CN103339538A - Highly adhesive polyester film for protection of polarizers - Google Patents

Highly adhesive polyester film for protection of polarizers Download PDF

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Publication number
CN103339538A
CN103339538A CN2012800075825A CN201280007582A CN103339538A CN 103339538 A CN103339538 A CN 103339538A CN 2012800075825 A CN2012800075825 A CN 2012800075825A CN 201280007582 A CN201280007582 A CN 201280007582A CN 103339538 A CN103339538 A CN 103339538A
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CN
China
Prior art keywords
quality
polyvinyl alcohol
mylar
polaroid
resin
Prior art date
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Granted
Application number
CN2012800075825A
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Chinese (zh)
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CN103339538B (en
Inventor
中谷充晴
熊谷荣二
东浦真哉
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Toyobo Co Ltd
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Toyobo Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/30—Polarising elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00—Coating compositions 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; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C09D129/02—Homopolymers or copolymers of unsaturated alcohols
    • C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02—Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • 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
    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
    • 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
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
    • 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
    • C09J2429/00—Presence of polyvinyl alcohol
    • 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
    • C09J2467/00—Presence of polyester
    • 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
    • C09J2467/00—Presence of polyester
    • C09J2467/006—Presence of polyester in the substrate
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/133528—Polarisers
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2201/00—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00
    • G02F2201/50—Protective arrangements
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2202/00—Materials and properties
    • G02F2202/28—Adhesive materials or arrangements

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nonlinear Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mathematical Physics (AREA)
  • Polarising Elements (AREA)
  • Laminated Bodies (AREA)
  • Liquid Crystal (AREA)
  • Paints Or Removers (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

Provided is a highly adhesive polyester film for protecting polarizers, which has excellent adhesion to polarizers. A highly adhesive polyester film for protecting polarizers, which has a highly adhesive layer on at least one surface thereof, wherein the highly adhesive layer comprises a polyester resin (A), a polyvinyl alcohol resin (B) and a cross-linking agent (C), the polyester resin (A) has an acid value of 20 KOHmg/g or less, and the polyvinyl alcohol resin (B) has a degree of saponification of 60-85 mol%.

Description

Polaroid protection easy-adhesion mylar
Technical field
The present invention relates to the polaroid protection easy-adhesion mylar for the protection of polaroid.Specifically, relate to polaroid excellent in adhesion protection easy-adhesion mylar with polaroid.
Background technology
In the liquid crystal watch showing device, owing to its image forming mode and at the both sides of the glass substrate that forms liquid crystal panel surface configuration Polarizer.Polarizer has following structure usually: the two sides at the polaroid that is formed by dichroic material such as polyvinyl alcohol film and iodine is fitted with polaroid protective film by hydrophilic adhesive such as polyvinyl alcohol resins.As the diaphragm for the protection of polaroid, from the aspect of optical characteristics, the transparency, use cellulose triacetate film so far always.
Yet the permanance of Triafol T is insufficient, and when using with cellulose triacetate film as the Polarizer of polaroid protective film under high temperature or high humidity, the performance of Polarizers such as degree of polarization, tone reduces sometimes.In addition, require the Polarizer filming for the slimming of tackling display in recent years, but from keeping the angle of moisture isolation characteristic, there is boundary in the filming of cellulose triacetate film.Therefore, as the polaroid protective film with permanance and moisture isolation, use mylar (referring to patent documentation 1～5) has been proposed.
Alkali treatment etc. has been implemented on the surface that is used as the cellulose triacetate film of polaroid protective film, has the compatibility high with hydrophilic adhesive.Therefore, has high cementability by the cellulose triacetate film diaphragm that forms and the polaroid that is coated with hydrophilic adhesive.Yet the cementability of mylar and hydrophilic adhesive is insufficient, and particularly for the mylar that has orientation by stretch processing, this tendency is more remarkable.Therefore, in the patent documentation 1～3 and 5 for improve with polaroid or coat polaroid hydrophilic adhesive cementability and proposed at mylar easy adhesive linkage to be set.
The prior art document
Patent documentation
Patent documentation 1: Japanese kokai publication hei 8-271733 communique
Patent documentation 2: Japanese kokai publication hei 8-271734 communique
Patent documentation 3: TOHKEMY 2009-157361 communique
Patent documentation 4: TOHKEMY 2010-277028 communique
Patent documentation 5: TOHKEMY 2011-8170 communique
Summary of the invention
The problem that invention will solve
The compatibility of mylar and water is low, and it is remarkable especially as this tendency of the mylar of dicarboxylic acid composition to have an aromatic dicarboxylic acid.In addition, it is lower to have the compatibility of the mylar of crystal orientation and water by stretching.And polaroid, be coated in the bonding agent on the polaroid, polyvinyl alcohol resin is principal ingredient, has high water wettability.Because the difference of this character, the compatibility of mylar and polaroid, this bonding agent is low, is difficult to both bonding securely.Therefore, even disclosed mylar with easy adhesive linkage in patent documentation 1～3 and 5 is compared with cellulose triacetate film, do not obtain sufficient cementability yet.Therefore; long-term when using with existing mylar to the Polarizer of diaphragm as display member; sometimes can float, peel off between diaphragm/polaroid, cause the polarized light property reduction by the variation of the amount of moisture in the polaroid, visual variation such as blank appear.
Under this present situation, the purpose of problem of the present invention is to provide a kind of mylar, and it has the polyvinyl alcohol resin layer that makes mylar and polaroid or be coated on bonding agent on the polaroid etc. bonding means securely.
For the scheme of dealing with problems
The inventor etc. carried out deep research and discussion in order to address the above problem and visualize between mylar and polyvinyl alcohol resin layer arrange contain the polyester resin high with the compatibility of mylar, with the high polyvinyl alcohol resin of the compatibility of polyvinyl alcohol resin layer and the layer of crosslinking chemical.Yet these compositions are only made up in discoveries such as the inventor merely can't give full play to the function that makes mylar and the driving fit of polyvinyl alcohol resin layer that each composition brings.Therefore, the inventor etc. day and night study, found that, in above-mentioned design, has the vibrin of certain acid number as vibrin by employing, and then, adopt the polyvinyl alcohol resin with certain saponification degree as polyvinyl alcohol resin, the separately and bonding effect high resin bed of compatibility that can bring into play effectively that each composition brings.
The inventor etc. have carried out further deep research based on above-mentioned cognition, found that, by adopting the reactive high crosslinking chemical with hydroxyl, can be further the polyvinyl alcohol resin layer of bonding mylar and polaroid, bonding agent etc. securely.The inventor etc. have carried out further discussion and improvement based on these understanding, thereby have finished the present invention.
Typical example of the present invention below is shown.
The 1st technical scheme is a kind of polaroid protection easy-adhesion mylar; it is for having the mylar of easy adhesive linkage at least at single face; described easy adhesive linkage contains polyester resin (A), polyvinyl alcohol resin (B) and crosslinking chemical (C); the acid number of described polyester resin (A) is below the 20KOHmg/g, and the saponification degree of described polyvinyl alcohol resin (B) is 60～85 moles of %.
The 2nd technical scheme is that the easy-adhesion mylar is used in aforementioned polaroid protection, and wherein, aforementioned vibrin (A) contains the 5-sulfoisophthalic acid composition of 1～15 mole of % that accounts for the dicarboxylic acid composition.
The 3rd technical scheme is that the easy-adhesion mylar is used in aforementioned polaroid protection, and wherein, aforementioned crosslinking chemical (C) is isocyanate compound or melamine compound.
The 4th technical scheme is that the easy-adhesion mylar is used in aforementioned polaroid protection, and wherein, in the aforementioned easy adhesive linkage, the mass ratio of polyester resin (A), polyvinyl alcohol resin (B) and crosslinking chemical (C) satisfies following formula:
0.8≤（A）/（B）≤5
2≤（（A）+（B））/（C）≤50。
The 5th technical scheme is a kind of Polarizer, and its two sides at polaroid has polaroid protective film, and the polaroid protective film of the face of at least one side is aforementioned polaroid protection easy-adhesion mylar.
The effect of invention
Polaroid of the present invention protection is with easy-adhesion mylar and polaroid or be coated with polyvinyl alcohol resin layer excellent in adhesion of bonding agent representative thereon.Therefore, mylar of the present invention can be used as the diaphragm of polaroid aptly.By using this mylar of the present invention as the diaphragm of polaroid, can make permanance and water preventing ability cheaplyer and be better than in the past Polarizer.In addition, the excellent in te pins of durability of Polarizer of the present invention therefore can further filming compared with the past.Therefore, by utilizing Polarizer of the present invention, can make the further slimming of LCD.
Embodiment
(mylar)
The mylar that uses as base material is the film that mainly is made of vibrin in the present invention.Here, " the mainly film that is made of vibrin " refers to the film that formed by the resin combination that contains the vibrin more than the 50 quality %, during with other polymer blendings, mean and contain the above vibrin of 50 quality %, during with other monomer copolymerizations, mean and contain the above polyester structural units of 50 moles of %.The preferred polyester film contains the above vibrin of 90 quality %, more preferably more than the 95 quality %, and 100 quality % more preferably.
As vibrin, material is not particularly limited multipolymer or its blending resin that can use dicarboxylic acid composition and glycol component polycondensation to form.As the dicarboxylic acid composition, for example can list: terephthalic acid (TPA), m-phthalic acid, phthalic acid, 2, the 5-naphthalenedicarboxylic acid, 2, the 6-naphthalenedicarboxylic acid, 1, the 4-naphthalenedicarboxylic acid, 1, the 5-naphthalenedicarboxylic acid, the diphenyl carboxylic acid, the biphenoxyl ethane dicarboxylic acid, the diphenylsulphone carboxylic acid, the anthracene dicarboxylic acid, 1,3-cyclopentane diacid, 1, the 3-cyclohexane diacid, 1, the 4-cyclohexane diacid, six hydrogen terephthalic acid (TPA)s, six hydrogen m-phthalic acids, malonic acid, dimethyl malonic acid, succinic acid, 3, the 3-diethyl succinic acid, glutaric acid, 2,2-dimethylated pentanedioic acid, hexane diacid, 2-methyl hexane diacid, trimethyladipic acid, heptandioic acid, azelaic acid, dimer acid, decanedioic acid, suberic acid, dodecanedioic acid etc.
As the glycol component that constitutes vibrin, for example can list: ethylene glycol, propylene glycol, 1,6-hexanediol, neopentyl glycol, 1,2-cyclohexanedimethanol, 1,4-cyclohexanedimethanol, 1,10-decanediol, 1, ammediol, 1,4-butylene glycol, 1,5-pentanediol, 1,6-hexanediol, 2, two (4-hydroxy phenyl) propane of 2-, two (4-hydroxy phenyl) sulfone etc.
The dicarboxylic acid composition and the glycol component that constitute vibrin can be used respectively more than a kind or 2 kinds.In addition, can suitably add other hydroxyl compositions such as other sour compositions, trimethylolpropane such as trimellitic acid.
As vibrin, particularly can list: polyethylene terephthalate, PTT, polybutylene terephthalate, PEN etc., in the middle of these for the balance of rerum natura and cost preferred polyethylene terephthalate.In addition, in order to control optical characteristics such as polarity and contain other copolymer compositions, other polymkeric substance also are preferred modes.The angle of optical characteristics from the control mylar as preferred copolymer composition, can list: diethylene glycol, have being copolymerized into of norborene at side chain and grade.
Therefore mylar of the present invention preferably has the high transparency as protective film for polarizing plate.Polaroid protection of the present invention is more than 85% with preferred its total light transmittance of the transparency of mylar, more preferably more than 87%, more preferably more than 88%, further is preferably more than 89%, is preferably more than 90% especially.In addition, mist degree is preferably below 3%, more preferably below 2.5%, more preferably below 2%, is preferably below 1.5% especially.The total light transmittance of mylar for example can be measured according to the method for putting down in writing among the embodiment described later.
Sometimes make for processing such as the sliding that improves mylar, coiling and contain inert particle in the film, but in order to keep the high transparency, the content of the inert particle in the preferred film is few as far as possible.Therefore, preferably make the multilayer that only contains particle on the top layer of film and constitute, perhaps, make not contain particle in fact in the film and only make the easy adhesive linkage of the single face at least that is layered in mylar contain particulate.
In addition, " not containing particle in fact " refers to, for example inorganic particle is below the 50ppm when with x-ray fluorescence analysis the element that derives from particle being carried out quantitative test, is preferably below the 10ppm, most preferably is the following content of detection limit.This be because, even initiatively particle is not added in the base film, derive from the dirt that adheres on production line in the manufacturing process of pollutant component, material resin or film of external foreign matter, the device sometimes and can peel off and be blended in the film.
In addition, when base film was made the multilayer formation, internal layer did not contain inert particle in fact, only makes two kinds of three layers of formations that outermost layer contains inert particle can take into account the transparency and processability, is preferred.
Thickness to film is not particularly limited in the present invention, and when reducing the thickness of Polarizer for the slimming of display, the thickness of film is preferably below the 200 μ m, more preferably below the 100 μ m.And for keeping as for the physical strength of diaphragm, the thickness of film is preferably more than the 10 μ m, more preferably more than the 12 μ m, more preferably more than the 20 μ m.
Mylar as base material can be individual layer, also can be folded the forming layer by layer more than 2 kinds.In addition, as long as in the scope of performance effect of the present invention, can make as required and contain various adjuvants in the film.As adjuvant, for example can list: antioxidant, photostabilizer, antigelling agent, organic wetting agent, antistatic agent, ultraviolet light absorber, surfactant etc.When film had stacked formation, it also was preferred containing adjuvant according to the function of each layer as required.For example, adding ultraviolet light absorber etc. for the light deterioration that prevents polaroid at internal layer also is preferred mode.
Mylar can be by for example melt extruding into above-mentioned vibrin the film shape, making its cooling curing come film forming method etc. to obtain with the curtain coating drum.As mylar of the present invention, can use in no oriented film, the oriented film any, from the preferred oriented film in the aspect of permanance such as physical strength, chemical proofing.When mylar is oriented film, its drawing process is not particularly limited, can adopts vertical uniaxial tension method, laterally uniaxial tension method, progressively biaxial stretch-formed method, biaxial stretch-formed method etc. simultaneously in length and breadth in length and breadth.
(easily adhesive linkage)
Mylar of the present invention for improve with polaroid and be arranged on its single face or two sides water system bonding agent etc. the polyvinyl alcohol resin layer cementability and its at least single face be laminated with easy adhesive linkage, described easy adhesive linkage is that the polyester resin (A) below the 20KOHmg/g, polyvinyl alcohol resin (B) that saponification degree is 60～85 moles of % and the resin combination of crosslinking chemical (C) form by containing acid number.Easily adhesive linkage can arrange on the two sides of mylar, also can be only in the single face setting of mylar, at another side setting resin-coated layer not of the same race.
Though bound by theory not, can think, by the combination acid number be the specific polyester resin (A) below the 20KOHmg/g, specific polyvinyl alcohol resin (B) and the crosslinking chemical (C) that saponification degree is 60～85 moles of %, polyester resin and polyvinyl alcohol resin are easily forming unit, independent structures territory respectively in the adhesive linkage, form the phase separation structure that is also become island structure usually.Can think, by forming the isolating construction of this domain unit, the domain that is made of polyester resin is that bring with cementability mylar and brought by the domain that polyvinyl alcohol resin constitutes taking into account aptly with these two functions of the cementability polyvinyl alcohol resin layer and can be not impaired mutually.Can think that crosslinking chemical (C) promotes the formation of this domain structure and keeps by making the crosslinked and cohesion of polyvinyl alcohol resin (B).
Each composition of following commute adhesive linkage is elaborated.
(polyester resin (A))
The polyester resin (A) that uses in the easy adhesive linkage of the present invention is the multipolymer that dicarboxylic acid composition and glycol component polycondensation form, and as dicarboxylic acid composition and glycol component, can use the material as the mylar of aforementioned substrates.From the angle of raising with the cementability of mylar base material, the preferred use and the dicarboxylic acid composition of the dicarboxylic acid composition that has identical or similar structural property as the dicarboxylic acid composition in the mylar of base material as polyester resin (A).Therefore, when for example adopting aromatic dicarboxylic acid as the dicarboxylic acid composition of mylar, preferably use aromatic dicarboxylic acid as the dicarboxylic acid composition of polyester resin (A).As this aromatic dicarboxylic acid composition, most preferably terephthalic acid (TPA) and m-phthalic acid.Can add other aromatic dicarboxylic acids with 10 moles of scopes below the % with respect to whole dicarboxylic acid compositions and make its copolymerization.
In addition, as the glycol component of polyester resin (A), preferably with the glycol of ethylene glycol and side chain as constituent.Can think, by having the stress relaxation that branched structure can help easy adhesive linkage place, bring into play adaptation aptly.Glycol component for aforementioned side chain, for example can list: 2,2-dimethyl-1, ammediol, 2-methyl-2-ethyl-1, ammediol, 2-methyl-2-butyl-1, ammediol, 2-methyl-2-propyl group-1, ammediol, 2-methyl-2-isopropyl-1, ammediol, 2-methyl-2-n-hexyl-1, ammediol, 2,2-diethyl-1, ammediol, 2-ethyl-2-normal-butyl-1, ammediol, 2-ethyl-2-n-hexyl-1, ammediol, 2,2-di-n-butyl-1, ammediol, 2-normal-butyl-2-propyl group-1, ammediol, and 2,2-di-n-hexyl-1, ammediol etc.
For the mol ratio of the glycol component of aforementioned side chain, with respect to whole glycol component, lower limit is preferably 10 moles of %, is preferably 20 moles of % especially.And the upper limit is preferably 80 moles of %, and more preferably 70 moles of % are preferably 60 moles of % especially.In addition, can be as required and also with diethylene glycol, propylene glycol, butylene glycol, hexanediol or 1,4-cyclohexanedimethanol etc.
From with the aspect of the compatibility of polyvinyl alcohol resin (B), the polyester resin that uses among the present invention (A) preferably uses water-soluble or water-dispersed resin.For water-solubleization or the aqueous dispersionization of polyester resin, preferred copolymerization contains the compound of hydrophilic radicals such as sulphonate-base, carboxylate group.Wherein, hang down to control with crosslinking chemical reactive from the acid number that keeps polyester resin (A) and give hydrophilic angle simultaneously, be suitably the dicarboxylic acid composition with sulphonate-base.As the dicarboxylic acid composition with sulphonate-base, for example can list: sulfo group terephthalic acid (TPA), 5-sulfoisophthalic acid, 4-sulfo group naphthalene m-phthalic acid-2,7-dicarboxylic acid and 5-(4-sulfophenoxy) m-phthalic acid or its alkali metal salt, wherein especially preferred 5-sulfoisophthalic acid.Dicarboxylic acid composition with sulphonate-base preferably accounts for 1～15 mole of % of the dicarboxylic acid composition of vibrin (A), more preferably 1.5～12 moles of %, more preferably 2～10 moles of %.Dicarboxylic acid composition with sulphonate-base is above-mentioned lower limit when above, suits for water-solubleization or the aqueous dispersionization of polyester resin.In addition, the dicarboxylic acid composition with sulphonate-base is above-mentioned upper limit when following, suits for the cementability with the mylar base material.
Polyester resin (A) preferably conduct is less with the carboxylic acid group of the reactive group of crosslinking chemical (C).Can think, owing to have reactivity reduction feasible with reactive carboxyl of crosslinking chemical and crosslinking chemical by minimizing, as a result of, not mix fully with polyvinyl alcohol resin, can keep by the formed domain structure of crosslinked polyvinyl alcohol resin.From this angle, the acid number of polyester resin (A) is below the 20KOHmg/g, is preferably below the 15KOHmg/g, more preferably below the 10KOHmg/g, more preferably below the 8KOHmg/g, further is preferably below the 5KOHmg/g.The acid number of polyester resin (A) can be obtained theoretically according to the result based on the constituent analysis of titrimetry described later or NMR etc.
Want the acid number of polyester resin (A) is controlled in above-mentioned scope, the preferred introducing amount that reduces the carboxylate group that is used for water-solubleization or aqueous dispersionization, perhaps adopt carboxylate group hydrophilic radical in addition, perhaps reduce the terminal concentration of carboxylic acid of polyester resin.As the method for the terminal concentration of the carboxylic acid that reduces polyester resin, the preferred polyester resin that carries out end modified to the carboxylic acid terminal groups that adopts perhaps adopts the big polyester resin of number-average molecular weight of polyester resin.Therefore, the number-average molecular weight of polyester resin (A) is preferably more than 5000, more preferably more than 6000, more preferably more than 10000.In addition, preferred content constituent, that have the sour composition of 3 above carboxyls that reduces as polyester resin (A).
Glass transition temperature to polyester resin (A) is not particularly limited, and is preferably 20～90 ℃, more preferably 30～80 ℃.Glass transition temperature is above-mentioned lower limit when above, suits for anti-adhesive, and glass transition temperature is above-mentioned upper limit when following, suits for the cementability with the mylar base material.
Easily the content of the polyester resin (A) in the adhesive linkage is preferably more than the 40 quality % and below the 90 quality %, more preferably more than the 45 quality % and below the 85% quality %, more preferably more than the 50 quality % and below the 80 quality %.The content of polyester resin (A) is above-mentioned lower limit when above, suits for the cementability with the mylar base material, is above-mentioned upper limit when following, suits for the cementability with the polyvinyl alcohol resin of polaroid, hydrophilic adhesive etc.
(polyvinyl alcohol resin (B))
Polyvinyl alcohol resin is not particularly limited, for example can lists: the polyvinyl alcohol (PVA) that the polyvinyl acetate (PVA) saponification is obtained; Its derivant; Further saponified with the multipolymer of the monomer that has copolymerization with vinyl acetate; Polyvinyl alcohol (PVA) has been carried out the modified polyvinylalcohol of acetalation, urethane, etherificate, grafting, Phosphation etc.; Deng.As aforementioned monomer, can list: unsaturated carboxylic acid and ester classes thereof such as maleic acid (acid anhydride), fumaric acid, crotonic acid, itaconic acid, (methyl) acrylic acid; Alpha-olefin such as ethene, propylene, (methyl) allyl sulphonic acid (sodium), sodium sulfonate (monoalkyl malate), sodium disulfonate alkyl malate, N hydroxymethyl acrylamide, acrylamide alkyl sulfonic acid alkali salt, N-vinyl pyrrolidone, N-vinyl pyrrolidone derivant etc.These polyvinyl alcohol resins can only use a kind, and also two or more kinds may be used.
As the polyvinyl alcohol resin that uses among the present invention (B), can example illustrate: vinyl alcohol-vinyl acetate co-polymer, vinyl alcohol-vinyl butyral multipolymer, ethylene-vinyl alcohol copolymer, optimal ethylene alcohol-vinyl acetate co-polymer, ethylene-vinyl alcohol copolymer in the middle of these.The degree of polymerization of polyvinyl alcohol resin (B) is not particularly limited, and from the aspect of coating fluid viscosity, preferred degree of polymerization is below 3000.
The copolymerization ratio of vinyl alcohol is represented with saponification degree.It is above and 85 moles below the % that the saponification degree of polyvinyl alcohol resin of the present invention (B) is preferably 60 moles of %, more preferably 65 moles of % are above and 83 moles below the %, more preferably 68 moles of % are above and 80 moles below the %, further be preferably more than 70 moles of % and less than 80 moles of %, more preferably 71 moles of % are above and 78 moles below the % again, and it is above and 75 moles below the % to be preferably 73 moles of % especially.The saponification degree of polyvinyl alcohol resin (B) is above-mentioned lower limit when above, can more appropriately form cross-linked structure with crosslinking chemical (C).In addition, when the saponification degree of polyvinyl alcohol resin (B) is the above-mentioned upper limit following (or less than it), can more appropriately bring into play the compatibility with polyester resin (A).The saponification degree of ethenol system resin can be by the required quantity of alkali consumption of the hydrolysis of copolymerization units such as vinyl acetate, obtain based on the composition analysis of NMR.
As the content of polyvinyl alcohol resin (B), in easy adhesive linkage, be preferably more than the 10 quality % and below the 60 quality %, more preferably 15 quality % are above and below the 55% quality %, and more preferably 20 quality % are above and below the 50 quality %.The content of polyvinyl alcohol resin (B) is above-mentioned lower limit when above, suits for the cementability with the polyvinyl alcohol resin layer of polaroid, bonding agent etc., is above-mentioned upper limit when following, suits for the cementability with the mylar base material.
(crosslinking chemical (C))
As crosslinking chemical (C), then be not particularly limited as long as have bridging property with hydroxyl, can list: the compound of melamine class, isocyanates, carbodiimide Lei, oxazoline class, epoxies etc.From the aspect of the ageing stability of coating fluid, the compound of preferred melamine class, isocyanates, carbodiimide Lei, oxazoline class.And then crosslinking chemical preferably carries out melamine compounds or the isocyanate ester compound of cross-linking reaction aptly with the hydroxyl of polyvinyl alcohol resin (B).Can think, this be because, carbodiimide class crosslinking chemical and carboxyl reaction, and melamine compounds or isocyanate ester compound and hydroxyl reaction, thereby more appropriately form cross-linked structure with the polyvinyl alcohol resin (B) that has hydroxyl as functional group.Wherein, carry out cross-linking reaction and the excellent angle of the transparency aptly from the hydroxyl with polyvinyl alcohol resin, especially preferably use isocyanate ester compound.In addition, suitably use catalyzer etc. as required in order to promote cross-linking reaction.
As isocyanate compound, can use low molecule or high molecular diisocyanate or the polyisocyanates more than 3 yuan.For example, as isocyanate compound, can list: 2, the 4-toluene diisocyanate, 2, the 6-toluene diisocyanate, 4,4 '-methyl diphenylene diisocyanate, 2,4 '-methyl diphenylene diisocyanate, 2,2 '-methyl diphenylene diisocyanate, 1, the 5-naphthalene diisocyanate, 1, the 4-naphthalene diisocyanate, phenylene diisocyanate, tetramethylbenzene dimethyl diisocyanate, 4,4 '-diphenyl ether diisocyanate, 2-nitro diphenyl-4,4 '-diisocyanate, 2,2 '-diphenyl propane-4,4 '-diisocyanate, 3,3 '-dimethyl diphenylmethane-4,4 '-diisocyanate, 4,4 '-diphenyl propane diisocyanate, 3,3 '-dimethoxy diphenyl-4, aromatic diisocyanate classes such as 4 '-diisocyanate, aromatic series aliphatic diisocyanate classes such as xylylene diisocyanate, isophorone diisocyanate and 4, the 4-dicyclohexyl methyl hydride diisocyanate, 1, ester ring type diisocyanates such as two (isocyanates methyl) cyclohexanes of 3-, hexamethylene diisocyanate and 2,2, aliphatic diisocyanate classes such as 4-trimethyl hexamethylene diisocyanate, and the trimer of these isocyanate compounds.And then, the high molecular end that can list the reaction of the excess quantity of these isocyanate compounds and following compound and obtain contains isocyanate-based compound: low molecular activity hydrogen compounds such as ethylene glycol, propylene glycol, trimethylolpropane, glycerine, sorbierite, ethylenediamine, monoethanolamine, diethanolamine, triethanolamine, or polyester polyols alcohols, polyether glycol class, polyamide-based contour molecular activity hydrogen compound.
As melamine compound, can list and be substituted base-(CH 2) nIn-O-R(the formula, n is 1～3 integer, and R is the alkyl of carbon number 1～4.) melamine compound that replaced, the R in the aforementioned formula is preferably methyl.The above-mentioned substituent quantity that 1 melamine structure has is preferably 3～6.Object lesson as melamine compound, can list: M-3, the MK of the manufacturing Sumitex Resin of Sumitomo Chemical Co series, M-6, M-100, MC etc., SANWA Chemical Co., methylated melamine resin M W-22, MX-706, MX-042 etc. that Ltd. makes.
As the crosslinking chemical that uses among the present invention (C), the blocked isocyanate compounds also is preferred.By adding the blocked isocyanate compounds, can more appropriately improve the ageing stability of coating fluid.
The blocked isocyanate compounds can make above-mentioned isocyanate compound and end-capping reagent carry out addition reaction by existing known method to prepare.As isocyanate-terminated dose, for example can list: phenols such as phenol, cresols, xylenols, resorcinol, nitrophenol, chlorophenol; Sulfo-phenols such as thiophenol, methyl thiophenol; Oximes such as acetyl oxime, methyl ethyl ketoxime, cyclohexanone-oxime; Alcohols such as methyl alcohol, ethanol, propyl alcohol, butanols; Chlorohydrin, 1, halogens such as 3-two chloro-2-propyl alcohol replace alcohols; Tertiary alcohols such as the tert-butyl alcohol, tert-pentyl alcohol; Lactams such as epsilon-caprolactams, δ-valerolactam, butyrolactam, azetidinone; Aromatic amine; Acid imide; Diacetone, acetoacetate, malonic ester isoreactivity methylene compound; Thio-alcohol; The imines class; The urea class; The biaryl compound class; Sodium bisulfite etc.
As the content of crosslinking chemical (C), easily be preferably in the adhesive linkage more than the 2 quality % and below the 50 quality %, more preferably more than the 5 quality % and below the 40% quality %, more preferably more than the 8 quality % and below the 30 quality %.The content of crosslinking chemical (C) is above-mentioned lower limit when above, suits for being cross-linked to form of polyvinyl alcohol resin, is above-mentioned upper limit when following, and the cementability effect of bringing for the performance resin glue suits.
The compounding of polyester resin (A) and polyvinyl alcohol resin (B) is than (A)/(B) be preferably 0.8～5 by mass ratio, and more preferably 1～4, more preferably 2～4, be preferably 2.5～3.5 especially.(A)/(B) be above-mentioned lower limit when above, suit for the cementability with the mylar base material, be above-mentioned upper limit when following, suit for the cementability with the polyvinyl alcohol resin layer of polaroid, bonding agent etc.
The compounding of polyester resin (A) and polyvinyl alcohol resin (B) and crosslinking chemical (C) is than ((A)+(B))/(C) be preferably 2～50 by mass ratio, and more preferably 5～40, more preferably 8～30.((A)+(B))/(C) is above-mentioned lower limit when above, and the cementability effect of bringing for performance resin glue composition suits, and is above-mentioned upper limit when following, and the cementability effect of bringing for being separated suits.
Easy adhesive linkage of the present invention with respect to polaroid, the aqueous adhesive of polaroid, aqueous adhesive, particularly polyvinyl alcohol, shows the high adhesiveness equal with Triafol T by adopting above-mentioned composition.Particularly, be preferably more than 90% based on the remaining area after the adhesive test described later water system bonding agent is peeled off for 1 time, more preferably more than 95%, more preferably 100%, remaining area after peeling off continuously for 5 times is preferably more than 75%, more preferably more than 85%, more preferably more than 95%, the remaining area after peeling off continuously for 10 times is preferably more than 50%, more preferably more than 80%, more preferably more than 90%, further be preferably more than 93%, be preferably more than 95% especially.
(adjuvant)
In easy adhesive linkage of the present invention, can in the scope of not damaging effect of the present invention, add known adjuvant, for example the particle of surfactant, antioxidant, catalyzer, heat-resisting stabilizing agent, weather-proof stabilizing agent, ultraviolet light absorber, organically easy lubrication prescription, pigment, dyestuff, organic or inorganic, antistatic agent, nucleator etc.
Among the present invention, in order further to improve the anti-adhesive of easy adhesive linkage, adding particle in the easy adhesive linkage also is preferred mode.In the present invention as making the particle that contains in the easy adhesive linkage, for example can list inorganic particle, organic polymer particles, described inorganic particle has: titanium dioxide, barium sulphate, calcium carbonate, calcium sulphate, silicon dioxide, aluminium oxide, talcum, porcelain earth, clay etc. or their potpourri, and with other conventional inorganic particles, calcium phosphate for example, mica, hectorite, zirconia, tungsten oxide, lithium fluoride, calcium fluoride etc. are used in combination inorganic particle that forms etc., and described organic polymer particles can list phenylethylene, acrylic compounds, melamine class, the benzocarbamidine amine, silicone based etc.
Easily the mean grain size of the particle in the adhesive linkage is (based on the mean grain size of the number benchmark of SEM.Be preferably 0.04～2.0 μ m, more preferably 0.1～1.0 μ m down together).The mean grain size of inert particle is during less than 0.04 μ m, becomes insufficient in the concavo-convex formation of film surface, and therefore processing such as the sliding of film, batching property can reduce sometimes, and the processability reduction when fitting.Otherwise, when surpassing 2.0 μ m, particle detachment takes place easily and not preferred.Easily the granule density in the adhesive linkage is preferably 1～20 quality % in solid constituent, more preferably 5～15 quality %.
Easily the thickness of adhesive linkage can suitably be set in the scope of 0.001～2.00 μ m in the present invention, wants to take into account processability and cementability, is preferably the scope of 0.01～1.00 μ m, more preferably 0.02～0.80 μ m, more preferably 0.05～0.50 μ m.When easily the thickness of adhesive linkage was less than 0.01 μ m, it is insufficient that cementability becomes.If easily the thickness of adhesive linkage surpasses 2.00 μ m, then stick together sometimes.
(the polaroid protection manufacturing of easy-adhesion mylar)
For the manufacture method of polaroid protection of the present invention with the easy-adhesion mylar, be that example describes with polyethylene terephthalate (following brief note is PET) film, but be not limited to this certainly.
After the PET resin fully carried out vacuum drying, supply with extruder, about 280 ℃ fusion PET resin is melt extruded with sheet to the rotation chill roll from the T mould, apply method by static and carry out the cooling curing PET sheet that do not stretched.The aforementioned PET of stretching sheet can be that individual layer constitutes, and the multilayer that also can be based on coetrusion constitutes.
The PET sheet is not implemented uniaxial tension or the biaxial stretch-formed crystal orientationization that makes by gained is stretched.When for example biaxial stretch-formed, longitudinally be stretched to 2.5～5.0 times with the roller that is heated to 80～120 ℃ and obtain controlling the end of film with clip after the uniaxial tension PET film, cause the hot blast district that is heated to 80～180 ℃, broad ways is stretched to 2.5～5.0 times.In addition, during uniaxial tension, in stenter in-draw to 2.5～5.0 times.The heat-treatment zone that continues to cause 140～240 ℃ after the stretching carries out the thermal treatment in 1～60 second, finishes crystal orientation.
Easily adhesive linkage can arrange after the manufacturing of film or in the manufacturing process.Especially, from the aspect of throughput rate, preferably at any Duan Bands of thin film fabrication operation, namely do not stretch or uniaxial tension after the coating of the single face at least coating fluid of PET film, form easy adhesive linkage.
Can use known arbitrary method for the method for this coating fluid being coated the PET film.For example can list: reverse roll rubbing method, photogravure rubbing method, engagement rubbing method, mould coating machine method, roller brush method, spraying rubbing method, air knife rubbing method, the excellent rubbing method that winds the line, tubular type are scraped the skill in using a kitchen knife in cookery (Pipe Doctor, パ イ プ De Network タ ー) method, impregnation rubbing method, curtain formula rubbing method etc.These methods can separately or make up and apply.
The thickness of the easy adhesive linkage that finally obtains in the present invention, is preferably 0.03～0.20g/m 2Less than 0.03g/m 2The time, cementability reduces, and is thicker than 0.20g/m 2The time, adhesive, sliding reduce, so not preferred.
(Polarizer)
Polarizer of the present invention has polaroid protective film on the two sides of polaroid, and the polaroid protective film of the face of preferred at least one side is aforementioned polaroid protection easy-adhesion mylar.The polaroid protective film of opposite side can be that the easy-adhesion mylar is used in polaroid protection of the present invention, and using with cellulose triacetate film, acrylate film, norborene class film also is preferred as the film of the free of birefringence of representative.
As polaroid, for example can enumerate the polyvinyl alcohol film that contains dichroic material such as iodine.Polaroid protective film directly or by bond layer and polaroid is fitted, and from improving the aspect of cementability, preferably fits by bonding agent.At this moment, easy adhesive linkage preferred disposition of the present invention at polarization unilateral or bonding agent aspect.As the polaroid that is preferred for bonding mylar of the present invention, for example can enumerate the following polaroid that obtains: in polyvinyl alcohol film dyeing absorption iodine, dichroic material, in boric acid aqueous solution, carry out uniaxial tension, keep extended state to wash with drying and obtain.The stretching ratio of uniaxial tension is generally about 4～8 times.As the polyvinyl alcohol film, polyvinyl alcohol (PVA) suits, can utilize commercially available products such as " Kuraray Vinylon " [Kuraray Co., Ltd.'s manufacturing], " Tohcello Vinylon " [Mitsui Chemicals Tohcello, Inc. makes], " day is closed Vinylon " [Japanese synthetic chemistry Co., Ltd. make].As dichroic material, can list: iodine, bis-azo compound, polymethin dyes etc.
From the angle of attenuate bond layer, coat the material of the preferred water system of bonding agent of polaroid, that is, the bonding agent composition is dissolved in water or is scattered in water and the material that obtains.For example, can use polyvinyl alcohol resin, urethane resin etc. as principal ingredient, the composition of isocyanate ester compound, epoxy compound etc. that used compounding as required in order to improve cementability.The thickness of bond layer is preferably below the 10 μ m, more preferably below the 5 μ m, more preferably below the 3 μ m.
When using polyvinyl alcohol resin as the principal ingredient of bonding agent; except partly-hydrolysed polyvinyl alcohol (PVA), fully saponified polyvinyl alcohol (PVA), can also use carboxy-modified polyvinyl alcohol (PVA), acetoacetyl modified polyvinylalcohol, methylol modified polyvinylalcohol, this modification of amino modified polyvinyl alcohol (PVA) polyvinyl alcohol resin.The concentration of the polyvinyl alcohol resin in the bonding agent is preferably 1～10 quality %, more preferably 2～7 quality %.
Embodiment
Then, describe the present invention in detail with embodiment, comparative example and reference example, but the present invention is not limited to following embodiment certainly.In addition, the evaluation method of using among the present invention is as follows.
(1) glass transition temperature
According to JIS K7121, use differential scanning calorimeter (Seiko Instruments Inc. manufacturing, DSC6200), the 10mg resin sample is heated up in 25～300 ℃ temperature range with the speed of 20 ℃/min, will be changed the beginning temperature by the extrapolation glass that the DSC curve obtains as glass transition temperature.
(2) number-average molecular weight
The 0.03g resin is dissolved in the 10ml tetrahydrofuran, polystyrene), 30 ℃ of column temperatures use the manufacturing of GPC-LALLS device low angle light light scattering photometer LS-8000(TOSOH Co., Ltd, tetrahydrofuran solvent, reference:, flow 1ml/ minute, use chromatographic column (Showa Denko K. K makes shodex KF-802,804,806) to measure number-average molecular weight.
(3) resin is formed
Resin is dissolved in deuterochloroform, uses Varian, Inc. makes magnetic nuclear resonance analyzer (NMR) Gemini-200 and carries out 1H-NMR analyzes, and determines mole % ratio that each is formed by its integration ratio.
(4) acid number
With the 1g(solid constituent) sample be dissolved in chloroform or the dimethyl formamide of 30ml, carry out titration as indicator with the potassium hydroxide-ethanol solution of 0.1N with phenolphthalein, obtain the amount (mg) of the required KOH of the carboxyl of the every 1g sample of neutralization.
(5) saponification degree
Use NaOH that the remaining acetoxy group (mole %) of polyvinyl alcohol resin is carried out quantitatively according to JIS-K6726, it is worth as saponification degree (mole %).Same sample is carried out 3 times measures, with its mean value as saponification degree (mole %).
(6) the polaroid protection total light transmittance of mylar
Polaroid protection according to JIS K7105, uses nephelometer (Japanese electric look Co., Ltd. makes, NDH2000) to measure with the total light transmittance of mylar.
(7) the polaroid protection mist degree of mylar
The mist degree of polaroid protection mylar is according to JIS K7136, uses nephelometer (Japanese electric look Co., Ltd. makes, NDH2000) to measure.
(8) PVA cementability
Be adjusted to the polyvinyl alcohol water solution (Kuraray Co., Ltd. makes PVA117) of solid component concentration 5 quality % with the coating of coiling rod with the easy adhesive linkage surface of mylar in the polaroid protection; make that the thickness of dried polyvinyl alcohol resin layer is 2 μ m, with 70 ℃ of dryings 5 minutes.For the ease of judging, use the polyvinyl alcohol water solution that has added orchil.For the evaluation object film of making, on the glass plate of the thickness 5mm that posts double faced adhesive tape, the opposite face of the face with being formed with the polyvinyl alcohol resin layer of the laminate film of evaluation object is attached at above-mentioned double faced adhesive tape.Then, use the cutter guide formation of clearance gap 2mm to run through the otch that the polyvinyl alcohol resin layer arrives 100 lattice-shapeds of base film.Then, with adhesive strip (Nichiban Co., Ltd. makes the Cellotape(registered trademark) CT-24; 24mm is wide) be attached to the cut sides of lattice-shaped.When attaching, press with rubber after the residual air in interface makes its complete driving fit, will implement 1 time, 5 times, 10 times the operation that adhesive strip is vertically peeled off suddenly.Number goes out the number of the unstripped grid of polyvinyl alcohol resin layer, as the PVA cementability.That is, the PVA layer is complete when unstripped, and when the bonding rate note of PVA was made 100, PVA layer and all peeled off, the bonding rate note of PVA did 0.What in addition, part was peeled off in 1 grid is also included within the number of peeling off.
(polymerization of vibrin)
In the stainless steel autoclave that possesses stirring machine, thermometer and partial reflux formula refrigeratory, add 194.2 mass parts dimethyl terephthalate (DMT), 184.5 mass parts dimethyl isophthalate, 14.8 mass parts dimethyl-5-sulfoisophthalic acid sodium, 233.5 mass parts diethylene glycols, 136.6 mass parts ethylene glycol and 0.2 mass parts tetra-n-butyl titanate esters, with 160 ℃～220 ℃ temperature with carrying out ester exchange reaction in 4 hours.Then, be warming up to 255 ℃, after reaction system was slowly reduced pressure, reaction was 1 hour 30 minutes under the decompression of 30Pa, obtains copolymer polyester resin (A-1).Gained copolymer polyester resin (A-1) is faint yellow transparent.Measure the reduced viscosity of copolymer polyester resin (A-1), the result is 0.70dl/g.Glass transition temperature based on DSC is 40 ℃.
The copolymer polyester resin (A-2)～(A-5) that uses the same method and obtain other compositions.These copolymer polyester resins are used 1The composition that H-NMR records (mole % ratio) and other characteristics are shown in table 1.
[table 1]
Figure BDA00003613564700181
(preparation of polyester water dispersion)
Add 30 mass parts vibrin (A-1), 15 mass parts ethylene glycol n-butyl ethers in the reactor that stirring machine, thermometer and reflux are housed, with 110 ℃ of heating, stirring with resin dissolves.After resin dissolves fully, while stirring 55 mass parts water are slowly added in the polyester liquid.After the interpolation, liquid is cooled to room temperature while stirring, makes the milky polyester water dispersion (Aw-1) of solid constituent 30 quality %.Similarly use vibrin (A-2)～(A-5) to replace vibrin (A-1) to make aqueous dispersion, respectively as polyester water dispersion (Aw-2)～(Aw-5).
(preparation of polyvinyl alcohol water solution)
In the container that stirring machine and thermometer are housed, add 90 mass parts water, slowly add the polyvinyl alcohol resin (Kuraray Co., Ltd.'s manufacturing) of the 10 mass parts degree of polymerization 500 while stirring (B-1).After the interpolation, liquid is heated to 95 ℃ while stirring, makes resin dissolves.After the dissolving, be cooled to room temperature while stirring, make the polyvinyl alcohol water solution (Bw-1) of solid constituent 10 quality %.Similarly use polyvinyl alcohol resin (B-2)～(B-7) to replace polyvinyl alcohol resin (B-1) to make aqueous solution, respectively as (Bw-2)～(Bw-7).The saponification degree of polyvinyl alcohol resin (B-1)～(B-7) is shown in table 2.
[table 2]
? B-1 B-2 B-3 B-4 B-5 B-6 B-7
Saponification degree (mole %) 88 83 79 74 70 67 40
(polymerization of blocked polyisocyanates crosslinking chemical)
In the flask that stirring machine, thermometer, reflux condenser are housed, add the polyisocyanate compound with isocyanurate structure that 100 mass parts are raw material with the hexamethylene diisocyanate (Asahi Chemical Corp's manufacturing, DURANATE TPA), 55 mass parts propylene glycol monomethyl ether acetate, 30 mass parts poly glycol monomethyl ethers (mean molecular weight 750), under blanket of nitrogen, kept 4 hours with 70 ℃.Then, reacting liquid temperature is cooled to 50 ℃, drips 47 mass parts methyl ethyl ketoximes.The infrared spectrum of assaying reaction liquid, the absorption that confirms isocyanate group disappears, and obtains the blocked polyisocyanates aqueous dispersions (C-1) of solid constituent 75 quality %.
Embodiment 1
(1) preparation of coating fluid
Mix following smears, the mass ratio of making polyester resin (A)/polyvinyl alcohol resin (B) is 70/30 coating fluid.Polyester water dispersion uses and is dispersed with acid number and is the aqueous dispersion (Aw-1) of the vibrin of 2KOHmg/g, and polyvinyl alcohol water solution uses and is dissolved with the aqueous solution that saponification degree is the polyvinyl alcohol (PVA) of 74 moles of % (Bw-4).
Water 40.61 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 11.67 quality %
Polyvinyl alcohol water solution (Bw-4) 15.00 quality %
Blocked isocyanate class crosslinking chemical (C-1) 0.67 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Catalyzer
(organic tin compound solid constituent concentration 14 quality %) 0.3 quality %
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
(2) the polaroid protection manufacturing of mylar
As the film raw material polymkeric substance, with limiting viscosity (solvent: phenol/tetrachloroethane=60/40) for 0.62dl/g and the PET resin granular material that do not contain particle in fact under the decompression of 133Pa, with 135 ℃ of dryings 6 hours.Then, supply with extruder, melt extrude slabbing with about 280 ℃, solidify remaining on the rotation cool metal roller of 20 ℃ of surface temperatures the chilling driving fit, the PET sheet is not stretched.
With warmed-up roller group and infrared heater this PET sheet that do not stretch is heated to 100 ℃, longitudinally is stretched to 3.5 times with the roller group with difference then, obtain uniaxial tension PET film.
Then, aforementioned coating fluid is coated on after the single face of PET film with the roller rubbing method, with 80 ℃ of 15 seconds of drying.In addition, adjust so that the dried coating weight of final (biaxial stretch-formed back) is 0.12g/m 2Then be stretched to 4.0 times with stenter with 150 ℃ of broad ways; under the state of the length of the Width of having fixed film; with 230 ℃ of 0.5 seconds of heating, further with 230 ℃ of relaxation processes of carrying out the Width in 10 seconds 3%, obtain the polaroid protection mylar of thickness 38 μ m.Evaluation result is shown in table 3.
Embodiment 2
Polyester water dispersion changed to be dispersed with the aqueous dispersion that acid number is the vibrin of 4KOHmg/g (Aw-2), in addition obtain polaroid protection mylar similarly to Example 1.
Embodiment 3
Polyester water dispersion changed to be dispersed with the aqueous dispersion that acid number is the vibrin of 6KOHmg/g (Aw-3), in addition obtain polaroid protection mylar similarly to Example 1.
Embodiment 4
The saponification degree that polyvinyl alcohol water solution is changed to polyvinyl alcohol (PVA) is the polyvinyl alcohol water solution (Bw-3) of 79 moles of %, in addition obtains polaroid protection mylar similarly to Example 1.
Embodiment 5
The saponification degree that changes to polyvinyl alcohol (PVA) is the polyvinyl alcohol water solution (Bw-2) of 83 moles of %, in addition obtains polaroid protection mylar similarly to Example 1.
Embodiment 6
Change to the following smears of mixing and make that the mass ratio of polyester resin (A)/polyvinyl alcohol resin (B) is 60/40, in addition obtain polaroid protection mylar similarly to Example 1.
Water 37.28 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 10.00 quality %
Polyvinyl alcohol water solution (Bw-4) 20.00 quality %
Blocked isocyanate class crosslinking chemical (C-1) 0.67 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Catalyzer
(organic tin compound solid constituent concentration 14 quality %) 0.3 quality %
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Embodiment 7
Change to the following smears of mixing and make that the mass ratio of polyester resin (A)/polyvinyl alcohol resin (B) is 80/20, in addition obtain polaroid protection mylar similarly to Example 1.
Water 43.95 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 13.33 quality %
Polyvinyl alcohol water solution (Bw-4) 10.00 quality %
Blocked isocyanate class crosslinking chemical (C-1) 0.67 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Catalyzer
(organic tin compound solid constituent concentration 14 quality %) 0.3 quality %
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Embodiment 8
Change to the following smears of mixing and make that the mass ratio of polyester resin (A)/polyvinyl alcohol resin (B) is 50/50, in addition obtain polaroid protection mylar similarly to Example 1.
Water 33.95 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 8.33 quality %
Polyvinyl alcohol water solution (Bw-4) 25.00 quality %
Blocked isocyanate class crosslinking chemical (C-1) 0.67 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Catalyzer
(organic tin compound solid constituent concentration 14 quality %) 0.3 quality %
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Embodiment 9
The composition change of coating fluid is as follows, in addition obtain polaroid protection mylar similarly to Example 1.
Water 40.87 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 1.67 quality %
Polyvinyl alcohol water solution (Bw-4) 15.00 quality %
Melamine class crosslinking chemical (C-2) 0.71 quality %
(NIKALAC MX-042 SANWA Chemical Co., Ltd. makes solid component concentration 70%)
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Embodiment 10
Polyvinyl alcohol water solution is changed to the aqueous solution (Bw-5) that the saponification degree that is dissolved with polyvinyl alcohol (PVA) is the polyvinyl alcohol (PVA) of 70 moles of %, in addition obtain polaroid protection mylar similarly to Example 1.
Embodiment 11
Polyvinyl alcohol water solution is changed to the aqueous solution (Bw-6) that the saponification degree that is dissolved with polyvinyl alcohol (PVA) is the polyvinyl alcohol (PVA) of 67 moles of %, in addition obtain polaroid protection mylar similarly to Example 1.
Embodiment 12
The composition change of coating fluid is as follows, in addition obtain polaroid protection mylar similarly to Example 1.
Water 40.33 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 11.67 quality %
Polyvinyl alcohol water solution (Bw-2) 15.00 quality %
Oxazoline class crosslinking chemical (C-3) 1.25 quality %
(EPOCROS WS-500, Nippon Shokubai Co., Ltd's manufacturing, solid component concentration 40 quality %)
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Embodiment 13
Polyester water dispersion changed to be dispersed with the aqueous dispersion that acid number is the vibrin of 10KOHmg/g (Aw-5), in addition obtain polaroid protection mylar similarly to Example 1.
Comparative example 1
Change to the following smears of mixing and make that the mass ratio of polyester resin (A)/polyvinyl alcohol resin (B) is 100/0, in addition obtain polaroid protection mylar similarly to Example 1.
Water 50.62 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 16.66 quality %
Blocked isocyanate class crosslinking chemical (C-1) 0.67 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Catalyzer
(organic tin compound solid constituent concentration 14 quality %) 0.3 quality %
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Comparative example 2
Change to the following smears of mixing and make that the mass ratio of polyester resin (A)/polyvinyl alcohol resin (B) is 0/100, in addition obtain polaroid protection mylar similarly to Example 1.
Water 17.28 quality %
Isopropyl alcohol 30.00 quality %
Polyvinyl alcohol water solution (Bw-4) 50.00 quality %
Blocked isocyanate class crosslinking chemical (C-1) 0.67 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Catalyzer
(organic tin compound solid constituent concentration 14 quality %) 0.3 quality %
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Comparative example 3
Polyester water dispersion changed to be dispersed with the aqueous dispersion that acid number is the vibrin of 25KOHmg/g (Aw-4), in addition obtain polaroid protection mylar similarly to Example 1.
Comparative example 4
Polyvinyl alcohol water solution changed to be dissolved with the aqueous solution that saponification degree is the polyvinyl alcohol (PVA) of 88 moles of % (Bw-1), in addition obtain polaroid protection mylar similarly to Example 1.
Comparative example 5
Polyvinyl alcohol water solution changed to be dissolved with the aqueous solution that saponification degree is the polyvinyl alcohol (PVA) of 40 moles of % (Bw-7), in addition obtain polaroid protection mylar similarly to Example 1.
Comparative example 6
Change to and mix following smears, mixed cross-linker not, in addition obtain polaroid protection mylar similarly to Example 1.
Water 41.58 quality %
Isopropyl alcohol 30.00 quality %
Polyester water dispersion (Aw-1) 11.67 quality %
Polyvinyl alcohol water solution (Bw-4) 15.00 quality %
Particle 1.25 quality %
(silicon dioxide gel of mean grain size 100nm, solid component concentration 40 quality %)
Surfactant 0.5 quality %
(silicon class, solid component concentration 10 quality %)
Reference example 1
Illustrate and use TAC film (Fuji Photo Film Co., Ltd.'s manufacturing, thickness 80 μ m, saponification processing) to carry out the result of aforementioned adhesive test with film as the polaroid protection.
[table 3]
Figure BDA00003613564700271
Utilizability on the industry
Polaroid of the present invention protection has high adhesiveness with polaroid and water system bonding agent with the easy-adhesion mylar.Therefore, can be aptly as polaroid protection member.

Claims (5)

1. a polaroid protection is used the easy-adhesion mylar, and it is the mylar that has easy adhesive linkage at least at single face,
Described easy adhesive linkage contains polyester resin (A), polyvinyl alcohol resin (B) and crosslinking chemical (C),
The acid number of described polyester resin (A) is below the 20KOHmg/g,
The saponification degree of described polyvinyl alcohol resin (B) is 60～85 moles of %.
2. the easy-adhesion mylar is used in polaroid protection according to claim 1, and wherein, described vibrin (A) contains the 5-sulfoisophthalic acid composition of 1～15 mole of % that accounts for the dicarboxylic acid composition.
3. the easy-adhesion mylar is used in polaroid protection according to claim 1 and 2, and wherein, described crosslinking chemical (C) is isocyanate compound or melamine compound.
4. use the easy-adhesion mylar according to each described polaroid protection in the claim 1～3, wherein, in the described easy adhesive linkage, the mass ratio of polyester resin (A), polyvinyl alcohol resin (B) and crosslinking chemical (C) satisfies following formula:
0.8≤（A）/（B）≤5
2≤（（A）+（B））/（C）≤50。
5. Polarizer, its two sides at polaroid has polaroid protective film,
The polaroid protective film of the face of at least one side is each described polaroid protection easy-adhesion mylar in the claim 1～4.
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