set to 5~300 seconds, more preferably 10~240 seconds.
In washing procedure, for example can also may be used using carrying out washing treatment and the water washing combination of liquor kalii iodide
To use the solution for being suitably combined with the liquid alcohols such as methyl alcohol, ethanol, isopropanol, butanol, propyl alcohol.
<Drying process>
In addition, in the manufacture method for applying polarizer of the invention, it is final to implement dry after implementing above-mentioned each treatment
Dry treatment, so as to manufacture polarizer.In dried process, corresponding to the moisture rate needed for resulting polarizer (film), setting
Optimal drying time and drying temperature.Specifically, drying temperature is preferably set to 20~150 DEG C, more preferably 40~100
℃.When drying temperature is too low, drying time is elongated, it is impossible to efficiently manufactured, therefore not preferred.On the other hand, temperature is dried
When spending high, the polarizer deterioration for obtaining is deteriorated in terms of optical characteristics and tone.Heat drying time is preferably set to 1~
10 minutes.
<Water soluble antioxidant>
In the manufacture method for applying polarizer of the invention, at least one work that can be after above-mentioned dyeing process
The treatment using the treatment fluid containing at least one water soluble antioxidant is carried out in sequence.
In treatment using the treatment fluid containing water soluble antioxidant, that layered product is implemented after dyeing treatment is each
Contain water soluble antioxidant in any at least one in each bath used in treatment.Or, individually implement to utilize in addition
The treatment of the treatment fluid containing water soluble antioxidant.Using the treatment fluid containing water soluble antioxidant treatment preferably with friendship
Connection treatment and/or stretch processing are carried out together.
It should be noted that crosslinking Treatment, stretch processing can be entered by carrying out being uniformly processed for multiple treatment simultaneously
OK.Carry out at the same time in being uniformly processed of multiple treatment, water soluble antioxidant is contained in the bath used during this is uniformly processed.
In addition, in the multistage for individually carrying out crosslinking Treatment and stretch processing in addition is processed, in any of crosslinking Treatment and stretch processing
Contain water soluble antioxidant at least one treatment.
As water soluble antioxidant, can enumerate for example：Ascorbic acid (vitamin C), arabo-ascorbic acid, thio sulphur
Acid, sulfurous acid, chlorogenic acid, citric acid, Rosmarinic acid and their salt etc..
As salt, alkali metal salts such as sodium salt, sylvite etc. can be enumerated.
Wherein, ascorbic acid, erythorbate, thiosulfate, sulphite are preferably used.These water-soluble antioxygens
Agent can be used alone a kind of or be applied in combination two or more.
The addition of water soluble antioxidant according to dyeing process after each treatment fluid contained by dichroic substance (iodine
Or dichroic dye) pollution concentration determine.The pollution concentration caused by dichroic substance in the treatment fluid of pollution is higher,
The addition of the water soluble antioxidant for then adding is also more.
Throughout reason liquid in, preferably according to water soluble antioxidant concentration relative to the weight portion of solvent 100 be 0.005~
The mode of 1 weight portion adds water soluble antioxidant, more preferably 0.005~0.5 weight portion.The concentration of water soluble antioxidant
In the case of less than 0.005 weight portion, the ratio of the water soluble antioxidant in treatment fluid after pollution reduces, it is impossible to fully suppression
The reduction of the characteristic (monomer transmissivity, degree of polarization) of the polarizer obtained by system.On the other hand, the concentration of water soluble antioxidant
In the case of more than 1 weight portion, the ratio increase of the water soluble antioxidant in bath, therefore, resulting polarizer decolourizes, thoroughly
Penetrate rate rising.Accompany with this, it is possible to need to improve the iodine concentration of dye bath, but asked in the absence of reduction etc. in terms of optical characteristics
Topic.
<Polarizer>
The polarizer manufactured by the manufacture method for applying polarizer of the invention is formed on thermoplastic resin base material,
But above-mentioned thermoplastic resin base material can not also be used and non-stretched PVA resins film is implemented above-mentioned each as reel film
Process to manufacture.In this case, the thickness of polarizer can be more than 10 μm, preferably 5~50 μm.
Thermoplastic resin base material can directly be used as the transparent protective film of polarization plates described later.Furthermore it is possible to inclined
Shake piece with transparent protective film of being fitted on the face of the opposition side of thermoplastic resin base material.On the other hand, thermoplastic resin is not used
In the case of base material, can be in the both sides of polarizer laminating transparent protective film.In addition, thermoplastic resin base material is shelled from polarizer
From rear, can be fitted transparent protective film in the both sides of the polarizer.
As the material for constituting transparent protective film, for example, can be hindered using the transparency, mechanical strength, heat endurance, moisture
The excellent thermoplastic resins such as gear property, isotropism.As the concrete example of such thermoplastic resin, tri acetyl cellulose etc.
Celluosic resin, polyester resin, polyethersulfone resin, polysulfone resin, polycarbonate resin, polyamide, polyimide resin,
Vistanex, (methyl) acrylic resin, cyclic polyolefin resin (norbornene resin), polyarylate resin, polyphenyl
Vinyl, polyvinyl alcohol resin and their mixture.
<Dyeing liquor containing crosslinking agent>
The PVA systems resin used in above-mentioned dyeing process is preferably and is unstained.Additionally, applying polarization of the invention
In the manufacture method of piece, the dyeing liquor used in above-mentioned dyeing process contains crosslinking agent.As crosslinking agent, for example can be from boron
The boron compounds such as acid, borax, glyoxal, glutaraldehyde etc. are middle to be used at least one or shares two or more use.Wherein, preferably make
With boron compound, boric acid is further preferably used.
In above-mentioned dyeing process, micro boric acid (crosslinking agent) is contained by making dyeing liquor, the boric acid makes from PVA systems tree
Lipid layer is dissolved in PVA crosslinkings (complexing materialization) in dyeing liquor.Thus, the PVA and dyeing liquor being dissolved in dyeing liquor are generated
In iodine and boric acid bonding gelatinous iodine/PVA/ boric acid complex (hereinafter referred to as complex compounds).
In order that PVA crosslinkings (complexing materialization) in being dissolved in dyeing liquor, the concentration of the boric acid (crosslinking agent) in dyeing liquor
0.01~0.1 weight portion, more preferably 0.02~0.1 weight portion are preferably set to relative to the weight portion of solvent 100.Boric acid it is dense
Spend during for more than 0.01 weight portion, the PVA being dissolved in dyeing liquor can be made to be crosslinked (complexing materialization).On the other hand, boric acid
When concentration is more than 0.2 weight portion, boric acid is in the surface of layered product (reel film), the table of the roller for transporting layered product (reel film) sometimes
Face etc. separates out, and causes defect of polarizer etc..
Can be to the boric acid that ormal weight is added in dyeing liquor as the method for the concentration of the boric acid in regulation dyeing liquor
Method.In addition, in the case of there is the treatment bath containing boric acid before dyeing treatment, it is possible to use from the treatment bath and layered product
The boric acid brought into together.
In the manufacture method for applying polarizer of the invention, above-mentioned dyeing liquor contains micro boric acid (crosslinking agent),
The boric acid makes the PVA that is dissolved in dyeing liquor be crosslinked (complexing materialization), thus, it is possible to avoid the attachment of PVA as conventional,
The problems such as dyeing kinetics are reduced.That is, the PVA being dissolved in dyeing liquor crosslinks (complexing materialization), is thus difficult to be attached to PVA
Resin (reel film).In addition, de- liquid (dehydration) property of dyeing liquor when reel film is taken out from dye bath is improved.Thus,
The uneven polarizer of dye-free can be obtained.
<The filtering of dyeing liquor>
Additionally, in the manufacture method for applying polarizer of the invention, being filtered to dyeing liquor using filter material.
The complex compounds generated thereby, it is possible to the PVA that is dissolved in dyeing liquor will be made to be crosslinked (complexing materialization) from
Separated in dyeing liquor.For example, the surface treatment that regulation constitutes the film forming condition of the flat film of film or carries out for being separated into film,
So as to the organic matters such as PVA are separated with the heterogeneity of dyeing liquor.As filter material, for example can using polypropylene filter material,
Polyester filter material, nylon filter etc..Module is not particularly limited, it is however preferred to have filter material is accommodated in sealable container and can
Handling ground sets the filter cartridge type of structure in a device.
More specifically, by the inside aperture of the flat film inside adjusting film (for example, be adjusted to not make molecular weight 300 with
On material pass through) or formed according to the difference of ionic charge repulsive force come determine material whether the function that can be passed through on film
Property coated film or Surface Treated Films, thus, it is possible to the organic matters such as PVA are separated with other compositions in dyeing liquor.
As filter membrane, for example, can use ultrafiltration (UF) film, fine filtering (MF) film, nanofiltration (NF) film, reverse osmosis
(RO) film etc. thoroughly, wherein preferably using UF films, MF films.In addition, in filter membrane, preferably using can set and can have PVA etc.
Multiple mistakes for separating benchmark (for example, molecular weight and ionic charge repulsive force) that machine thing is isolated from the different composition of dyeing liquor
Filter membrane.
In addition, the dyeing liquor in dye bath is circulated preferably via filter material.(caught thereby, it is possible to efficiently be removed using filter material
Collection) complex compounds in dye bath.In addition, dyeing liquor can be recycled.
In addition, the dyeing liquor in dye bath is preferably stirred.Thereby, it is possible to the PVA's that promotes to be dissolved in dyeing liquor
Crosslinking (complexing materialization), efficiently can remove complex compounds from dyeing liquor.
Method as dyeing liquor is stirred, it is possible to use the agitating units such as stirring vane are set in dye bath in dyeing
The method for stirring dyeing liquor in bath.In addition, by the circulation of above-mentioned dyeing liquor, it is also possible to stir the dyeing liquor in dye bath
Mix.Additionally, by transporting the reel film of (discrepancy) in dye bath the dyeing liquor in dye bath can also stirred.
As described above, in the manufacture method for applying polarizer of the invention, can remove and be dissolved in dyeing liquor
PVA.Thereby, it is possible to brought in the PVA in avoiding being dissolved in dyeing liquor influence while can also extend dyeing liquor more
Period newly (is changed), therefore, it is possible to further improve the productivity ratio of polarizer.
Embodiment
Below, make effect of the invention clearer by embodiment.It should be noted that the present invention is not limited to down
Embodiment is stated, implementation can be suitably changed in the scope for not changing its purport.
(embodiment 1)
In embodiment 1, using the manufacture method for applying polarizer of the invention, produce in thermoplastic resin base material
On be formed with the polarizability stacked film of polarizer.
Specifically, first, as thermoplastic resin base material, amorphous polyethylene terephthalate (A-PET) is prepared
Film (Mitsubishi chemical Co., Ltd's system, trade name " ノ バ Network リ ァ mono- (registration mark) ", thickness：200μm).
Then, the one side to the thermoplastic resin base material implements sided corona treatment (treatment conditions：90W minutes/m2), at this
Implement and be coated with the degree of polymerization 4000,99.0 moles of aqueous solution of the PVA of more than % of saponification degree at 65 DEG C on the face of sided corona treatment, so
After dry it.Thus, as reel film, the one side obtained in thermoplastic resin base material is formed with the PVA systems of 8.3 μm of thickness
The layered product of resin bed.
Then, resulting reel film is carried out into uniaxial tension (stretch processing) in 90 DEG C of baking oven with 1.8 times.
Then, the insoluble bath by the reel film after stretching in 30 DEG C of liquid temperature (is dissolved with boric acid relative to the weight portion of water 100
The boric acid aqueous solution of 3 weight portions) middle dipping 30 seconds (insoluble treatment).
Then, in the way of the transmissivity of polarizer is for about 42.0%, while regulation iodine concentration, dip time, while will
Reel film immersion (dyeing treatment) in dye bath.
In embodiment 1, prepared to have dissolved the weight portion of iodine 0.18, the weight of KI 1.26 relative to the weight portion of water 100
Part, the dyeing liquor of the weight portion of boric acid 0.02.Then, the liquid temperature of the dyeing liquor is set as 30 DEG C, by reel film immersion 13 seconds.
In addition, PVA0.05 weight portions are added in the dyeing liquor, using magnetic stirrer 15 minutes, while making profit
Liquor circulation after being filtered with polypropylene filter material.
Then, by reel film 40 DEG C of liquid temperature crosslinking bath (relative to the weight portion of water 100 be dissolved with the weight portion of KI 3,
The boric acid aqueous solution of the weight portion of boric acid 3) 30 seconds (crosslinking Treatment) of middle dipping.
Then, while the boric acid aqueous solution by reel film immersion in 70 DEG C of liquid temperature (has dissolved boron relative to the weight portion of water 100
Sour 4 weight portions, the aqueous solution of the weight portion of KI 5) while carrying out uniaxial tension in longitudinal direction (length direction) (in liquid longitudinally
Stretching).Now, the maximum tension multiplying power of layered product is 5.94 times.
Then, the washing bath by reel film in 30 DEG C of liquid temperature (has dissolved the weight portion of KI 4 relative to the weight portion of water 100
The aqueous solution) in dipping 5 seconds, be then dried (carrying out washing treatment and dried process) using 60 DEG C of warm wind.
By by above-mentioned operation, having made the inclined of the polarizer that 4.5 μm of thickness is formed with thermoplastic resin base material
Shaking property stacked film.
(embodiment 2)
In example 2, make boric acid for 0.05 weight portion, dyeing liquor similarly to Example 1 is prepared in addition.So
Afterwards, using the dyeing liquor, polarizer has been made by method similarly to Example 1.
(embodiment 3)
In embodiment 3, make boric acid for 0.1 weight portion, dyeing liquor similarly to Example 1 is prepared in addition.So
Afterwards, using the dyeing liquor, polarizer has been made by method similarly to Example 1.
(embodiment 4)
In example 4, make boric acid for 0.2 weight portion, dyeing liquor similarly to Example 1 is prepared in addition.So
Afterwards, using the dyeing liquor, polarizer has been made by method similarly to Example 1.
(embodiment 5)
In embodiment 5, make boric acid for 0.01 weight portion, dyeing liquor similarly to Example 1 is prepared in addition.So
Afterwards, using the dyeing liquor, carry out to dyeing processing by method similarly to Example 1.
(comparative example 1)
In comparative example 1, boric acid is not contained, dyeing liquor similarly to Example 1 is prepared in addition.
Then, using the dyeing liquor, polarizer has been made by method similarly to Example 1.
Then, each polarizer for being made for these embodiments 1~5 and comparative example 1, by visual observation observation whether there is generation
" dyeing is uneven ".In addition, the level of residue of the complex compounds to being trapped using filter material is measured, " the filtering to dyeing liquor
Property " evaluated.Wherein, " ◎ " is set to, it is set to very good good "○", poor is set to "×".Further,
Observe by visual observation and be attached to the presence or absence of " being polluted caused by boric acid " of device etc. in dyeing treatment.They are collected and is shown in down
In stating table 1.
[table 1]
As shown in table 1, it is known that：Compared with the embodiment 1~5 containing boric acid in dyeing liquor, boron is not contained in dyeing liquor
In the comparative example 1 of acid, filterability is poor, generates dyeing uneven.
On the other hand, compared with embodiment 1~3,5, in example 4, the amount excess of the boric acid contained in dyeing liquor is seen
Pollution caused by the precipitation of boric acid is observed.
On the other hand, in embodiment 1~3,5, filterability is good, uneven without dyeing, boric acid is also not observed and leads
The pollution of cause.
Claims (10)
1. a kind of manufacture method of polarizer, it includes dyeing process, in the dyeing process, by polyvinyl alcohol resin film immersion
In the dyeing liquor comprising dichroism pigment, thus the polyvinyl alcohol resin film is dyeed,
The dyeing liquor contains crosslinking agent,
The dyeing liquor is filtered using filter material.
2. the manufacture method of polarizer as claimed in claim 1, wherein, the dyeing liquor is circulated via the filter material.
3. the manufacture method of polarizer as claimed in claim 1 or 2, wherein, the dyeing liquor is stirred.
4. the manufacture method of the polarizer as any one of claims 1 to 3, wherein, the crosslinking agent is boron compound.
5. the manufacture method of polarizer as claimed in claim 4, wherein, the boron compound is boric acid.
6. the manufacture method of the polarizer as any one of Claims 1 to 5, described its thickness of polyvinyl alcohol resin film
It is less than 10 μm, is formed on thermoplastic resin base material.
7. the manufacture method of the polarizer as any one of claim 1~6, wherein, the concentration of the crosslinking agent is
0.01~0.1 weight portion.
8. the manufacture method of the polarizer as any one of claim 1~7, wherein, the dichroism pigment is iodine.
9. the manufacture method of the polarizer as any one of claim 1~8, wherein, the concentration of the dichroism pigment
It is 0.01~10 weight portion.
10. the manufacture method of the polarizer as any one of claim 1~9, wherein, the dyeing liquor contains iodate
Potassium.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2015-231961 | 2015-11-27 | ||
| JP2015231961 | 2015-11-27 | ||
| JP2016138720A JP6105795B1 (en) | 2015-11-27 | 2016-07-13 | Manufacturing method of polarizer |
| JP2016-138720 | 2016-07-13 |
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| JP (2) | JP6105795B1 (en) |
| KR (1) | KR101811959B1 (en) |
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| TW (1) | TWI606253B (en) |
Cited By (3)
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|---|---|---|---|---|
| CN107619566A (en) * | 2017-10-18 | 2018-01-23 | 中国石油化工集团公司 | A kind of preparation method of polyvinyl alcohol polaroid |
| CN107632335A (en) * | 2017-09-13 | 2018-01-26 | 住华科技股份有限公司 | Method and system for manufacturing polarizing film |
| CN111045139A (en) * | 2019-12-26 | 2020-04-21 | 东华大学 | Preparation method of raincoat brim polaroid |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6713372B2 (en) * | 2016-08-02 | 2020-06-24 | 日東電工株式会社 | Film processing method and polarizing film manufacturing method |
| JP7014559B2 (en) * | 2017-10-02 | 2022-02-01 | 住友化学株式会社 | Method for manufacturing polarizing film |
| JP7260266B2 (en) * | 2017-10-02 | 2023-04-18 | 住友化学株式会社 | Polarizing film manufacturing equipment |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP2017107162A (en) | 2017-06-15 |
| TW201727266A (en) | 2017-08-01 |
| JP6105795B1 (en) | 2017-03-29 |
| TWI606253B (en) | 2017-11-21 |
| KR101811959B1 (en) | 2017-12-22 |
| CN106842403B (en) | 2018-04-24 |
| KR20170062400A (en) | 2017-06-07 |
| JP2017107238A (en) | 2017-06-15 |
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