CN106950634A - The manufacture method of polarizer and the detection method of polyvinyl alcohol - Google Patents
The manufacture method of polarizer and the detection method of polyvinyl alcohol Download PDFInfo
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- CN106950634A CN106950634A CN201611051164.2A CN201611051164A CN106950634A CN 106950634 A CN106950634 A CN 106950634A CN 201611051164 A CN201611051164 A CN 201611051164A CN 106950634 A CN106950634 A CN 106950634A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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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
- C08L31/00—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 acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers
- C08L31/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C08L31/04—Homopolymers or copolymers of vinyl acetate
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- G—PHYSICS
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- 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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- 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
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Abstract
The present invention provides a kind of manufacture method of polarizer, and it can be such that renewal (replacing) period of dyeing liquor optimizes so as to stably manufacture polarizer by carrying out quantitative analysis to the PVA being dissolved in dyeing liquor.The manufacture method includes:Dyeing process, wherein, polyvinyl alcohol (PVA) resin film is immersed in the dyeing liquor containing dichroism pigment (iodine), thus PVA resin films dyed;And analysis procedure, wherein, a part for dyeing bath is extracted out as sample, the absorbance of the sample is determined, and quantitative analysis thus is carried out to the PVA being dissolved in dyeing liquor, dyeing liquor contains crosslinking agent (boric acid).
Description
Technical field
The present invention relates to the manufacture method of polarizer and the detection method of polyvinyl alcohol.
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 polarization has been used as
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 swelling treatment to non-stretched polyvinyl alcohol (PVA) resin film (reel film), 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 for less than 10 μm polarizer by thermoplastic resin base material be coated with PVA system's resin solutions and make its dry 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 PVA part from PVA systems tree
Adipose membrane is dissolved in dyeing liquor.Particularly filming is to dissolubility of the thickness for 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 dissolved is accumulated in dye bath, dyeing liquor
In PVA concentration rise 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 out of dye bath, the de- liquid (dehydration) of dyeing liquor is deteriorated.The result is that producing the yield drop for causing polarizer
Low such the problem of.In addition, in addition to the above problems, due to the PVA concentration rise in dyeing liquor, can also produce iodine in PVA
The problem of adsorption rate (dyeing kinetics) on resin film is reduced, infringement productivity ratio is such.
As its countermeasure, disclose contacted by the foreign matter comprising PVA for making to produce in crosslinking bath with activated carbon so that
Adsorb the method (referring to above-mentioned patent document 1) removed.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, is typically updated periodically (replacing) treatment fluid before above mentioned problem is produced.But, in existing dyeing process, and
The method that quantitative analysis is not carried out to the PVA being dissolved in dyeing liquor, it is difficult to hold the renewal (replacing) of dyeing liquor exactly
Period.Therefore, can actually occur the problems such as above-mentioned PVA attachment, reduction of dyeing kinetics, therefore implementation is handled in most cases
The renewal of liquid.
The present invention be in view of above-mentioned present situation and propose, its object is to provide the manufacture method and polyvinyl alcohol of polarizer
Detection method, the manufacture method of the polarizer can make by carrying out quantitative analysis to the PVA being dissolved in dyeing liquor
Renewal (replacing) period of dyeing liquor optimizes stably to manufacture polarizer, and the detection method of the polyvinyl alcohol can be right
The PVA being dissolved in dyeing liquor is detected.
The means used to solve the problem
As the means for solving the above problems, according to the mode of the present invention there is provided a kind of manufacture method of polarizer,
It includes:Dyeing process, wherein, polyvinyl alcohol (PVA) resin film is immersed in the dyeing liquor comprising dichroism pigment, by
This is dyed to above-mentioned PVA resin films;And analysis procedure, wherein, a part for above-mentioned dyeing liquor is extracted out as sample, is surveyed
The absorbance of the fixed sample, thus carries out quantitative analysis, above-mentioned dyeing liquor is containing crosslinking to the PVA being dissolved in above-mentioned dyeing liquor
Agent.
In addition, the manufacture method of the polarizer of aforesaid way can be following manufacture method:In above-mentioned analysis procedure, from
Regularly extract above-mentioned sample in above-mentioned dyeing liquor out, the absorbance of each sample is determined, while the absorbance of each sample in measure
In the rheological parameters' change with time based on the absorbance under specific wavelength quantitative analysis is carried out to the PVA that is dissolved in above-mentioned dyeing liquor.
In addition, the manufacture method of the polarizer of aforesaid way can be following manufacture method:As above-mentioned specific wavelength, from
At least one wavelength is selected in 500~700nm of wavelength.
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
Spend for 0.01~0.1 parts by weight.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way:Above-mentioned dichroism pigment
For 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 parts by weight.
In addition, can be following manufacture method in the manufacture method of the polarizer of aforesaid way:Above-mentioned dyeing liquor contains
KI.
In addition, according to the mode of the present invention, there is provided a kind of detection method of polyvinyl alcohol, the detection method of the polyvinyl alcohol
It is thus to be detected to above-mentioned PVA by the way that polyvinyl alcohol (PVA) resin film is immersed in the dyeing liquor comprising dichroism pigment
The PVA being dissolved in above-mentioned dyeing liquor when resin film is dyed, wherein, the detection method includes:To above-mentioned PVA systems tree
Adipose membrane determines the absorbance of above-mentioned dyeing liquor before being dyed the step of, make in above-mentioned dyeing liquor containing crosslinking agent thus make from
The step of PVA that above-mentioned PVA resin films are dissolved in above-mentioned dyeing liquor is crosslinked, above-mentioned PVA resin films are dyed after
After the step of determining the absorbance of above-mentioned dyeing liquor and absorbance based on the dyeing liquor determined before above-mentioned dyeing and above-mentioned dyeing
The step of change between the absorbance of the dyeing liquor of measure carries out quantification to the PVA being dissolved in above-mentioned dyeing liquor.
Invention effect
As described above, according to the mode of the present invention, there is provided the manufacture method of polarizer and the detection method of polyvinyl alcohol, institute
The renewal of dyeing liquor can be made by carrying out quantitative analysis to the PVA being dissolved in dyeing liquor by stating the manufacture method of polarizer
(replacing) period optimizes stably to manufacture polarizer, and the detection method of the polyvinyl alcohol can be to being dissolved in dyeing liquor
In PVA detected.
Brief description of the drawings
Fig. 1 is the extinction for determining dyeing liquor when having dissolved PVA to the dyeing liquor containing certain boric acid in the 2nd embodiment
The curve map of the change of degree.
Embodiment
Below, refer to the attached drawing is described in detail to embodiments of the present invention.
In the present embodiment, as the manufacture method for the polarizer for applying the present invention, enumerate exemplified 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 processing using the layered product as reel film, thus manufactures the polarizer below 10 μm of thickness.
< thermoplastic resin base materials >
First, the thermoplastic resin base material used in the manufacture method to applying the polarizer of the present invention is illustrated.
As thermoplastic resin base material, the thermoplastic resin base material for being used as the transparent protective film of polarizer with rice in the past can be used.
As the material for constituting thermoplastic resin base material, for example, it can use the transparency, mechanical strength, heat endurance, water
Divide the excellent thermoplastic resins such as block, isotropism, draftability., can be with as the concrete example of such thermoplastic resin
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
To implement surface treatment (such as sided corona treatment), the thin layers such as priming coat (prime coat) can also be formed.
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 an only few part has amorphous or noncrystalline state the thermoplastic of 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
To the resin referred to as amorphous (ァ モ Le Off ァ ス) or amorphous (non-Jing Quality of crystalline state) resin.Here, amorphous or amorphous
The amorphous resin difference of property of the resin with not forming crystalline state is used.
As crystalline resin, for example, it 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
One of levy is general to have by heating, stretching orientation so that macromolecule arrangement and the property that is crystallized.The physical property of resin
Various change occurs according to the degree of crystallization.
On the other hand, for example for crystalline resin as polypropylene (PP), polyethylene terephthalate (PET)
For, it can also hinder, by high molecular arrangement caused by heating, stretching orientation, crystallization can be suppressed.It will suppress
Such polypropylene (PP) of crystallization, polyethylene terephthalate (PET) are referred to as amorphism polypropylene, amorphism and gathered
Ethylene glycol terephthalate, they is referred to as respectively amorphism olefin-based resin, amorphism ester system resin.
For example in the case of polypropylene (PP), by atactic (the ァ タ Network チ Star Network grooves for forming no 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 make and inhibit crystallization
Amorphism polyethylene terephthalate (PET).
The thickness of thermoplastic resin base material (before stretching) can determine suitably, 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 for 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 of polarizer of the present invention is applied, formed and included on above-mentioned thermoplastic resin base material
The layered product of PVA resins (film).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 it has been used as since preferably using in the past.As PVA systems resin,
PVA or derivatives thereof can be enumerated.As PVA derivative, polyvinyl formal, polyvinyl acetal can be enumerated
Deng.In addition, it 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 PVA degree of polymerization is preferably 100~10000, and more preferably 1000~10000.On saponification degree, typically using soap
Change degree is 80~100 moles of % PVA.
The additives such as plasticizer, surfactant can also be contained in PVA systems resin.As plasticizer, it can enumerate
Polyalcohol and its condensation product etc..Specifically, it can such as 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 parts by weight PVA systems resin for 20 parts by weight with
Under.
< layered products (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 forming PVA resins to obtain.In addition, layered product can be thermoplastic resin base material and PVA systems tree
The structure that lipid layer is laminated across priming coat.In addition, layered product can also be that thermoplastic resin base material and PVA resins are straight
Connect the structure being laminated or be substrate layer and hydrophilic macromolecule layer integration state layered product.
The aqueous solution such as can by by the powder or crushed material of PVA systems resin, cut-out thing be dissolved in after appropriate heating
Water (hot water) in prepare.The concentration of the aqueous solution is preferably set to 2~20 parts by weight relative to the parts by weight of water 100, more preferably
For 4~10 parts by weight.
Painting solution can be selected suitably using such as wire rod 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
It is coated with (ト of カ Application マ Us one) method, lip rubbing 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 formed for less than 10 μm of thickness.The thickness of non-stretched PVA resins is preferably set to 3~20 μ
M, more preferably 5~15 μm.
< treatment process >
Apply the present invention polarizer manufacture method in, to layered product (reel film) at least implements dyeing processing with
Stretch processing.In addition, in the manufacture method of polarizer of the present invention is applied, it is possible to implement crosslinking Treatment.Dyeing handle,
Bath is respectively handled in crosslinking Treatment and stretch processing using dye bath, crosslinking bath and stretch bath respectively.In the situation using processing bath
Under, the treatment fluid (aqueous solution etc.) corresponding with each processing can be used.
< dyeing process >
In dyeing process, by make PVA resins that iodine or dichroic dye be adsorbed in layered product and be orientated come
Carry out dyeing processing.In dyeing process, dyeing processing can be carried out together with stretch processing.
Dyeing processing is carried out by the way that layered product is immersed in the dyeing liquor in dye bath into (dye bath).It is used 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 can 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..It is used as iodide, preferably KI.In addition, in the present embodiment
The iodide used for being used in other processes in the case of it is also same with above-mentioned iodide.
Iodine concentration in iodine solution is preferably set to 0.01~10 parts by weight relative to the parts by weight of solvent 100, more preferably
0.02~5 parts by weight, more preferably 0.1~1.0 parts by weight.Iodide concentration is preferably set relative to the parts by weight of solvent 100
It is set to 0.1~10 parts by weight, more preferably 0.2~8 parts by weight.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 in the way of it can reach the degree of polarization specified or transmissivity within the optional time
Stain.
< stretching process >
In stretching process, dry type stretching processing and wet tensile processing 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 of the cross directional stretch that stretching and width relative to layered product are carried out.
, can also be while carrying out stretching in width while being shunk in length direction in cross directional stretch.It is used as transverse direction
Stretching mode, can be enumerated for example:The fixing end monoaxial stretching method of one end is fixed via stenter, do not fix the freedom of one end
Hold monoaxial stretching method etc..
On the other hand, in longitudinal stretching, it can 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.In addition, stretch processing can be drawn by using twin shaft
Stretch, oblique extension etc. is carried out.
Dry type stretching processing 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 processing, preferably in dyeing process
Preceding implementation dry type stretching processing.
In the treatment fluid used in wet tensile processing, iodide can be contained.Contain iodide in treatment fluid
In the case of, iodide concentration is preferably set to 0.1~10 parts by weight, more preferably 0.2~5 weight relative to the parts by weight of solvent 100
Measure 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 at dyeing processing, crosslinking
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 with 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
Process etc. in stretching in the case of include the accumulation stretching ratio of stretching in other processes.Total stretching ratio is being examined
Suitably determined in the case of considering the stretching ratio in other processes etc..
When always stretching ratio is low, orientation is not enough, it is difficult to obtain the polarizer of high optical characteristics (degree of polarization).On the other hand,
When always stretching ratio is too high, easily occurs tension failure.In addition, polarizer becomes too thin, the processability in subsequent handling has can
Can reduction.
In stretching process, such as " No. 4751481 publications of Japanese Patent No. " it is described, auxiliary that can be in atmosphere
Implement wet tensile processing after stretch processing.The draft temperature in assisting tension processing in atmosphere is preferably preset
For 60~180 DEG C, be further 95~150 DEG C of so high temperature.In addition, in atmosphere assisting tension processing 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 handles it
Treatment temperature in the wet tensile processing 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 processing
Rate is set as 4~7 times, more preferably 5~6 times.
In stretching process, including in atmosphere assisting tension processing and wet tensile processing in the case of, preferably
Implement the assisting tension processing in atmosphere before dyeing processing, implement wet tensile processing after dyeing processing.It is this
In the case of, the processing bath for wet tensile processing is also used as crosslinking bath, preferably implements together with wet tensile processing at crosslinking
Reason.
< cross-linking process steps >
In cross-linking process step, crosslinking Treatment is carried out using boron compound as crosslinking agent.Crosslinking Treatment can with dyeing
Reason, stretch processing are carried out together.In addition, crosslinking Treatment can be divided into multiple progress.As boron compound, such as boron can be used
Acid, borax etc..Boron compound is typically used with the form of the aqueous solution or water-organic solvent mixed solution.
In the case of using boric acid aqueous solution, heat resistance, therefore, the boric acid concentration of boric acid aqueous solution are assigned by the degree of cross linking
1~10 parts by weight, more preferably 2~7 parts by weight are preferably set to relative to the parts by weight 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 solvent
100 parts by weight are preferably set to 0.1~10 parts by weight, more preferably 0.5~8 parts by weight.
Crosslinking Treatment can be carried out by the way that layered product is immersed in boric acid aqueous solution etc..Processing 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.Treatment time is preferably set to 5~
800 seconds, more preferably 8~500 seconds.
The insoluble process > of <
Apply the present invention polarizer manufacture method in, to layered product implement dyeing processing or crosslinking Treatment it
Before can implement insoluble processing.The purpose of insoluble process is to implement to be used to make PVA resins undissolved insoluble
Processing.
, can be by making the PVA resins in layered product be immersed in such as boric acid or containing boron in insoluble process
Insoluble processing is carried out in the solution of the boron compounds such as sand.The general shape with the aqueous solution or water-organic solvent mixed solution of solution
State is used.
In the case of using boric acid aqueous solution, the boric acid concentration of boric acid aqueous solution is preferably set relative to the parts by weight of solvent 100
It is set to 1~4 parts by weight.Treatment temperature in insoluble process is preferably set to more than 25 DEG C, more preferably 30~85 DEG C, enters one
Walk as 30~60 DEG C.Treatment time is preferably set to 5~800 seconds, more preferably 8~500 seconds.
< washing procedures >
In the manufacture method of polarizer of the present invention is applied, dyeing processing, stretch processing can be implemented to layered product
And further implement crosslinking Treatment, but carrying out washing treatment can be implemented after these processing are implemented.
In washing procedure, liquor kalii iodide can be used to carry out carrying out washing treatment.Iodate potassium concn in liquor kalii iodide
0.5~10 parts by weight, more preferably 0.5~8 parts by weight, more preferably 1 are preferably set to relative to the parts by weight of solvent 100
~6 parts by weight.
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.Utilize the rank of the carrying out washing treatment of liquor kalii iodide
As long as just it is not particularly limited before section drying process.
In addition, being used as carrying out washing treatment, it is possible to implement water washing.Water washing is by the way that PVA systems resin is immersed in
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, it can will be combined, for example, also may be used using the carrying out washing treatment and water washing of liquor kalii iodide
To use the solution for being suitably combined with the liquid alcohols such as methanol, ethanol, isopropanol, butanol, propyl alcohol.
< drying processes >
In addition, in the manufacture method of polarizer of the present invention is applied, implement after above-mentioned each processing, it is final to implement dry
Dry processing, so as to manufacture polarizer.In drying 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, obtained polarizer deterioration is deteriorated in terms of optical characteristics and tone.Heat drying time is preferably set to 1~
10 minutes.
< water soluble antioxidants >
In the manufacture method of polarizer of the present invention is applied, at least one work that can be after above-mentioned dyeing process
The processing using the treatment fluid containing at least one water soluble antioxidant is carried out in sequence.
In processing using the treatment fluid containing water soluble antioxidant, that layered product is implemented after dyeing processing is each
Contain water soluble antioxidant in any at least one in each bath used in processing.Or, individually implement to utilize in addition
The processing for the treatment of fluid containing water soluble antioxidant.Using the treatment fluid containing water soluble antioxidant processing preferably with friendship
Connection processing 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 processing simultaneously
OK.Carry out at the same time in being uniformly processed of multiple processing, contain water soluble antioxidant in the bath used during this is uniformly processed.
In addition, in the multistage processing of crosslinking Treatment and stretch processing is individually carried out in addition, in any of crosslinking Treatment and stretch processing
Contain water soluble antioxidant at least one processing.
As water soluble antioxidant, it 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.
Dichroic substance (iodine of the addition of water soluble antioxidant according to contained by each treatment fluid after dyeing process
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 then added is also more.
Throughout reason liquid in, preferably according to water soluble antioxidant concentration relative to the parts by weight of solvent 100 be 0.005~
The mode of 1 parts by weight adds water soluble antioxidant, more preferably 0.005~0.5 parts by weight.The concentration of water soluble antioxidant
In the case of less than 0.005 parts by weight, 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 polarizer obtained by system.On the other hand, the concentration of water soluble antioxidant
In the case of more than 1 parts by weight, the ratio increase of the water soluble antioxidant in bath, therefore, resulting polarizer decolourizes, thoroughly
Penetrate rate rise.Accompany with this, it is possible to need to improve the iodine concentration of dye bath, but asked in terms of optical characteristics in the absence of reduction etc.
Topic.
< polarizers >
The polarizer manufactured by the manufacture method for the polarizer for applying the present invention is formed on thermoplastic resin base material,
But non-stretched PVA resins film can also be implemented above-mentioned each as reel film without using above-mentioned thermoplastic resin base material
Handle 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 side opposite with thermoplastic resin base material face on fit transparent protective film.On the other hand, without using thermoplastic resin
In the case of base material, can fit transparent protective film in the both sides of polarizer.In addition, thermoplastic resin base material is shelled from polarizer
From rear, can fit transparent protective film in the both sides of the polarizer.
As the material for constituting transparent protective film, for example, it can use the transparency, mechanical strength, heat endurance, moisture resistance
The excellent thermoplastic resins such as gear property, isotropism.It is used 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.
< analysis procedures >
The PVA systems resin used in above-mentioned dyeing process is preferably to be unstained.In addition, applying the polarization of the present invention
In the manufacture method of piece, the dyeing liquor used in above-mentioned dyeing process contains crosslinking agent., for example can be from boron as crosslinking agent
Using at least one or share two or more use in the boron compounds such as acid, borax, glyoxal, glutaraldehyde etc..Wherein, preferably make
With boron compound, further preferably using boric acid.
In above-mentioned dyeing process, contain micro boric acid (crosslinking agent) by making dyeing liquor, the boric acid makes from PVA systems tree
Lipid layer is dissolved in the 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 the concentration of the boric acid (crosslinking agent) in the PVA crosslinkings (complexing materialization) being dissolved in dyeing liquor, dyeing liquor
0.01~0.1 parts by weight, more preferably 0.02~0.1 parts by weight are preferably set to relative to the parts by weight of solvent 100.Boric acid it is dense
When spending to be more than 0.01 parts by weight, 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 parts by weight, boric acid is in the surface of layered product (reel film), the table for the roller for transporting layered product (reel film) sometimes
Face etc. is separated out, and causes defect of polarizer etc..
Can be the boric acid of addition ormal weight into 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 processing bath containing boric acid before dyeing processing, can use from the processing bath and layered product
The boric acid brought into together.In this case, concentration that can be in advance to boric acid is monitored.
The complex compounds generated in dyeing liquor are so that the absorbance change of dyeing liquor.Therefore, the present invention is being applied
Polarizer manufacture method in, as analysis procedure, extract a part for dyeing liquor out as sample, determine the extinction of the sample
Degree.Specifically, preferably:Regularly extract sample out from dyeing liquor, determine the absorbance of each sample, meanwhile, in each of measure
Rheological parameters' change with time based on the absorbance under specific wavelength in the absorbance of sample is quantitatively divided the PVA being dissolved in dyeing liquor
Analysis.Absorbance can be for example measured by commercially available spectrophotometer.At this point it is possible to use appropriate solvent dilute sample.
Specific wavelength preferably selects at least one wavelength from 500~700nm of wavelength.That is, the specific wavelength preferably exists
The wavelength of maximum is shown in the absorbance of each sample.In the present embodiment, in the maximum absorption wavelength with iodo-complexes
There is the maximum absorption wavelength of complex compounds near different about 620nm.
As described above, in the present invention, containing micro boric acid (crosslinking agent) by making dyeing liquor, the boric acid makes to be dissolved in
PVA crosslinkings (complexing materialization) in dyeing liquor, the amount thus, it is possible to PVA simply to being dissolved in the dyeing liquor is monitored
(quantification).Thereby, it is possible to avoided in the continuous production of polarizer the PVA attachment as in the past, dyeing kinetics drop
Low problem, and renewal (replacing) period of dyeing liquor can be judged exactly.
That is, in the manufacture method of polarizer of the present invention is applied, it is preferably provided with following process:With complex compounds
Amount as benchmark, preferably using the absorbance of complex compounds as benchmark, to dyeing liquor part or all carry out more
Change.
The detection method > of < polyvinyl alcohol (PVA)
The detection method for applying the polyvinyl alcohol (PVA) of the present invention is preferably used in above-mentioned analysis procedure.That is, the PVA
Detection method include:Determined before being dyed to PVA resins (PVA resin films) as the dyeing liquor referred to
The step of absorbance, make in dyeing liquor containing boric acid (crosslinking agent) thus make from PVA resins be dissolved in dyeing liquor in PVA
The step of crosslinking, PVA resins are dyed after determine dyeing liquor absorbance the step of and based on dyeing before determine
Change between the absorbance of the dyeing liquor determined after the absorbance of dyeing liquor and dyeing is carried out to the PVA being dissolved in dyeing liquor
The step of quantification.
When being continuously manufactured by polarizer, handled after dyeing before processing being carried out in (on the time) using dyeing with not stopping
In dyeing liquor be used as the quantitative subject sample of reference sample or PVA.
In the PVA detection method of the present invention is applied, be not limited to as above-mentioned analysis procedure regularly from
Sample is extracted out in dyeing liquor and determines the situation of the absorbance of each sample, can also the extinction based on the dyeing liquor determined before dyeing
Change (poor) between the absorbance of the dyeing liquor determined after degree and dyeing carries out quantification to the PVA being dissolved in dyeing liquor.
Embodiment
Below, make the effect of the present 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.
[the 1st embodiment]
First, in the 1st embodiment, PVA (0.02 parts by weight, 0.03 parts by weight or 0.05 weight for ormal weight of sening as an envoy to are made
Amount part) be dissolved in dyeing liquor at the same change the amount of the boric acid contained in the dyeing liquor embodiment 1~11 and comparative example 1 it is each
Sample.Then, the absorbance under wavelength 620nm is determined to each sample, and observes having for the caused pollution of boric acid by visual observation
Nothing.They are collected and is shown in table 1 below.
[table 1]
(embodiment 1)
In embodiment 1, as sample, it is prepared for being dissolved with the parts by weight of iodine 0.18, KI relative to the parts by weight of water 100
1.26 parts by weight, PVA0.02 parts by weight, the dyeing liquor of the parts by weight of boric acid 0.01.
Then, the UV visual absorption spectrum of the dyeing liquor is determined, the wavelength from iodine/PVA/ boric acid complex is determined
620nm absorbance.UV visual absorption spectrum is entered using spectrophotometer (Co., Ltd. island Feng makes made UV-2450)
Row is determined.It should be noted that in determining, using glass unit (optical path length:1mm).In addition, prepare after the dyeing liquor,
The presence or absence of boric acid for being separated out in glass unit is observed by visual observation.
(embodiment 2)
In example 2, as sample, it is 0.02 parts by weight to make boric acid, in addition, is prepared similarly to Example 1
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 3)
In embodiment 3, as sample, make PVA be 0.03 parts by weight, make boric acid be 0.02 parts by weight, in addition, system
For the dyeing liquor gone out similarly to Example 1.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 4)
In example 4, as sample, make PVA be 0.05 parts by weight, make boric acid be 0.02 parts by weight, in addition, system
For the dyeing liquor gone out similarly to Example 1.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 5)
In embodiment 5, as sample, it is 0.07 parts by weight to make boric acid, in addition, is prepared similarly to Example 1
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 6)
In embodiment 6, as sample, it is 0.10 parts by weight to make boric acid, in addition, is prepared similarly to Example 1
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 7)
In embodiment 7, as sample, it is 0.2 parts by weight to make boric acid, in addition, is prepared similarly to Example 1
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 8)
In embodiment 8, as sample, it is 0.07 parts by weight to make boric acid, in addition, is prepared similarly to Example 3
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 9)
In embodiment 9, as sample, it is 0.07 parts by weight to make boric acid, in addition, is prepared similarly to Example 4
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 10)
In embodiment 10, as sample, it is 0.10 parts by weight to make boric acid, in addition, is prepared similarly to Example 3
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(embodiment 11)
In embodiment 11, as sample, it is 0.10 parts by weight to make boric acid, in addition, is prepared similarly to Example 4
Dyeing liquor.Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
(comparative example 1)
In comparative example 1, as sample, boric acid is not contained, in addition, dyeing liquor similarly to Example 1 is prepared.
Then, measure similarly to Example 1 and observation are carried out to the dyeing liquor.
As shown in table 1, it is known that:For making in dyeing liquor for the sample of the embodiment 1~11 containing boric acid, in each boric acid
In the sample of content, with PVA amount increase, the absorbance approximately linear under wavelength 620nm increases.On the other hand, it is known that:It is right
For the sample of comparative example 1 that boric acid is not contained in dyeing liquor, no complex compound is formed, therefore, with containing boron in dyeing liquor
The embodiment 1~6 of acid is compared with the sample of comparative example 2, and the absorbance under wavelength 620nm is extremely low.
On the other hand, for the sample of embodiment 7, compared with the sample of embodiment 1~6,8~11, in dyeing liquor
The amount of the boric acid contained is excessive, it was observed that being polluted caused by the precipitation of boric acid.
On the other hand, for the sample of embodiment 1~6,8~11, the absorbance under wavelength 620nm is high, does not also have
It was observed that being polluted caused by the precipitation of boric acid.
(the 2nd embodiment)
Then, in the 2nd embodiment, prepare and be dissolved with the parts by weight of iodine 0.18, KI relative to the parts by weight of water 100
The dyeing liquor of 1.26 parts by weight, the parts by weight of boric acid 0.02.Then, the dyeing liquor is determined by the method same with the 1st embodiment
Absorbance.Then, determined by the method same with the 1st embodiment dissolved in the dyeing liquor 0.013 parts by weight,
Each absorbance when 0.029 parts by weight, the PVA of 0.051 parts by weight, obtains the difference with the absorbance before dissolving PVA.By it
Collect it is shown in Figure 1.
As shown in Figure 1, it is known that:With the amount increase for the PVA being dissolved in dyeing liquor, absorbance increase.Understand:Particularly
The maximum of absorbance is shown under wavelength 620nm.Therefore, the change to the absorbance under wavelength 620nm is measured, energy
Enough PVA to being dissolved in dyeing liquor carry out quantification.That is, according to the present invention, carry out quantitatively holding by the amount to PVA
The replacing period of liquid, therefore, it is possible to stably manufacture the polarizer of no irregular colour.
Claims (11)
1. a kind of manufacture method of polarizer, it includes:
Dyeing process, by polyvinyl alcohol resin film immersion in the dyeing liquor comprising dichroism pigment, thus to the poly- second
Enol resin film is dyed;With
Analysis procedure, extracts a part for the dyeing liquor out as sample, the absorbance of the sample is determined, thus to being dissolved in
The polyvinyl alcohol stated in dyeing liquor carries out quantitative analysis,
The dyeing liquor contains crosslinking agent.
2. the manufacture method of polarizer as claimed in claim 1, wherein, in the analysis procedure, from the dyeing liquor
Regularly extract the sample out, determine the absorbance of each sample, and based on certain wave in the absorbance of each sample of measure
The rheological parameters' change with time of absorbance under long carries out quantitative analysis to the polyvinyl alcohol being dissolved in the dyeing liquor.
3. the manufacture method of polarizer as claimed in claim 2, wherein, at least one ripple is selected from 500~700nm of wavelength
Length is used as the specific wavelength.
4. such as manufacture method of polarizer according to 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. such as the manufacture method of polarizer according to any one of claims 1 to 5, described its thickness of polyvinyl alcohol resin film
For less than 10 μm, it is formed on thermoplastic resin base material.
7. such as manufacture method of polarizer according to any one of claims 1 to 6, wherein, the concentration of the crosslinking agent is
0.01~0.1 parts by weight.
8. such as manufacture method of polarizer according to any one of claims 1 to 7, wherein, the dichroism pigment is iodine.
9. such as manufacture method of polarizer according to any one of claims 1 to 8, wherein, the concentration of the dichroism pigment
For 0.01~10 parts by weight.
10. such as manufacture method of polarizer according to any one of claims 1 to 9, wherein, the dyeing liquor contains iodate
Potassium.
11. a kind of detection method of polyvinyl alcohol, the detection method of the polyvinyl alcohol is by the way that polyvinyl alcohol resin film is soaked
Thus stain detects dissolving when being dyed to the polyvinyl alcohol resin film in the dyeing liquor comprising dichroism pigment
Polyvinyl alcohol in the dyeing liquor, wherein,
The detection method includes:
The step of absorbance of the dyeing liquor being determined before being dyed to the polyvinyl alcohol resin film;
Make containing crosslinking agent thus to make from the polyvinyl alcohol resin film is dissolved to the dyeing liquor in the dyeing liquor
Polyvinyl alcohol crosslinked step;
The step of absorbance of the dyeing liquor being determined after being dyed to the polyvinyl alcohol resin film;With
Between the absorbance of the dyeing liquor determined after absorbance and the dyeing based on the dyeing liquor determined before the dyeing
Change, the step of quantification is carried out to the polyvinyl alcohol being dissolved in the dyeing liquor.
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JP7302951B2 (en) * | 2018-06-28 | 2023-07-04 | 日東電工株式会社 | Polarizer manufacturing method and polarizer manufacturing apparatus |
CN111337442A (en) * | 2020-03-24 | 2020-06-26 | 安徽皖维高新材料股份有限公司 | Method for measuring PVA optical film dissolution amount |
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