CN107703577A - Polarizer and its manufacture method - Google Patents
Polarizer and its manufacture method Download PDFInfo
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- CN107703577A CN107703577A CN201710668721.3A CN201710668721A CN107703577A CN 107703577 A CN107703577 A CN 107703577A CN 201710668721 A CN201710668721 A CN 201710668721A CN 107703577 A CN107703577 A CN 107703577A
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- Prior art keywords
- polarizer
- polyvinyl alcohol
- weight
- liquid
- alcohol resin
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Classifications
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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
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J129/00—Adhesives based on 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; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
- C09J129/02—Homopolymers or copolymers of unsaturated alcohols
- C09J129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- 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
-
- 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
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polarising Elements (AREA)
Abstract
The present invention relates to Polarizer and its manufacture method; in more detail; it is related to Polarizer and its manufacture method; the Polarizer is characterised by; the moisture rate of Polarizer is 2.8~4.8%, and the thickness of the bond layer formed by the adhesive composite of the water soluble salt comprising acetoacetyl modified polyvinyl alcohol resin, glyoxal crosslinking agent and polyvalent metal ion of more than two kinds is 30~200nm.
Description
Technical field
The present invention relates to show excellent water resistance and can prevent Polarizer and its manufacturer of light characteristic reduction
Method.
Background technology
Polarizer can use as one of optical component for forming liquid crystal display device.Polarizer generally has in polarizer
Two sides be laminated the structure of diaphragm, and insert in liquid crystal display device.It is known also to have only in the one side setting guarantor of polarizer
Cuticula, but be not simple diaphragm in another side in most cases, but by the layer with other function such as optical function
Engaged in a manner of as diaphragm.
It is general to use the Polarizer formed as follows：Using make iodine in polyvinyl alcohol the iodine mesentery of gas absorption quantity, make two colors
The dyestuff mesentery of property dyestuff gas absorption quantity in polyvinyl alcohol is as polarizer, at least in the one side of film via using polyvinyl alcohol
Be resin the aqueous solution (polyethenol series bonding agent) formed adhesive linkage the diaphragm of triacetyl cellulose (TAC) etc. is connect
Close, but the Polarizer of such composition has what the end face of diaphragm and polarizer was easily peeled off in damp and hot lower long-time use
Problem.
Thus propose following Polarizer：Polarizer (light polarizing film) is engaged with diaphragm using polyethenol series bonding agent
Afterwards, by the heat drying at a temperature of 80~100 DEG C, so as to improve humidity resistance, but the feelings used in damp and hot lower long-time
Under condition, still it is easily peeled off without the end face for solving the problems, such as diaphragm and polarizer.
It is such in order to solve the problems, such as, Patent Document 1 discloses comprising acetoacetyl modified polyvinyl alcohol resin,
The bonding agent combination of polyvinyl alcohol resin (cross-linking regulator), glyoxal system (crosslinking agent) and zinc chloride (crosslinking catalyst)
Thing.But in the case of above-mentioned composition, there are the following problems：Due to comprising cross-linking regulator, therefore curing rate is slow,
The degree of polarization as caused by damp and hot deterioration is caused to reduce.
Therefore, separated to be also prevented from diaphragm under wet heat condition with the short side of polarizer, present situation is that requirement is opened
Hair excellent water resistance, the adhesive composite that can prevent the light characteristic resulted from from reducing.
Prior art literature
Patent document
Patent document 1：Japanese Patent Publication 1995-134212 publications
The content of the invention
The invention problem to be solved
In order to solve the above problems, it is an object of the invention to provide show excellent water resistance and can prevent that light is special
Property reduce Polarizer and its manufacture method.
Means for solving the problems
To achieve these goals, Polarizer of the invention is characterised by, moisture rate is 2.8~4.8%, by including second
The water soluble salt of acyl acetyl group modified polyvinylalcohol system resin, glyoxal crosslinking agent and polyvalent metal ion of more than two kinds glues
The thickness for connecing the bond layer of agent composition formation is 30~200nm.
In addition, to achieve these goals, according to the manufacture method of the Polarizer of the present invention, it is characterised in that include：
(a) acetoacetyl modified polyvinyl alcohol resin, glyoxal crosslinking agent and of more than two kinds are included in the two sided coatings of polarizer
The adhesive composite of the water soluble salt of polyvalent metal ion, generate the stage of bond layer；(b) will on above-mentioned bond layer
The diaphragm of at least more than one is engaged using nip rolls, makes the stage of Polarizer；Above-mentioned Polarizer pass through at least 2 (c)
It is individual more than drying path and by the dry stage.
The effect of invention
According to the Polarizer of the present invention, by adjusting the moisture rate of Polarizer and the thickness of bond layer, so as to will not
With the effect for improving water resistance while reducing light characteristic.
In addition, the Polarizer manufactured using the manufacture method of the Polarizer according to the present invention also has the effect above.
Brief description of the drawings
Fig. 1 is the figure for showing schematically the evaluation test method according to the water resistance of experimental example.
Embodiment
In the present invention during certain part "comprising" inscape, as long as without especially opposite record, it is not precluded from it
His inscape, it is meant that can further include other inscapes.
The preferred embodiment of the present invention is explained below.
<Polarizer>
Polarizer according to an embodiment of the present invention, by making moisture rate be 2.8~4.8%, make by comprising acetyl
The bonding of the water soluble salt of acetyl group modified polyvinylalcohol system resin, glyoxal crosslinking agent and polyvalent metal ion of more than two kinds
The thickness for the bond layer that agent composition is formed turns into 30~200nm, so as to have following effect：Will not accompany has light characteristic
Reduction, diaphragm is also prevented under wet heat condition and is separated with the short side of polarizer, therefore water resistance can be improved.
The moisture rate of above-mentioned Polarizer means the moisture rate determined using following weight moisture rate determination method：To terminating
Whole drying process and the Polarizer completed is heat-treated 2 hours front/rear weight changes at 105 DEG C and observed.
So-called Polarizer in the present invention, may mean that Polarizer used in the art, as one, can be
The product for forming more than one diaphragm bonding at least one side of polarizer.
Bond layer
For the Polarizer of the present invention, by being 30~200nm, by including acetoacetyl modified poly- second comprising thickness
What the adhesive composite of the water soluble salt of enol system resin, glyoxal crosslinking agent and polyvalent metal ion of more than two kinds was formed
Bond layer, so as to which the short side of diaphragm and polarizer with the reduction of light characteristic, will not be also prevented under wet heat condition
Separation, thus with can make water resistance improve effect, above-mentioned bond layer thickness less than 30nm in the case of, can send out
Raw apparent problem, in the case of more than 200nm, occurs damp and hot deterioration, and the problem of light characteristic reduces can occur.
Above-mentioned adhesive composite includes：Comprising acetoacetyl modified polyvinyl alcohol resin and glyoxal crosslinking agent
The B liquid of A liquid and water soluble salt comprising acetoacetyl modified polyvinyl alcohol resin and polyvalent metal ion of more than two kinds,
Above-mentioned A liquid and B liquid can be mixed and manufactured.
Each contained acetoacetyl modified polyvinyl alcohol resin can be with water (distilled water) for above-mentioned A liquid and B liquid
Mixing and they are mixed in the form of the aqueous solution, just above-mentioned A liquid and B liquid each contained by acetoacetyl modified polyethylene
For the content of the solid constituent of alcohol system resin, relative to the above-mentioned acetoacetyl modified polyvinyl alcohol resin aqueous solution 100
Weight %, containing 2.5~4.5 weight %, so as to have the effect that：Will not be with the reduction of light characteristic, even in damp and hot bar
Diaphragm is also prevented under part to separate with the short side of polarizer, therefore can improve water resistance.Specifically, above-mentioned A liquid and B liquid are each
From the content of the solid constituent of contained acetoacetyl modified polyvinyl alcohol resin less than 2.5% in the case of, can send out
The problem of raw water resistance effect reduces, in the case of 4.5%, can occur the problem of optical characteristics reduces.
Acetoacetyl modified polyvinyl alcohol resin
Contained adhesive composite is by including acetoacetyl modified polyethenol series in the bond layer of the present invention
It resin, can improve the bonding force of diaphragm and polarizer.
Above-mentioned acetoacetyl modified polyvinyl alcohol resin with it is carboxy-modified, methylol-modified, amino modified etc. so
The polyvinyl alcohol resin of modification compare, it is excellent in terms of the raising of durability containing the high functional group of reactivity.
Above-mentioned acetoacetyl modified polyvinyl alcohol resin by using known method make polyvinyl alcohol resin with
Dienone (diketene) reacts and obtained.Specifically, using make polyvinyl alcohol resin in acetic acid equal solvent disperse after to
The method for wherein adding dienone；After polyvinyl alcohol resin is dissolved in advance in dimethylformamide Huo dioxane equal solvents
The method for adding dienone thereto；Or make what polyvinyl alcohol resin directly contacted with dienone gas or liquid diene ketone
Method etc. obtains.
As long as the above-mentioned acetoacetyl modified degree of acetoacetyl modified polyvinyl alcohol resin is 0.1 mole of more than %,
Then there is no particular restriction, preferably 0.1~40 mole of %, more preferably 1~20 mole of %, most preferably 2~7 moles of %.On
In the case of less than the 0.1 mole % of modification degree for stating acetoacetyl, because the water resistance of bond layer is insufficient and unsuitable,
In the case of more than 40 moles % of the modification degree of above-mentioned acetoacetyl, the raising effect of water resistance is extremely low.
To the saponification degree of above-mentioned acetoacetyl modified polyvinyl alcohol resin, there is no particular restriction, preferably 80 moles of %
More than, in addition, more preferably 85 moles of more than %.The saponification degree of above-mentioned acetoacetyl modified polyvinyl alcohol resin is less than upper
In the case of stating scope, it is difficult to show sufficient water solubility, therefore the problem of cementability reduces can be produced.
The degree of polymerization of above-mentioned acetoacetyl modified polyvinyl alcohol resin is preferably in 100~1500.Above-mentioned acetyl second
The degree of polymerization of acyl modified polyvinyl alcohol resin be above range in the case of, have make the polarizer in Polarizer and guarantor
The effect that bonding force between cuticula improves.
Above-mentioned acetoacetyl modified polyvinyl alcohol resin can specifically include Z-100, Z-200, Z-200H, Z-
210th, Z-220 and Z-320 (Japan synthesizes chemical Gohsefimer Co., Ltd.) etc., but it is not limited to this.
Glyoxal crosslinking agent
Contained adhesive composite includes glyoxal crosslinking agent in the bond layer of the present invention.
In the case of containing above-mentioned glyoxal system crosslinking agent, by the aldehyde radical in above-mentioned glyoxal system crosslinking agent not only with it is upper
State acetoacetyl modified polyvinyl alcohol resin and carry out condensation reaction with hydroxyl contained in polarizer, diaphragm, from
And the degree of cross linking of adhesive composite is improved, having makes polarizer using its engagement and the intermembranous bonding force of protection and water-fast
Property improve effect.
For the content of above-mentioned glyoxal system crosslinking agent, relative to the acetoacetyl contained together in above-mentioned A liquid
The parts by weight of solid constituent 100 of modified polyvinylalcohol system resin, glyoxal system crosslinking agent can be contained with 30~70 parts by weight.On
In the case of the content of glyoxal system crosslinking agent is stated less than above range, it can occur by viscous comprising above-mentioned glyoxal system crosslinking agent
Connect agent composition formation bond layer water resistance reduce the problem of, more than above range in the case of, can produce adjust liquid it is steady
The problem of qualitative reduction.
The water soluble salt of polyvalent metal ion
Contained adhesive composite is by including the water of polyvalent metal ion of more than two kinds in the bond layer of the present invention
Soluble, so as to not only promote the effect of above-mentioned glyoxal system crosslinking agent, put forward the degree of cross linking comprising its adhesive composite
Height, and with the effect for making to improve using the polarizer that it the is bonded degree of cross linking intermembranous with protection.Thus there is following effect
Fruit：The bonding force and water resistance of above-mentioned bond layer can be improved, can also prevent the reduction of the optical durability associated with it.
The water soluble salt of above-mentioned polyvalent metal ion specifically can be from zinc chloride, cobalt chloride, magnesium chloride, magnesium acetate, nitric acid
Selected in aluminium, zinc nitrate and zinc sulfate, more preferably from the excellent zinc chloride of the effect of crosslinking catalyst, zinc nitrate and aluminum nitrate
Selection.
In the case that the water soluble salt of above-mentioned polyvalent metal ion includes zinc chloride, for its content, relative to above-mentioned B
The parts by weight of solid constituent 100 of the acetoacetyl modified polyvinyl alcohol resin contained together in liquid, can be with 2~10 weight
Part is contained.Above-mentioned zinc chloride content less than above range in the case of, the bonding agent by including above-mentioned zinc chloride can be produced
The problem of water resistance for the bond layer that composition is formed is insufficient, more than above range in the case of, can produce and adjust liquid stable
Property reduce the problem of.
In the case that the water soluble salt of above-mentioned polyvalent metal ion includes zinc nitrate or aluminum nitrate, relative in above-mentioned B liquid
The parts by weight of solid constituent 100 of contained acetoacetyl modified polyvinyl alcohol resin, its content can be 30~90 weight
Part.In the case that the content of above-mentioned zinc nitrate or aluminum nitrate is less than above range, it can occur by comprising above-mentioned zinc nitrate or nitric acid
The problem of water resistance for the bond layer that the adhesive composite of aluminium is formed is insufficient, more than above range in the case of, can send out
Raw the problem of adjusting liquid stability to reduce.
Viscosity in the bond layer of the present invention at 20 DEG C of contained adhesive composite is preferably 3~25mPasec
In the range of.In the case that the viscosity of adhesive composite is less than 3mPasec, it is impossible to fully show and combined by above-mentioned bonding agent
The water resistance for the bond layer that thing is formed, in the case that viscosity is more than 25mPasec, is present comprising the inclined of above-mentioned bond layer
The problem of optical characteristics of tabula rasa reduces.
Above-mentioned adhesive composite can further include plasticizer, silicon in the range of the effect of the present invention is not hindered
Alkane coupling agent, antistatic additive, particulate, autgmentability is set to become the additives such as good alcohol, levelling agent.
To the form of above-mentioned adhesive composite, there is no particular restriction, in order to as the polarizer and protection for being attached to body
The surface of film forms homogeneous bond layer, preferably liquid type.As the bonding agent of such liquid type, various solvents can be used
Solution-type or dispersion liquid type, if it is considered that in terms of the coating of base material, preferred solution-type, if it is considered that in terms of stability, then
It is preferred that the solution-type of solvent or dispersion liquid type are used as using water.
Polarizer (light polarizing film)
For forming the polyvinyl alcohol resin of polarizer by the way that the resin saponification of polyvinyl acetate system is obtained.As
Polyvinyl acetate system resin, in addition to as the polyvinyl acetate of the homopolymer of vinylacetate, acetic acid can be included
Vinyl acetate and the copolymer of other monomers that can be copolymerized with it etc..As with vinyl acetate copolymerized other monomers, such as can
Include unsaturated carboxylic acid class, unsaturated sulfonic acid class, olefines, vinyl ethers, the acrylic amide etc. with ammonium.Poly- second
The saponification degree of enol system resin is usually 85~100 moles of %, preferably 98 moles of more than %.Can be to the polyvinyl alcohol resin
It is further modified, such as can also use the polyvinyl alcohol polymer being modified with aldehydes, Pioloform, polyvinyl acetal etc..Form polarisation
The average degree of polymerization of the polyvinyl alcohol resin of device is usually 1000~10000, and preferably 1500~5000.
The product (polyvinyl alcohol resin film) that such polyvinyl alcohol resin is film-made on film is used for polarisation
The master film of device.The method that polyvinyl alcohol resin is filmed is not particularly limited, known film-forming method can be used.
Thickness as the polyvinyl alcohol resin film of master is not particularly limited, such as can be 10~150 μm.
Polarizer can generally manufacture with the following method, and this method includes：To such polyethenol series as master
Resin film carries out the process of uniaxial tension, polyvinyl alcohol resin film is dyed with dichroism pigment and makes the dichroism color
The process of element absorption, the process that is handled with boric acid aqueous solution the polyvinyl alcohol resin film for having adsorbed dichroism pigment and
In the process that the laggard water-filling of processing using the boric acid aqueous solution is washed.
Uniaxial tension can be carried out before dyeing, also can simultaneously be carried out with dyeing, can also be carried out after dyeing.After dyeing
In the case of carrying out uniaxial tension, uniaxial tension can be carried out in boric acid before processing, can also be carried out in boric acid processing, can also be in boron
Carried out after acid treatment.It is of course also possible to carry out uniaxial tension by their multiple steps., can be different in uniaxial tension
Uniaxial tension is carried out to master film between roller, hot-rolling can also be used and carry out uniaxial tension.Furthermore it is possible to it is to be stretched in an atmosphere
Deng dry type stretching or the wet tensile that is stretched in the state of with solvent swell.Stretching ratio is usually 3~
8 times.
In order to be dyed with dichroism pigment to polyvinyl alcohol resin film, such as can be by polyvinyl alcohol resin film
It is impregnated in the aqueous solution containing dichroism pigment.As dichroism pigment, specifically, iodine or dichroic dye can be used.Separately
Outside, polyvinyl alcohol resin film preferably carries out impregnation in dyeing before processing in water.
In the case of using iodine as dichroism pigment, generally use by polyvinyl alcohol resin film immersion in containing iodine and
The method dyed in the aqueous solution of KI.The content of iodine in the aqueous solution is usually every 100 parts by weight water 0.01~1
Parts by weight, the content of KI is usually every parts by weight of 100 parts by weight water 0.5~20.The temperature of the aqueous solution used in dyeing
Usually 20~40 DEG C, in addition, the dip time in the aqueous solution is usually 20~1800 seconds.
In the case of using dichroic dye as dichroism pigment, generally use by polyvinyl alcohol resin film immersion in
The method dyed in the aqueous solution comprising water-soluble dichroic dye.With regard to the dichroic dye in the aqueous solution content and
Speech, relative to the parts by weight of water 100, usually 1 × 10-4~10 parts by weight, preferably 1 × 10-3~1 parts by weight.The aqueous solution
The inorganic salts such as sodium sulphate can be contained as dyeing assistant.The temperature of the aqueous dye solutions utilized in dyeing is usually 20~
80 DEG C, in addition, the dip time for the aqueous solution is usually 10~1800 seconds.
Using after the dyeing of dichroism pigment boric acid processing by by dyed polyvinyl alcohol resin film immersion in
Carried out in the aqueous solution containing boric acid.For the amount of the boric acid in the aqueous solution containing boric acid, relative to the weight of water 100
Part, usually 2~15 parts by weight, preferably 5~12 parts by weight.In the case of using iodine as dichroism pigment, this contains boron
The aqueous solution of acid preferably comprises KI.For the amount of the KI in the aqueous solution containing boric acid, relative to the weight of water 100
Part, usually 0.1~15 parts by weight, preferably 5~12 parts by weight.Dip time in the aqueous solution containing boric acid is usually
60~1200 seconds, preferably 150~600 seconds, more preferably 200~400 seconds.The temperature of the aqueous solution containing boric acid is usually 50
More than DEG C, preferably 50~85 DEG C, more preferably 60~80 DEG C.
Washing process is generally carried out to the polyvinyl alcohol resin film after boric acid processing.Washing process is for example by will be through boron
The polyvinyl alcohol resin film immersion of acid treatment is carried out in water.The temperature of water in washing process is usually 5~40 DEG C, leaching
The stain time is usually 1~120 second.Implement drying process after washing, obtain polarizer.Drying process generally utilizes heated-air drying
Machine, far infra-red heater are carried out.The temperature of drying process is usually 30~100 DEG C, preferably 50~80 DEG C.Drying process
Time is usually 60~600 seconds, preferably 120~600 seconds.
Uniaxial tension is so carried out to polyvinyl alcohol resin film, is handled using the dyeing of dichroism pigment and boric acid, is obtained
To polarizer.The thickness of the polarizer is usually in the range of 5~40 μm, in the range of preferably 10~35 μm.
Diaphragm
Said protection film specifically can use cellulose-based resin film, cyclic olefine resin film, acrylic resin film,
The various transparent resin films such as polyester based resin film.
In the case of using cellulose-based resin film as said protection film, preferably at least a portion of cellulose is by ester
The acetate fiber prime system resin of change.Such as triacetyl cellulose, diacetyl cellulose, cellulose-acetate propionate etc. can be included.
Above-mentioned cyclic olefine resin is the list for example with cycloolefin as ENB, polycyclic norborneol alkene monomer
The thermoplastic resin of body unit can be the ring-opening polymerization polymer of above-mentioned cycloolefin, make use of the open loop of cycloolefin of more than two kinds
The hydride or cycloolefin of copolymer and chain olefin, the addition copolymer of the aromatic compound with vinyl.
In addition, polar group can be introduced in cyclic olefine resin.
To make use of the polarizer of adhesive composite and the joint method of diaphragm to be not particularly limited, such as can enumerate
Go out following method：Using the tape casting, wire rod rubbing method, gravure coating process, molding rubbing method, Dipcoat method, spray-on process
Deng the bonding plane that adhesive composite is coated on to polarizer and/or diaphragm, make both overlapping.Above-mentioned the tape casting is that side makes work
Moved up to be applied the incline direction of the polarizer of thing or diaphragm between generally vertical direction, general horizontal direction or both
It is dynamic, while adhesive composite to be coated on to the method on its surface.
After above-mentioned adhesive composite is coated with, clamps polarizer and diaphragm by using nip rolls (nip roll) and make
It is engaged.
In addition, in order to improve cementability, also plasma suitably can be carried out to the surface of polarizer and/or diaphragm
Processing, sided corona treatment, ultraviolet treatment with irradiation, flame treatment, saponification process etc. are surface-treated., can as above-mentioned saponification process
Include the method being impregnated in the aqueous alkali of sodium hydroxide, potassium hydroxide etc..
By polarizer and protection film layer poststack, implement drying process.Drying process for example by by hot blast spray carry out,
Temperature now properly selects in 50~100 DEG C of scopes.Drying time is usually 30~1000 seconds.
<The manufacture method of Polarizer>
Another embodiment of the present invention is the method for manufacturing above-mentioned Polarizer, it is characterised in that is included：(a) inclined
The two sided coatings of light device include acetoacetyl modified polyvinyl alcohol resin, glyoxal crosslinking agent and multivalence of more than two kinds gold
Belong to the adhesive composite of the water soluble salt of ion, generate the stage of bond layer；(b) binder is utilized on above-mentioned bond layer
Roller engages at least more than one diaphragm, makes the stage of Polarizer；(c) above-mentioned Polarizer by least two more than
Dry path, the stage being dried.The moisture rate that can make Polarizer using such method turns into 2.8~4.8%, will be inclined
The thickness of contained bond layer is adjusted to 30~200nm in tabula rasa.Therefore, it is possible to manufacture the Polarizer having the effect that：
Diaphragm will not be also prevented under wet heat condition and is separated with the short side of polarizer with the reduction of light characteristic, therefore can
Improve water resistance
For the polarizing plate making method of the present invention, below as long as no other record, the inscape energy of Polarizer
Enough use the inscape of above-mentioned Polarizer.
In above-mentioned (b) stage, nip rolls is the machinery for being bonded diaphragm at least one side of polarizer, in polarisation
Device, diaphragm top and bottom direction on can be respectively present more than at least one nip rolls, positioned at above-mentioned polarizer, diaphragm
Top and bottom nip rolls by applying pressure by the polarizer between them and diaphragm, so as to which diaphragm is bonded
In polarizer.
In order to which above-mentioned polarizer can be with protecting pressure, the i.e. binder pressure of nip rolls that is intermembranous bonding and applying
0.3~0.9MPa, in the case that above-mentioned binder pressure is less than above range, polarizer is made with protecting intermembranous bond layer to exceed
For the 200nm of the composition of the present invention, damp and hot deterioration occurs, light characteristic reduces, and above-mentioned binder pressure exceedes the situation of above range
Under, less than the 30nm of the composition as the present invention bad order can occur for bond layer.
A part of face on nip rolls for being contacted with above the polarizer by nip rolls, diaphragm and with above-mentioned polarisation
The interval in a part of face on the nip rolls contacted below device, diaphragm, i.e. binder gap (nipgap) can be -1500~
500μm.In the case that above-mentioned binder gap is less than above range, the thickness of above-mentioned bond layer is less than the composition as the present invention
30nm, bad order can occur, more than above range in the case of, the thickness of above-mentioned bond layer exceedes as of the invention
The 200nm of composition, damp and hot deterioration occurs, the problem of light characteristic reduces can occur.Now, made to determine above-mentioned binder gap
Nip rolls positioned at polarizer, the top and bottom of diaphragm is set to mutually closest nip rolls.
The diaphragm being bonded at least one side of polarizer engagement is formed using nip rolls in above-mentioned (b) stage
Polarizer can be dried in above-mentioned (c) stage by drying path more than at least two, the present invention in, for convenience
For the sake of, by the order that Polarizer passes through by multiple dry paths be named as the 1st drying path, the 2nd dry path, the 3rd dry it is logical
Road etc..Above-mentioned dry path can use hot blast, when Polarizer is by more than at least two drying path, preferred follow-up phase
Drying path in hot blast temperature it is higher than the temperature of the hot blast in the drying path of previous stage.For example, the 2nd dries path
The temperature that the temperature of interior hot blast dries the hot blast in path than the 1st is high.More specifically, the 1st dries the temperature of the hot blast in path
Degree is preferably less than 50 DEG C, and the temperature of the hot blast in multiple dry paths in last drying path is preferably more than 80 DEG C.On
In the case of the temperature in the 1st drying path is stated more than 50 DEG C, damp and hot deterioration, light characteristic occur due to moisture evaporation drastically
Reduce, in the case that the temperature of the hot blast in last drying path is less than 80 DEG C, the moisture rate rise of Polarizer, light can occur
Learn characteristic through when reduce the problem of.
<Image display device>
Another program of the present invention is the image display device for possessing above-mentioned Polarizer.
The image display device of the present invention possesses above-mentioned Polarizer, if enumerating specific example, can include liquid crystal
Show device, OLED, flexible display etc., but be not limited to this.
Below in order to contribute to the understanding of the present invention, preferred embodiment is proposed, following embodiment is only to this
Invention is illustrated, and can be variously changed and be corrected in the range of scope of the invention and technological thought, this is for ability
It is clear for field technique personnel, such deformation and amendment belong to appended Patent right requirement, and this is also certain.
In following embodiment and comparative example, represent that " % " and " part " of content is then weight basis as long as no special instructions.
Production Example
The manufacture of the polarizer of Production Example 1.
It is 2400 by average degree of polymerization, the polyvinyl alcohol film for 75 μ m-thicks that saponification degree is 99.9 moles of more than % is with dry type list
Axle stretches about 5 times, and in the case where maintaining extended state, dipping is after 1 minute in 60 DEG C of water (distilled water), with iodine/KI/distillation
The weight of water is than 28 DEG C of the aqueous solution for 0.05/5/100 impregnated of 60 seconds.Then, in the weight of KI/boric acid/distilled water
Amount at 65 DEG C than to be impregnated 300 seconds in 8.5/8.5/100 72 DEG C of aqueous solution, after cleaning 20 seconds with 26 DEG C of distilled water, doing
It is dry, manufacture the polarizer for making iodine in PVA mesentery gas absorption quantities.
The manufacture of the diaphragm of Production Example 2.
Used as the KC8UX of triacetyl cellulose mesentery (Konica company, T) saponification.
The manufacture of the adhesive composite of Production Example 3.
The manufacture of A liquid compositions：Dissolving saponification degree is the acetoacetyl modified of 99.2 moles of % in the water (distilled water)
Polyvinyl alcohol resin (the Le Z200 of one セ ノ of go mono-, the Nippon Synthetic Chemical Industry Co., Ltd), manufacture the content of solid constituent
The aqueous solution as shown in table 1.The aqueous solution of glyoxal crosslinking agent 40% has been added with the content described in table 1 in the above-mentioned aqueous solution
After (big wellization gold), mixing, adhesive A liquid composition has been manufactured.
The manufacture of B liquid compositions：Dissolving saponification degree is the acetoacetyl modified of 99.2 moles of % in the water (distilled water)
Polyvinyl alcohol resin (the Le Z200 of one セ ノ of go mono-, the Nippon Synthetic Chemical Industry Co., Ltd), has manufactured containing for solid constituent
Measure the aqueous solution as shown in table 1.Added in the above-mentioned aqueous solution using the content described in table 1 and be used as the water-soluble of polyvalent metal ion
Property salt zinc chloride (big wellization gold) and zinc nitrate (big wellization is golden) mix afterwards, manufactured bonding agent B liquid compositions.
The A liquid composition of above-mentioned manufacture and B liquid composition are mixed at normal temperatures, stir about 30 minutes, manufactured bonding
Agent composition.
Embodiment 1~8 and comparative example 1~7：The manufacture of Polarizer
The two sides of the polarizer manufactured in above-mentioned Production Example 1 is coated with the content described in table 1 and utilizes above-mentioned manufacture
After the adhesive composite of the method manufacture of example 3, the diaphragm for making above-mentioned Production Example 2 using nip rolls engages.Now, process bar
Part (binder pressure, binder gap) like that, the hot blast dried in path is utilized using the Polarizer of nip rolls engagement as shown in table 1
Drying machine is dried.Process is dried with 5 stages altogether, the 1st, which dries the temperature of the hot blast in path and the 5th, dries in path
Hot blast temperature as shown in table 1, in addition, the 2nd dry path in hot blast temperature be 50 DEG C, the 3rd dry path in
Hot blast temperature be 70 DEG C, the 4th dry path in hot blast temperature be 75 DEG C, in each dry path dry 5 minutes, most
Polarizer has been manufactured eventually.The thickness of contained bond layer in the moisture rate and above-mentioned Polarizer of the Polarizer that measure so manufactures
Degree, is recorded in table 1 together.
Now, the moisture rate of above-mentioned Polarizer is used to the front/rear weight for the heat treatment that 2 hours have been carried out at 105 DEG C
The weight moisture rate determination method measure that amount change is observed.
【Table 1】
Experimental example
The bonding force of experimental example 1. evaluates (cutting tool evaluation)
After the Polarizer of above-mentioned manufacture placed into 1 hour at normal temperatures, in each intermembranous (polarizer and the polarisation of Polarizer
Between device diaphragm) sword of cutting tool is put into, in the way of sword when following standard evaluation promotes sword enters, by it
As a result it is shown in Table 2.
◎：The sword of cutting tool does not enter into all intermembranous.
○：When sword is promoted, at least any one intermembranous, sword stops when entering 1~2mm.
△：When sword is promoted, at least any one intermembranous, sword stops when entering 3~5mm.
×：When sword is promoted, at least any one intermembranous, sword readily enters.
The water resistance of experimental example 2. is evaluated
Each Polarizer for placed 24 hours in the environment of 23 DEG C, relative humidity 55%, using as described below
Method carries out the water-based experiment of heatproof, have rated water resistance.
Using the absorption axiss of Polarizer as long side, Polarizer is cut to 5 × 2cm size and sample is made, correctly
Determine the size of its long side direction.Now, above-mentioned sample is due to being adsorbed in the iodine of light polarizing film, and comprehensively equably shows
Distinctive color.Fig. 1 is the figure for the evaluation method for showing schematically water resistance, and (A) represents the sample 1 before warm water immersion, (B) table
Sample 1 after temperature indicating water retting.As shown in Fig. 1 (A), a short brink of sample is held with tool 5 is held, by length side
To 80% or so be impregnated in 60 DEG C of tank, maintain 8 hours.Then, sample 1 is taken out from tank, wipes moisture.
By above-mentioned such warm water immersion, the polarizer 4 of Polarizer shrinks.By determining from the short side of sample 1
Terminal part 1a (terminal of diaphragm) at centre evaluates the receipts of above-mentioned polarizer 4 to the distance of the end of the polarizer 4 shunk
Contracting degree, is set to contracted length.In addition, as shown in Fig. 1 (B), by warm water immersion, make positioned at the central of Polarizer
Polarizer 4 shrinks, so as to which iodine from the peripheral part dissolution of polarizer 4, produces what is decolourized in the peripheral part of sample 1 between diaphragm
Part 3.Terminal part by the polarizer 4 for the contraction for determining the centre from the short side of sample 1 is peculiar to Polarizer is remained
The distance in region of color evaluate such bleaching level, be set to the length of iodine decolouring.Above-mentioned contracted length is taken off with iodine
The length sum of color is set to total etch length x.Total etch length x is the end 1a from the sample 1 of the centre of the short side of sample 1
To the distance in the region of the distinctive color residual of Polarizer.Contracted length, the decolouring length of iodine and total etch length x are smaller, energy
Enough judge that the cementability in the presence of water is higher.According to total etch length x, evaluated with 4 following grades, its result is recorded in
In table 2.
◎：Total etch length x is less than 0.1mm
○：Total etch length x is more than 0.1mm and less than 0.5mm
△：Total etch length x is more than 0.5mm and less than 2mm
×：Total etch length x is more than 2mm
The transmissivity of experimental example 3., degree of polarization (%)
The Polarizer of manufacture is cut to 4cm × 4cm size, makes test film, the test film is attached to measure branch
After frame, using UV, visible light light spectrometer (V-7100, JASCO Corporation are manufactured) measure, its result is recorded in
In table 2.
【Table 2】
| Adaptation | Water resistance | Transmissivity | Degree of polarization | |
| Embodiment 1 | ◎ | ◎ | 43.1 | 99.996 |
| Embodiment 2 | ◎ | ◎ | 42.9 | 99.997 |
| Embodiment 3 | ◎ | ◎ | 42.8 | 99.997 |
| Embodiment 4 | ◎ | ◎ | 42.8 | 99.997 |
| Embodiment 5 | ◎ | ◎ | 42.9 | 99.997 |
| Embodiment 6 | ◎ | ◎ | 43 | 99.995 |
| Embodiment 7 | ◎ | ◎ | 43 | 99.993 |
| Embodiment 8 | ◎ | ◎ | 42.9 | 99.996 |
| Comparative example 1 | ◎ | ○ | 43 | 99.997 |
| Comparative example 2 | ◎ | ◎ | 43 | 99.992 |
| Comparative example 3 | ◎ | ○ | 42.8 | 99.995 |
| Comparative example 4 | ◎ | ◎ | 42.9 | 99.996 |
| Comparative example 5 | ◎ | ○ | 42.9 | 99.992 |
| Comparative example 6 | ◎ | △ | 43 | 99.995 |
| Comparative example 7 | ◎ | △ | 42.9 | 99.995 |
With reference to table 2, it is thus identified that solid constituent in the aqueous solution of acetoacetyl modified polyvinyl alcohol resin contains
In the case of measuring less than preferable scope (2.5~4.5 weight %) of the invention (comparative example 1), with meeting that the present invention's is preferred
The situation (embodiment 1~8) of scope compare, the moisture rate deficiency of Polarizer, poor water resistance, in the situation more than above range
Under (comparative example 2), the moisture rate increase of Polarizer, the thickness of contained bond layer is thickening in Polarizer, and light characteristic drop occurs
The problem of low.Confirm in addition, the process conditions (binder pressure, binder gap) of Polarizer of the invention depart from the scope of the present invention
In the case of (comparative example 3~4), manufacture departs from contained viscous in the moisture rate of Polarizer required in the present invention, Polarizer
The Polarizer of the thickness range of oxidant layer is connect, thus, it is thus identified that water resistance, light characteristic reduce.The 1st in the drying process of Polarizer
The temperature for drying the hot blast in path exceedes in the case of temperature range (less than 50 DEG C) of the invention (embodiment 7), Neng Gouman
The thickness range of bond layer contained in the moisture rate and Polarizer of required Polarizer in the foot present invention, but with satisfaction
The situation for stating (embodiment 1~6 and 8) of temperature range is compared, and produces the problem of light characteristic slightly reduces, and is dried for the 5th logical
The temperature range of hot blast in road, in the case where departing from the temperature range (more than 80 DEG C) of the present invention (comparative example 5), it is thus identified that
More than the moisture rate of Polarizer required in the present invention, there is the reduction of water resistance and light characteristic.In addition, only use a kind
In the case of the water soluble salt of polyvalent metal ion (comparative example 6 and 7), it is thus identified that water resistance reduces.
Claims (15)
1. Polarizer, it is included：In the diaphragm that at least one side of polarizer engages via bond layer, it is characterised in that institute
State Polarizer moisture rate be 2.8~4.8%, the bond layer by comprising acetoacetyl modified polyvinyl alcohol resin,
The adhesive composite of the water soluble salt of glyoxal crosslinking agent and polyvalent metal ion of more than two kinds is formed, the bond layer
Thickness be 30~200nm.
2. Polarizer according to claim 1, it is characterised in that the adhesive composite includes：Include acetoacetyl
The A liquid of base modified polyvinylalcohol system's resin aqueous solution and glyoxal crosslinking agent and include acetoacetyl modified polyethenol series
The B liquid of the water soluble salt of resin aqueous solution and polyvalent metal ion of more than two kinds.
3. Polarizer according to claim 2, it is characterised in that relative to acetoacetyl modified polyvinyl alcohol resin
The weight % of the aqueous solution 100, the A liquid and B liquid each contained acetoacetyl modified polyvinyl alcohol resin solid into
The content divided is 2.5~4.5 weight %.
4. Polarizer according to claim 1, it is characterised in that the water soluble salt of the polyvalent metal ion is selected from chlorine
Change two or more in zinc, zinc nitrate and aluminum nitrate.
5. Polarizer according to claim 1, it is characterised in that the acetoacetyl modified polyvinyl alcohol resin
Average degree of polymerization is 100~1500.
6. Polarizer according to claim 2, it is characterised in that change relative to acetoacetyl contained in the A liquid
Property polyvinyl alcohol resin total 100 parts by weight of solid constituent, the content of contained glyoxal system crosslinking agent is 30 in the A liquid
~70 parts by weight.
7. Polarizer according to claim 2, it is characterised in that the water soluble salt of the polyvalent metal ion is included and is selected from
Two or more in zinc chloride, zinc nitrate and aluminum nitrate, relative to acetoacetyl modified polyvinyl alcohol contained in the B liquid
It is total 100 parts by weight of solid constituent of resin, the content of the zinc chloride is 2~10 parts by weight.
8. Polarizer according to claim 2, it is characterised in that the water soluble salt of the polyvalent metal ion is included and is selected from
Two or more in zinc chloride, zinc nitrate and aluminum nitrate, relative to acetoacetyl modified polyvinyl alcohol contained in the B liquid
It is total 100 parts by weight of solid constituent of resin, the content of the zinc nitrate or aluminum nitrate is 30~90 parts by weight.
9. image display device, it is included according to Polarizer according to any one of claims 1 to 8.
10. the manufacture method of Polarizer, the moisture rate for being Polarizer is 2.8~4.8%, bonding agent contained in the Polarizer
The thickness of layer is the manufacture method of 30~200nm Polarizer, it is characterised in that is included：
(a) polarizer two sided coatings include acetoacetyl modified polyvinyl alcohol resin, glyoxal crosslinking agent and 2 kinds with
On polyvalent metal ion water soluble salt adhesive composite, generate stage of bond layer；
(b) at least more than one diaphragm is engaged using nip rolls on the bond layer, makes the stage of Polarizer；
With
(c) Polarizer by drying path more than at least two and by the dry stage.
11. the manufacture method of Polarizer according to claim 10, it is characterised in that to Polarizer in (b) stage
The binder pressure of the nip rolls of application is 0.3~0.9MPa.
12. the manufacture method of Polarizer according to claim 10, it is characterised in that binder gap in (b) stage
For -1500 μm~-500 μm.
13. the manufacture method of Polarizer according to claim 10, it is characterised in that in (c) stage, Polarizer leads to
When crossing drying path more than at least two, drying of the temperature than previous stage of the hot blast in the drying path of follow-up phase is led to
The temperature of hot blast in road is high.
14. the manufacture method of Polarizer according to claim 13, it is characterised in that drying more than described at least two
The temperature that the hot blast in path is dried in the 1st initially there are in path is less than 50 DEG C.
15. the manufacture method of Polarizer according to claim 13, it is characterised in that drying more than described at least two
The temperature for the hot blast in drying path being ultimately present in path is more than 80 DEG C.
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| KR1020160100725A KR101775594B1 (en) | 2016-08-08 | 2016-08-08 | Polarizing plate and preparing method for the same |
| KR10-2016-0100725 | 2016-08-08 |
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| JP7046901B2 (en) * | 2018-12-25 | 2022-04-04 | 日東電工株式会社 | Polarizer and its manufacturing method |
| JP2021043370A (en) * | 2019-09-12 | 2021-03-18 | 住友化学株式会社 | Polarizer |
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| CN101363933A (en) * | 2007-08-07 | 2009-02-11 | 住友化学株式会社 | Polarizing plate and production method thereof |
| CN101813799A (en) * | 2009-02-20 | 2010-08-25 | 住友化学株式会社 | Polarization plates and manufacture method thereof |
| KR20160004187A (en) * | 2014-07-02 | 2016-01-12 | 수미토모 케미칼 컴퍼니 리미티드 | Adhesive composition and polarizing plate comprising the same |
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| JP2002221619A (en) * | 2001-01-25 | 2002-08-09 | Gunze Ltd | Polarizing plate |
| JP2005326531A (en) * | 2004-05-13 | 2005-11-24 | Nitto Denko Corp | Polarizing plate equipped with protecting film, manufacturing method therefor, and image display device using polarizing plate |
| JP2008129258A (en) * | 2006-11-20 | 2008-06-05 | Nitto Denko Corp | Method for producing polarizing plate, polarizing plate, optical film and image display device |
| JP2008180765A (en) * | 2007-01-23 | 2008-08-07 | Sumitomo Chemical Co Ltd | Manufacturing method of polarizing film |
| JP5051696B2 (en) * | 2007-04-06 | 2012-10-17 | 住友化学株式会社 | Polarizer |
| JP5147014B2 (en) * | 2008-10-08 | 2013-02-20 | 住友化学株式会社 | High contrast polarizing plate and liquid crystal display device |
| KR101211745B1 (en) * | 2009-06-24 | 2012-12-12 | 주식회사 엘지화학 | Retardation film, fabrication method thereof, and liquid crystal display comprising the same |
| JP2012047799A (en) * | 2010-08-24 | 2012-03-08 | Nitto Denko Corp | Manufacturing method of polarizer |
| KR101459126B1 (en) * | 2011-12-21 | 2014-11-07 | 제일모직주식회사 | Polarizer plate and liquid crystal display comprising the same |
| KR101397705B1 (en) * | 2011-12-30 | 2014-05-23 | 제일모직주식회사 | Adhesive composition for polarizing plate |
| WO2016002808A1 (en) * | 2014-07-02 | 2016-01-07 | 住友化学株式会社 | Adhesive composition and polarizing plate containing same |
| KR20160028316A (en) * | 2014-09-03 | 2016-03-11 | 스미또모 가가꾸 가부시키가이샤 | Adhesive composition and polarizing plate using the same |
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| CN101363933A (en) * | 2007-08-07 | 2009-02-11 | 住友化学株式会社 | Polarizing plate and production method thereof |
| CN101813799A (en) * | 2009-02-20 | 2010-08-25 | 住友化学株式会社 | Polarization plates and manufacture method thereof |
| KR20160004187A (en) * | 2014-07-02 | 2016-01-12 | 수미토모 케미칼 컴퍼니 리미티드 | Adhesive composition and polarizing plate comprising the same |
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| CN107703577B (en) | 2021-09-21 |
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