CN1651540A - Adhesive composition, adhesive layer and adhesive sheet for optical element and optical element - Google Patents
Adhesive composition, adhesive layer and adhesive sheet for optical element and optical element Download PDFInfo
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- CN1651540A CN1651540A CNA2005100062066A CN200510006206A CN1651540A CN 1651540 A CN1651540 A CN 1651540A CN A2005100062066 A CNA2005100062066 A CN A2005100062066A CN 200510006206 A CN200510006206 A CN 200510006206A CN 1651540 A CN1651540 A CN 1651540A
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- optical elements
- acrylic acid
- acid polymer
- polymer emulsion
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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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
-
- 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
Abstract
To prepare an adhesive layer for an optical member, which prevents floating and peeling by change of a temperature and humidity environment, has excellent durability of heat resistance and moisture resistance and is readily releasable even in preservation after long-time passage and in a high-temperature and high-humidity environment after adhesion of an optical part, to prepare an adhesive sheet for an optical member, which is equipped with the adhesive layer for an optical member, to obtain an adhesive composition for an optical member, which is used for obtaining the adhesive layer for an optical member, and to provide an optical member having an optical part arranged on the adhesive layer for an optical member.The adhesive composition for an optical member comprises an acrylic polymer emulsion obtained by subjecting an emulsion composed of a monomer mixture having >=80 wt.% of a (meth) acrylic acid ester, a reactive emulsifying agent and a polymerization initiator to emulsion polymerization and 0.01-1 pt.wt., based on 100 pts.wt. of the solid content of the acrylic polymer emulsion, of a silane coupling agent, and the adhesive composition is applied to a substrate and dried to give the adhesive layer for the optical member.
Description
Technical field
The present invention relates to used for optical elements binding compositions, used for optical elements bonding coat, used for optical elements adhesive sheet and optical element, the optics that more specifically relates to the optical elements such as polaroid, polarizer, ellipsoidal polarizing plate that are used to fit also relates to the optical element that this used for optical elements bonding coat is arranged at optical element with binding compositions, used for optical elements bonding coat and used for optical elements adhesive sheet.
Background technology
Be used for the optical element of liquid crystal indicators such as panel display screen, for example, polaroid and polarizer etc. are fitted in liquid crystal cell with tackiness agent.The tackiness agent that is used for this purposes stretches because of the variation of humiture environment usually, follows this phenomenon optical element easily to float and peel off from liquid crystal cell, so the weather resistance requirement to some extent to tackling above-mentioned situation.
In addition, when fitting, there is foreign matter to be mingled with or occurs under the situation of position skew, optical element can be peeled off from liquid crystal cell, liquid crystal cell is utilized again, but require tackiness agent the gap of liquid crystal cell to be changed to some extent, can not make its fracture, easily peel off at the above-mentioned Shi Buhui of peeling off.Therefore, except requiring its bonding force and weather resistance improve, the releasable when also requiring to peel off is improved to the tackiness agent that is used for this purposes.
In addition, optical element can change to some extent because of the varying dimensions of humiture environment, therefore can produce internal stress thus, require tackiness agent can make that this internal stress homogeneous relaxes, noresidue stress is remaining on optical element, prevents the color spot and the blank spot that produce because of this residual stress.
In the past, the organic solvent type acrylic adhesive was used to such use.But, owing to can forming gas, distributes this organic solvent type acrylic adhesive organic solvent when being coated with, so be unfavorable for environment, therefore, attempt in recent years using the water soluble acrylic acid tackiness agent to substitute.
For example, having proposed with (methyl) alkyl acrylate is that to be the aqueous dispersion type tackiness agent that forms of water dispersion that monomer obtains by letex polymerization be set at the adhesive sheet of one side at least on the supporting mass as binder layer for the monomer mixture of principal constituent and silane, it is that the silane that monomer mixture corresponding to 100 weight parts contains 0.005～1 weight part is monomer, after fitting in the sheet glass clung body, bonding force after preserving 7 days under the condition of 70 ℃ and 20%RH is the sheet glass adhesive sheet more than 1.3 times of initial value, adopt optical thin film as supporting mass, the glass substrate that makes liquid crystal display is fitted with adhesive optical film (for example, opening the 2002-309212 communique with reference to the Japanese Patent spy).
But,, also be difficult to fully satisfy above-mentioned all rerum naturas such as desired weather resistance and releasable in this purposes even the Japanese Patent spy opens the sheet glass adhesive sheet of putting down in writing in the 2002-309212 communique.
Summary of the invention
The purpose of this invention is to provide and have the necessary rerum natura of the optical element of fitting in, promptly, what can prevent that variation because of the humiture environment from causing floats and peels off, the weather resistance of thermotolerance and wet fastness etc. is good, even fit in behind the optical element through for a long time or preserve the used for optical elements bonding coat that also can easily peel off in hot and humid atmosphere; The used for optical elements adhesive sheet that possesses this used for optical elements bonding coat; Be used to obtain the used for optical elements binding compositions of this used for optical elements bonding coat, and this used for optical elements bonding coat be arranged at optical element and the optical element that forms.
The feature of used for optical elements binding compositions of the present invention is, comprise acrylic acid polymer emulsion and divide 100 weight parts, be the silane coupling agent of 0.01～1 weight part that with respect to the solid formation of aforementioned acrylic acid polymer emulsion described acrylic acid polymer emulsion carries out letex polymerization by the emulsion that makes the monomer mixture, the reactive emulsifier that contains free-radical polymerised functional group and the polymerization starter that comprise (methyl) acrylate that contains more than the 80 weight % and obtains.
The invention still further relates to the used for optical elements bonding coat that forms by above-mentioned used for optical elements binding compositions.
The invention still further relates to the used for optical elements adhesive sheet that possesses above-mentioned used for optical elements bonding coat.
Above-mentioned used for optical elements adhesive sheet fits in glass, 60 ℃ through after 17 hours to the bonding force of aforementioned glass below 10N/25mm.
The invention still further relates to the optical element that above-mentioned used for optical elements bonding coat is arranged at the single face of optical element or two sides and forms.
Above-mentioned optical element is preferably any in polaroid, polarizer and the ellipsoidal polarizing plate.
Even used for optical elements bonding coat of the present invention that is formed by used for optical elements binding compositions of the present invention and used for optical elements adhesive sheet of the present invention also can prevent to float and peel off under hot and humid environment.In addition, behind the applying optical element, even, also peel off easily thereafter through long period or be stored in the hot and humid atmosphere.Therefore, the optical element that is provided with used for optical elements bonding coat of the present invention for example can be suitable as the optical element that is used for liquid crystal indicator and uses.
Description of drawings
Fig. 1 is the sectional view of one of embodiment of analog representation used for optical elements bonding coat of the present invention and used for optical elements adhesive sheet of the present invention.
Fig. 2 is the sectional view of one of embodiment of analog representation optical element of the present invention.
Embodiment
Used for optical elements binding compositions of the present invention contains acrylic acid polymer emulsion and silane coupling agent.
Acrylic acid polymer emulsion can be by comprising monomer mixture, reactive emulsifier and polymerization starter the letex polymerization of emulsion obtain.
Among the present invention, monomer mixture contains above (methyl) acrylate of 80 weight %.
(methyl) acrylate is meant methacrylic ester and/or acrylate, can exemplify the compound of following general formula (1) expression.
CH
2＝CR1COOR2???????(1)
In the formula, R1 is hydrogen or methyl, and R2 is the alkyl of the straight or branched of carbonatoms 1～18.
But R2 exemplified by methyl, ethyl, propyl group, sec.-propyl, butyl, isobutyl-, sec-butyl, the tertiary butyl, amyl group, neo-pentyl, isopentyl, hexyl, heptyl, octyl group, iso-octyl, 2-ethylhexyl, different nonyl, decyl, isodecyl, lauryl, bornyl, isobornyl, tetradecyl, pentadecyl, octadecyl etc.
More specifically can exemplify (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) propyl acrylate, (methyl) isopropyl acrylate, (methyl) butyl acrylate, (methyl) isobutyl acrylate, (methyl) sec-butyl acrylate, (methyl) tert-butyl acrylate, (methyl) vinylformic acid pentyl ester, (methyl) vinylformic acid peopentyl ester, (methyl) Ethyl acrylate, (methyl) vinylformic acid heptyl ester, (methyl) Octyl acrylate, (methyl) Isooctyl acrylate monomer, (methyl) 2-EHA, (methyl) vinylformic acid ester in the ninth of the ten Heavenly Stems, (methyl) vinylformic acid ester in the different ninth of the ten Heavenly Stems, (methyl) decyl acrylate, (methyl) isodecyl acrylate, (methyl) lauryl acrylate, (methyl) vinylformic acid norbornene ester, (methyl) isobornyl acrylate, (methyl) vinylformic acid tetradecyl ester, (methyl) vinylformic acid pentadecyl ester, (methyl) vinylformic acid stearyl.
These (methyl) acrylate can suitably use separately or and use.In addition, the content of these (methyl) acrylate more than 80 weight %, is preferably 85～99.5 weight % corresponding to monomer mixture.(methyl) is if the content of acrylate less than 80 weight %, then can become excessive to the bonding force of glass sometimes.
In the monomer mixture except (methyl) acrylate, also can contain can with the monomer of (methyl) acrylic ester copolymer.
It is monomer etc. that but the monomer of this copolymerization can exemplify the silane that contains the monomer, contains Siliciumatom that contains functional group.
The monomer that contains functional group for example has vinylformic acid; methacrylic acid; methylene-succinic acid; toxilic acid; Ba Dousuan; carboxylic monomer such as maleic anhydride or its acid anhydrides; for example; (methyl) 2-Hydroxy ethyl acrylate; (methyl) vinylformic acid-2-hydroxy propyl ester; the monomer of (methyl) vinylformic acid-hydroxyls such as 2-hydroxyl butyl ester; for example; (methyl) acrylamide; N; N-dimethyl (methyl) acrylamide; N-methylol (methyl) acrylamide; N-methoxymethyl (methyl) acrylamide; the monomer of amide-containings such as N-butoxymethyl (methyl) acrylic acid amides; for example; (methyl) vinylformic acid dimethylamino ethyl ester; (methyl) vinylformic acid tertiary butyl amino ethyl ester etc. contains amino monomer; for example; (methyl) glycidyl acrylate etc. contains the monomer of glycidyl, and other is as (methyl) vinyl cyanide; N-(methyl) acryloyl morpholine; N-vinyl-2-Pyrrolidone etc.
These monomers that contain functional group can suitably use separately or and use.These monomeric content that contain functional group less than 20 weight %, are preferably 0.47～14.9 weight % corresponding to monomer mixture.
In addition, silane is that can to exemplify the silane that good (methyl) acryloxyalkyl silane derivative of copolymerization with (methyl) acrylate etc. has (methyl) acryl be monomer to monomer.This silane is that monomer for example is the 3-methacryloxypropyl trimethoxy silane, 3-acryloxy propyl trimethoxy silicane, 3-methacryloxy triethoxyl silane, 3-acryloxy propyl-triethoxysilicane, 3-methacryloxypropyl methyl dimethoxysilane, 3-acryloxy propyl group methyl dimethoxysilane, 3-methacryloxypropyl methyldiethoxysilane, vinyltrimethoxy silane, vinyltriethoxysilane, 4-vinyl butyl Trimethoxy silane, 4-vinyl butyl triethoxyl silane, 8-vinyl octyl group Trimethoxy silane, 8-vinyl octyltri-ethoxysilane, 10-methacryloxy decyl Trimethoxy silane, 10-acryloxy decyl Trimethoxy silane, 10-methacryloxy decyl triethoxyl silane, 10-acryloxy decyl triethoxyl silane etc.
These silane are that monomer can use separately or and use.These silane are that monomeric content for example is 0.005～1 weight % corresponding to monomer mixture, are preferably 0.01～0.5 weight %, more preferably 0.03～0.1 weight %.If less than 0.005 weight %, polymer strength deficiency sometimes then, cohesive force descends.In addition, if surpass 0.1 weight %, then sometimes bonding force drop to can't the adherent degree.
Among the present invention, at first with above-mentioned (methyl) acrylate and can be mixed with monomer mixture with the monomer of (methyl) acrylic ester copolymer, add simultaneously reactive emulsifier and water therein, emulsification forms emulsion, in this emulsion, add polymerization starter then and add water as required, carry out letex polymerization.
Reactive emulsifier for example for having imported the emulsifying agent of free-radical polymerised functional groups such as propenyl, allyl ether, more specifically can exemplify ア Network ア ロ Application HS-10, HS-20, KH-10, BC-05, BC-10, BC-20 (Di-ichi Kogyo Seiyaku Co., Ltd.'s system), for example ア デ カ リ ア ソ-プ SE10N (Asahi Denka Kogyo K. K's system) etc.
By using this class reactive emulsifier, can improve thermotolerance and wet fastness.
These reactive emulsifiers can use separately or and use.The proportioning of these reactive emulsifiers for example is 0.2～10 weight part corresponding to the monomer mixture (the solid formation that is equivalent to acrylic acid polymer emulsion described later divides 100 weight parts, down together) of 100 weight parts, is preferably 0.5～5 weight part.
For example, above-mentioned (methyl) acrylate and the monomer mixture that can form with the monomer of (methyl) acrylic ester copolymer are added in the entry, in water, behind the interpolation reactive emulsifier, can modulate emulsion simultaneously by mixing.
Then, also adding water as required carries out letex polymerization to add polymerization starter in this emulsion.
Polymerization starter can be the known radical polymerization initiator that is commonly used for the polymerization starter of letex polymerization, for example, 2,2 '-Diisopropyl azodicarboxylate, 2,2 '-azo two (2-methyl-prop amidine) dithionate, 2,2 '-azo two (2-amidine propane) dihydrochloride, 2,2 '-azo two [2-(5-methyl-2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride, 2,2 '-azo, two (N, N '-dimethylene isobutyl amidine), 2, azo series initiators such as 2 '-azo two [N-(2-carboxy ethyl)-2-methyl-prop amidine] hydrate, for example, Sodium Persulfate, persulphate series initiators such as ammonium persulphate, for example, benzoyl peroxide, t-butyl hydroperoxide, superoxide series initiators such as hydrogen peroxide, for example, phenyl replaces replacement ethane series initiators such as ethane, for example, carbonyl series initiators such as aromatic carbonyl, for example, the combination of persulphate and sodium bisulfite, redox series initiators such as the combination of superoxide and sodium ascorbate etc.
These polymerization starters can use separately or and use.The proportioning of these polymerization starters for example is about 0.005～1 weight part corresponding to the monomer mixture of 100 weight parts.
Water can only mix when the modulation of emulsion, perhaps also can mix once more thereafter, can suitably select according to polymerization process described later.
Proportioning to water is not particularly limited, as long as the solid formation branch concentration of the acrylic acid polymer after the letex polymerization is adjusted into 30～75 weight %, is more preferably and is adjusted into 35～70 weight %.
Can suitably mix additives such as chain-transfer agent and linking agent as required in this emulsion.
Chain-transfer agent is not particularly limited, and for example is 1-dodecyl mercaptans, Thiovanic acid, 2 mercapto ethanol, 2-ethylhexyl mercaptoacetate, 2,3-dimercapto-thio-alcohols such as 1-propyl alcohol etc.
These chain-transfer agents can suitably use separately or and use.The proportioning of chain-transfer agent for example is about 0.001～0.5 weight part corresponding to the monomer mixture of 100 weight parts.
Linking agent is not particularly limited, can exemplifies the isocyanate-based linking agent, epoxy is that linking agent, oxazoline are that linking agent, ethylenimine are linking agent, metal-chelating system linking agent etc.Above-mentioned silane is that monomer also can be used as the linking agent use.
These linking agents can use separately or and use.The proportioning of linking agent for example is about 0.01～5 weight part corresponding to the monomer mixture of 100 weight parts.
Other additive for example has pH buffer reagent, neutralizing agent, anti-whipping agent, stablizer etc. to be commonly used for the known additive of the additive of letex polymerization.
Method of emulsion polymerization is not particularly limited, can from concentrate polymerization, full dose dripping method and two sections polymerizations that both combine etc., suitably selects.
For example, concentrate in the polymerization, in reaction vessel, add monomer mixture, reactive emulsifier and water, by mix make their emulsification modulate emulsion after, in this reaction vessel, add polymerization starter again and add water as required, carry out letex polymerization.
In addition, for example in the full dose dripping method, at first add monomer mixture, reactive emulsifier and water, make their emulsification modulate dropping liquid by mixing, and in reaction vessel, add polymerization starter and water, and in reaction vessel, splash into dropping liquid then, carry out letex polymerization.
Utilize the above-mentioned emulsion polymerization, monomer mixture generation polymerization, the synthesizing propylene acid polymer can obtain this acrylic acid polymer emulsive acrylic acid polymer emulsion in water.
Then, by in the acrylic acid polymer emulsion of gained, mixing silane coupling agent, modulate used for optical elements binding compositions of the present invention.
Can exemplify as silane coupling agent, for example, the 3-glycidoxypropyltrime,hoxysilane, 3-glycidoxy propyl group methyldiethoxysilane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane etc. contains the silane coupling agent of epoxy group(ing), for example, the 3-TSL 8330, N-2-(amino-ethyl)-3-aminopropyl methyl dimethoxysilane, 3-triethoxysilyl-N-(1,3-dimethyl-butylidene) propylamine etc. contains amino silane coupling agent, for example, 3-propenyloxy group propyl trimethoxy silicane, 3-metacryloxy propyl-triethoxysilicane etc. contains the silane coupling agent of (methyl) propenyl, for example, 3-isocyanic ester propyl-triethoxysilicane etc. contains silane coupling agent of isocyanate group etc.
By using these silane coupling agents, can improve weather resistance.
These silane coupling agents can use separately or and use.The proportioning of silane coupling agent promptly, corresponding to the solid formation branch of 100 parts by weight of acrylic based polymer emulsion, is 0.01～1 weight part corresponding to the monomer mixture of 100 weight parts, is preferably 0.03～0.5 weight part.If less than 0.01 weight part, then can not improve weather resistance, if surpass 1 weight part, then can not improve releasable.
As required, can further in used for optical elements binding compositions of the present invention, mix for example known additives such as UV light absorber, protective agent, tenderizer, dyestuff, pigment, weighting agent.
The weather resistance of the thermotolerance of the used for optical elements binding compositions of the present invention of above gained and wet fastness etc. is good, even and through long period or in hot and humid atmosphere, preserve, also can easily peel off, show good releasable, so be suitable as the used for optical elements bonding coat use that applying is used for the optical element of liquid crystal indicator.
Promptly, for example after on the base material of lift-off processing, carry out drying by used for optical elements binding compositions of the present invention being coated its surface, can form used for optical elements adhesive sheet with used for optical elements bonding coat of the present invention, it is replicated in optical element, can makes optical element of the present invention.
Base material is not particularly limited, for example, plastics film classes such as polypropylene film, ethylene-propylene copolymer film, polyester film, polyvinyl chloride, for example, stationeries such as kraft paper, for example, dry goods such as cotton, spun rayon cloth, for example, nonwoven dry goods such as polyester non-woven fabric, latitude nylon non-woven fabrics, for example, tinsel etc.
The thickness of base material can be done suitably to select according to its purpose and purposes etc., for example, and about 20～100 μ m.
Lift-off processing to substrate surface is not particularly limited, and for example can adopt silicon lift-off processing, chain alkyl lift-off processing, fluorine lift-off processing etc.
When coating used for optical elements binding compositions of the present invention on the base material, for example can adopt intaglio plate roller painting, two-sided roller painting, suitable roller painting, dipping roller painting, the rod of pressing to be coated with the coating method that method, scraper coating method, spraying method, curtain coating method, mould Tu Fa etc. are usually used in the lamination of binder layer.
In the above-mentioned coating, for example be 2～500 μ m according to the dried thickness that makes the used for optical elements binding compositions, the requirement that is preferably 5～100 μ m is coated with.
Thereafter drying can be undertaken by known method, for example in 50～200 ℃, better is to heat under the temperature about 80～160 ℃.
More than the gel component of the used for optical elements bonding coat of Huo Deing (being insoluble to the composition of solvent) is 30～95 weight %, is preferably 35～90 weight %.If less than 30 weight %, then too high to the bonding force of glass, under hot and humid, can foam sometimes, if surpass 95 weight %, then can float under hot and humid sometimes or occur peeling off.
As shown in Figure 1, can obtain the stacked used for optical elements adhesive sheet 3 of used for optical elements bonding coat 2 on base material 1 like this.
The used for optical elements bonding coat is replicated in optical element, can makes optical element by the base material of this used for optical elements adhesive sheet.
Optical element is not particularly limited, can exemplifies the polarization film (polaroid), phase-contrast film (polarizer), the elliptical polarization film optical thin films such as (ellipsoidal polarizing plates) that are used for liquid crystal indicator etc.
The polarizer that constitutes polarization film is not particularly limited, can uses various polarizers.Can exemplify as polarizer, for example, the polyvinyl alcohol film, the ethylene vinyl acetate copolymer pastern that make dichroic substance such as iodine or dichroic dye be adsorbed in polyvinyl alcohol film, part methylalization divide hydrophilic macromolecule films such as saponification film, stretch then and the oriented film that forms; Or further with the stacked film that forms in this oriented film of protective membranes such as tri acetyl cellulose film, polycarbonate film; Or on oriented film or protective membrane, formed the film of micro concavo-convex; Carried out the film of vapor deposition treatment; The film of stacked protection bonding film; Carried out various surface-treated films etc.In addition, can exemplify the processed thing of polyvinyl alcohol or the polyenoid such as desalination acid treatment thing of polyvinyl chloride is oriented film etc.Thickness to polarizer is not particularly limited, and is generally about 5～80 μ m.
In addition, be purpose with water tolerance etc., the coating layer that can polymkeric substance be set on the single face or the two sides of polarizer or the laminate layers of film etc. are as protective clear layer.The transparent polymer or the thin-film material that form protective clear layer can adopt suitable transparent material, but preferably adopt well behaved materials such as transparency, physical strength, thermostability and water preventing ability.Thickness to protective clear layer is not particularly limited, and is generally about 10～300 μ m.
Material as this protective clear layer; for example; polyester such as polyethylene terephthalate, PEN based polymer, for example, cellulose-based polymkeric substance such as secondary cellulose acetate, cellulose triacetate; for example; acrylic acid polymer such as polymethylmethacrylate, for example, polystyrene, acrylonitrile styrene copolymer styrenics such as (AS resins); for example, polycarbonate based polymer etc.In addition, for example can exemplify, polyethylene, polypropylene, ring system and polyolefine with norbornylene structure, polyolefin polymkeric substance such as ethylene propylene copolymer, vinyl chloride-based polymer, acid amides such as nylon and aromatic polyamide based polymer, the imide series polymkeric substance, sulfone based polymer, polyethersulfone based polymer, the polyether-ether-ketone based polymer, the poly-p-phenylene sulfide based polymer, vinyl alcohol system polymer, vinylidene chloride based polymer, the polyvinyl butyral acetal based polymer, the allylate based polymer, the polyoxymethylene based polymer, the polymer blend of epoxy based polymer or above-mentioned polymkeric substance etc.
As phase-contrast film, can exemplify the polymer starting material are carried out that uniaxial extension is handled or biaxial stretch-formed processing and the birefringent film that obtains or liquid crystal polymer film etc.Thickness to phase-contrast film is not particularly limited, and is generally about 20～150 μ m.Phase-contrast film can form the duplexer of two-layer above oriented film etc., also can form the film that optical characteristics such as phase differential is under control.
The polymer starting material can exemplify polyvinyl alcohol, polyvinyl butyral acetal, poly-ethylene methacrylic ether, Poly(Hydroxyethyl Methacrylate), Natvosol, hydroxypropylcellulose, methylcellulose gum, polycarbonate, polymethylmethacrylate, polyolefine, the polyene propyl ester, polysulfones, polyethylene terephthalate, PEN, polyethersulfone, poly-p-phenylene sulfide, polyphenylene oxide, polyene propyl group sulfone, polyvinyl alcohol, polymeric amide, polyimide, polyolefine, polyvinyl chloride, cellulose-based polymkeric substance or their two component system, the three component system multipolymer, graft copolymer, polymer blend etc.These polymer starting material wait by stretching and form directed thing (oriented film).
Liquid-crystalline polymer can exemplify various backbone chain types or the side chain type liquid crystal polymkeric substance that the conjugacy straight chain shape atomic group (mesomorphic unit, メ ソ グ Application) of giving liquid crystal aligning has been imported into main polymer chain or side chain.
It is liquid-crystalline polymer etc. in conjunction with for example nematic directional property polyester of the structure of mesomorphic unit that the object lesson of backbone chain type liquid crystal polymkeric substance has giving flexual interval base portion.
The object lesson of side chain type liquid crystal polymkeric substance has with polysiloxane, polyacrylic ester, polymethacrylate or poly-malonic ester and is main chain backbone, has a polymkeric substance that interval base portion that the conjugacy atomic group forms is connected to the mesomorphic unit that the ring compound unit by nematic directional property para-orientation on the main chain forms that passes through as side chain.These liquid-crystalline polymers, for example can obtain by following form, that is, carrying out the film of friction treatment or carried out sprawling on the directional process face of film etc. of silicon oxide inclination evaporation liquid-crystalline polymer solution, heat-treat and the material that obtains then being formed at film surfaces such as polyimide on the sheet glass or polyvinyl alcohol.
As the elliptical polarization film, with the expansion that prevents painted and angular field of view etc. the compensation etc. of the purpose phase differential that is used to liquid crystal cell, for example can be stacked and obtain by polarization film and phase-contrast film.
In addition, polarization film and phase-contrast film also can stackedly use.Can be used as uses such as reflective polarizing film, semi-transparent stratotype polarization film excessively, polarized light separation polarization film.
In addition, above-mentioned optical thin film also can be used as optical compensating film, other various visual angles enlarge film and use.In addition, also can be used as the film that improves brightness uses.Polarization film also can be provided with on its surface the micro concavo-convex structure the reflecting layer, use as antiglare sheet.
When the used for optical elements bonding coat is replicated in optical element, for example it is pressurizeed, only base material is peeled off from optical element then with the used for optical elements bonding coat and the optical element state of contact of used for optical elements adhesive sheet.
So as shown in Figure 2, can obtain single face (or the two sides that is illustrated by the broken lines) at optical element 4 stacked the optical element 5 of used for optical elements bonding coat 2.
Except aforesaid method, by with above-mentioned same method, after used for optical elements binding compositions of the present invention directly coated optical element, drying directly forms the used for optical elements bonding coat at optical element, also can make the optical element that this used for optical elements bonding coat is laminated in optical element thus.
Also between the unactual usage period, surface applying release liner of the used for optical elements bonding coat 2 that exposes that can be in above-mentioned used for optical elements adhesive sheet and optical element etc. has passed through the protective film of lift-off processing.Among Fig. 1 and Fig. 2, release liner with dashed lines (symbol 6) expression.
The used for optical elements bonding coat of the present invention and the used for optical elements adhesive sheet of above gained possess the necessary characteristic of the optical element of fitting in, promptly, under hot and humid environment, also can prevent to float or peel off, the weather resistance of thermotolerance and wet fastness etc. is good, after fitting in optical element, even, also can easily peel off thereafter through long-time or be stored under the hot and humid environment.
Used for optical elements adhesive sheet particularly of the present invention fits in glass, in 60 ℃ through after 17 hours to the bonding force of glass below 10N/25mm, can show good releasable.Therefore, when liquid crystal indicator is peeled off optical element, can not cause damage, can easily peel off optical element liquid crystal indicator.
Below exemplify embodiment and comparative example, the present invention is carried out more specific description.But the present invention is not limited in following embodiment and comparative example.
The gel component of the used for optical elements adhesive sheet of each embodiment and each comparative example gained adopts following calculating formula (1) to calculate.
The gel component measuring method
With bonding coat W
1[g] flooded 7 days in ethyl acetate in 23 ℃, and dried weight is W
2Gel component when [g] (weight %)=(W
2/ W
1) * 100 (1)
Embodiment 1
The ア Network ア ロ Application HS-10 (reactive emulsifier that has added 2 weight parts at 25 weight parts, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) adds 2-EHA 70 weight parts, butyl acrylate 30 weight parts, vinylformic acid 1 weight part and 3-propenyloxy group propyl-triethoxysilicane 0.07 weight part in the water, carry out emulsification with homomixer and modulate emulsion.
Then, possesses the four-hole boiling flask of nitrogen ingress pipe, prolong and thermometer after 1 hour with nitrogen replacement, in this four-hole boiling flask, add entry 30 weight parts and 2,2 '-azo two [N-(2-carboxy ethyl)-2-methyl-prop amidine] hydrate (VA-057, with the pure medicine of light Co., Ltd. system) 0.1 weight part, carry out letex polymerization in 59 ℃ with the emulsion that dripped above gained in 4.5 hours.Polymerization finishes the back ammonification, and pH is adjusted into 8, obtains acrylic acid polymer emulsion A1.
Then, the solid formation corresponding to acrylic acid polymer emulsion A1 divides 100 weight parts, interpolation 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) 0.2 weight part, acquisition used for optical elements binding compositions.
This used for optical elements binding compositions is coated PET (polyethylene terephthalate) film of 38 μ m of process silicon lift-off processing, make dried thickness reach 20 μ m, in 120 ℃ of dryings of carrying out 5 minutes, the used for optical elements adhesive sheet of the used for optical elements bonding coat that obtains the used for optical elements binding compositions stacked and form.Gel component is 72 weight %.
Then, the used for optical elements bonding coat of this used for optical elements adhesive sheet is copied to polarization film, makes optical element.
Embodiment 2
Except with ア Network ア ロ Application HS-10 (reactive emulsifier, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) changes ア Network ア ロ Application HS-20 (reactive emulsifier into, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) outside, operation similarly to Example 1 obtains acrylic acid polymer emulsion A2.
Then, the solid formation corresponding to acrylic acid polymer emulsion A2 divides 100 weight parts, interpolation 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) 0.2 weight part, acquisition used for optical elements binding compositions.
Below, by operation similarly to Example 1, obtain used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 71 weight %.
The ア Network ア ロ Application HS-10 (reactive emulsifier that has added 2 weight parts at 120 weight parts, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) adds 2-EHA 70 weight parts, butyl acrylate 30 weight parts, vinylformic acid 1 weight part in the water, carry out emulsification with homomixer and modulate emulsion.
Then, possesses the four-hole boiling flask of nitrogen ingress pipe, prolong and thermometer after 1 hour with nitrogen replacement, in this four-hole boiling flask, add gained emulsion and 2,2 '-azo two [N-(2-carboxy ethyl)-2-methyl-prop amidine] hydrate (VA-057, with the pure medicine of light Co., Ltd. system) 0.03 weight part, carried out letex polymerization 3.5 hours (concentrating polymeric part) in 56 ℃.
Then, ア Network ア ロ Application HS-10 (reactive emulsifier by 70 parts by weight of acrylic 2-ethylhexyls, 30 parts by weight of acrylic acid butyl esters, 1 parts by weight of acrylic acid, 2 weight parts, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) and 30 weight parts waters modulate emulsion, dripped this emulsion in 59 ℃ with 2.5 hours and carry out letex polymerization (dropping part).Polymerization finishes the back ammonification, and pH is adjusted into 8, obtains acrylic acid polymer emulsion A3.Concentrating polymeric part and dripping ratio partly is 70/30.
Then, the solid formation corresponding to acrylic acid polymer emulsion A3 divides 100 weight parts, interpolation 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) 0.2 weight part, acquisition used for optical elements binding compositions.
Below, by similarly to Example 1 operation, make used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 82 weight %.
Comparative example 1
Except with ア Network ア ロ Application HS-10 (reactive emulsifier, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) changes Ha イ テ ノ-Le NF8 (non-reacted emulsifying agent into, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) outside, operation similarly to Example 1 obtains acrylic acid polymer emulsion A4.
Then, the solid formation corresponding to acrylic acid polymer emulsion A4 divides 100 weight parts, interpolation 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) 0.2 weight part, acquisition used for optical elements binding compositions.
Below, by operation similarly to Example 1, obtain used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 58 weight %.
Comparative example 2
Except with ア Network ア ロ Application HS-10 (reactive emulsifier, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) changes ラ テ system Le E-118B (non-reacted emulsifying agent into, Kao Corp's system) outside, operation similarly to Example 1 obtains acrylic acid polymer emulsion A5.
Then, the solid formation corresponding to acrylic acid polymer emulsion A5 divides 100 weight parts, interpolation 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) 0.2 weight part, acquisition used for optical elements binding compositions.
Below, by operation similarly to Example 1, obtain used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 71 weight %.
Comparative example 3
Except with ア Network ア ロ Application HS-10 (reactive emulsifier, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) changes Ha イ テ ノ-Le NF8 (non-reacted emulsifying agent into, Di-ichi Kogyo Seiyaku Co., Ltd.'s system) outside, operation similarly to Example 3 obtains acrylic acid polymer emulsion A6.
Then, the solid formation corresponding to acrylic acid polymer emulsion A6 divides 100 weight parts, interpolation 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) 0.2 weight part, acquisition used for optical elements binding compositions.
Below, by operation similarly to Example 1, obtain used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 80 weight %.
Comparative example 4
Do not add 3-glycidoxy propyl-triethoxysilicane (KBE-403 among the acrylic acid polymer emulsion A1 except embodiment 1 gained, Shin-Etsu Chemial Co., Ltd's system) outside, other operation obtains the used for optical elements binding compositions similarly to Example 1.
Below, by operation similarly to Example 1, obtain used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 72 weight %.
Comparative example 5
Solid formation corresponding to the acrylic acid polymer emulsion A1 of embodiment 1 gained divides 100 weight parts, add the 3-glycidoxy propyl-triethoxysilicane (KBE-403 of 3 weight parts, Shin-Etsu Chemial Co., Ltd's system), obtain the used for optical elements binding compositions.
Below, by operation similarly to Example 1, obtain used for optical elements adhesive sheet and optical element.
The gel component of used for optical elements adhesive sheet is 72 weight %.
Comparative example 6
With 2 of 70 parts by weight of acrylic 2-ethylhexyls, 30 parts by weight of acrylic acid butyl esters, 1 parts by weight of acrylic acid, 0.15 parts by weight of acrylic 2-hydroxy methacrylate, 0.1 weight part, 2 '-Diisopropyl azodicarboxylate and ethyl acetate 200 weight part inputs possess in the four-hole boiling flask of nitrogen ingress pipe and prolong, after fully carrying out the nitrogen displacement, in 55 ℃ of letex polymerizations of carrying out 6 hours, obtain acrylic acid polymer solution A 8 when under nitrogen gas stream, stirring.
Then, solid formation corresponding to acrylic acid polymer emulsion A8 divides 100 weight parts, add 3-glycidoxy propyl-triethoxysilicane (KBE-403, Shin-Etsu Chemial Co., Ltd's system) polymeric polyisocyanate of the tolylene diisocyanate affixture of 0.2 weight part and TriMethylolPropane(TMP) formation is linking agent 1.5 weight parts, and homogeneous mixes the back and obtains the used for optical elements binding compositions.
This used for optical elements binding compositions is coated PET (polyethylene terephthalate) film of 38 μ m of process silicon lift-off processing, make dried thickness reach 20 μ m, carry out 5 minutes dry and crosslinked in 120 ℃, the used for optical elements adhesive sheet of the used for optical elements bonding coat that obtains the formation of used for optical elements binding compositions stacked.
The gel component of used for optical elements adhesive sheet is 69 weight %.
Then, the used for optical elements bonding coat of this used for optical elements adhesive sheet is copied to polarization film,, makes optical element in 50 ℃ of corrosion treatments of carrying out 24 hours.
Estimate
1) bonding force
On the non-alkali glass plate, come and go the optical element (width is 25mm) of 1 fit each embodiment and the acquisition of each comparative example with the cylinder of 2kg, carry out 30 minutes processing at 50 ℃ of autoclaves after with 0.5Mpa, with the condition of 90 ° of peel angle, peeling rate 300mm/ minute, measure peeling adhesion force (initial stage bonding force) (N/25mm).It the results are shown in table 1.
Carry out after autoclave handles, in 60 ℃ place 17 hours after, with the condition of 90 ° of peel angle, peeling rate 300mm/ minute, measure peeling adhesion force (durable back bonding force) (N/25mm).It the results are shown in table 1.The bonding force of wishing durable back bonding force and initial stage bonding force does not all increase.
2) thermotolerance
The optical element (12 inches) of each embodiment and the acquisition of each comparative example is fitted in the non-alkali glass of thick 0.5mm, carry out 30 minutes processing at 50 ℃ of autoclaves after with 0.5MPa, in 90 ℃ atmosphere, placed 300 hours the situation that the visual observation optical element floats and peels off from glass.It the results are shown in table 1.
Stable on heating determinating reference is as described below.
Zero: do not have and to float and peel off, *: peeling off generation corresponding to fitting area in less than 50% scope, * *: in corresponding to the scope of fitting area more than 50%, peel off generation.
3) wet fastness
The optical element (12 inches) of each embodiment and the acquisition of each comparative example is fitted in the non-alkali glass of thick 0.5mm, carry out 30 minutes processing at 50 ℃ of autoclaves after with 0.5MPa, in 60 ℃, the atmosphere of 90%RH, placed the situation that the visual observation optical element floats and peels off from glass 300 hours.It the results are shown in table 1.
The determinating reference of wet fastness is as described below.
Zero: do not have and to float and peel off, *: peeling off generation corresponding to fitting area in less than 50% scope, * *: in corresponding to the scope of fitting area more than 50%, peel off generation.
Table 1
| The embodiment comparative example | Emulsifying agent | Silane coupling agent (weight part) | Initial stage bonding force (N/25mm) | Durable back bonding force (N/25mm) | Thermotolerance | Wet fastness | ||
| Embodiment 1 | Reactive emulsifier | ??HS-10 | ??KBE403 | ????0.2 | ????3 | ????5 | ?○ | ??○ |
| Embodiment 2 | Reactive emulsifier | ??HS-20 | ??KBE403 | ????0.2 | ????3.2 | ????4.5 | ?○ | ??○ |
| Embodiment 3 | Reactive emulsifier | ??HS-10 | ??KBE403 | ????0.2 | ????5 | ????6.5 | ?○ | ??○ |
| Comparative example 1 | Non-reacted emulsifying agent | ??NF8 | ??KBE403 | ????0.2 | ????4 | ????5.4 | ?×× | ??×× |
| Comparative example 2 | Non-reacted emulsifying agent | ??E-118B | ??KBE403 | ????0.2 | ????3.3 | ????4.3 | ?×× | ??×× |
| Comparative example 3 | Non-reacted emulsifying agent | ??NF8 | ??KBE403 | ????0.2 | ????5.3 | ????6.2 | ?×× | ??×× |
| Comparative example 4 | Reactive emulsifier | ??HS-10 | Do not add | ????0 | ????4.2 | ????4.6 | ?○ | ??× |
| Comparative example 5 | Reactive emulsifier | ??HS-10 | ??KBE403 | ????3 | ????5 | ????11.2 | ?○ | ??○ |
| Comparative example 6 | ??- | ??- | ??KBE403 | ????0.2 | ????6.3 | ????13.1 | ?○ | ??○ |
Can find out that from table 1 each embodiment is showing good result aspect releasable, thermotolerance and the wet fastness, each comparative example all has at least result on the one hand undesirable.
The above illustrative embodiment of the present invention that is illustrated as, they are simple example, are not the explanation that is limited.Those of ordinary skill in the art's variation of the present invention is also contained in the scope of claim described later.
Claims (6)
1. used for optical elements binding compositions, it is characterized in that, comprise acrylic acid polymer emulsion and divide 100 weight parts, be the silane coupling agent of 0.01～1 weight part that with respect to the solid formation of aforementioned acrylic acid polymer emulsion described acrylic acid polymer emulsion carries out letex polymerization by the emulsion that makes the monomer mixture, the reactive emulsifier that contains free-radical polymerised functional group and the polymerization starter that comprise (methyl) acrylate that contains more than the 80 weight % and obtains.
2. used for optical elements bonding coat, it is characterized in that, by comprising acrylic acid polymer emulsion and forming branch 100 weight parts, be that the used for optical elements binding compositions of the silane coupling agent of 0.01～1 weight part forms that with respect to aforementioned acrylic acid polymer emulsion solid described acrylic acid polymer emulsion carries out letex polymerization by the emulsion that makes the monomer mixture, the reactive emulsifier that contains free-radical polymerised functional group and the polymerization starter that comprise (methyl) acrylate that contains more than the 80 weight % and obtains.
3. used for optical elements adhesive sheet, it is characterized in that, possesses the used for optical elements bonding coat that forms by the used for optical elements binding compositions, foregoing comprises acrylic acid polymer emulsion and divides 100 weight parts with respect to the solid formation of aforementioned acrylic acid polymer emulsion, be the silane coupling agent of 0.01～1 weight part, described acrylic acid polymer emulsion is by making the monomer mixture that comprises (methyl) acrylate that contains more than the 80 weight %, the emulsion that contains the reactive emulsifier of free-radical polymerised functional group and polymerization starter carries out letex polymerization and obtains.
4. used for optical elements adhesive sheet as claimed in claim 3, its feature also is, fits in glass, 60 ℃ through after 17 hours to the bonding force of aforementioned glass below 10N/25mm.
5. optical element, it is characterized in that, the used for optical elements bonding coat that is formed by the used for optical elements binding compositions is set at the single face or the two sides of optical element, foregoing comprises acrylic acid polymer emulsion and divides 100 weight parts with respect to the solid formation of aforementioned acrylic acid polymer emulsion, be the silane coupling agent of 0.01～1 weight part, described acrylic acid polymer emulsion is by making the monomer mixture that comprises (methyl) acrylate that contains more than the 80 weight %, the emulsion that contains the reactive emulsifier of free-radical polymerised functional group and polymerization starter carries out letex polymerization and obtains.
6. optical element as claimed in claim 5, its feature are that also aforementioned optical element is any in polaroid, polarizer, the ellipsoidal polarizing plate.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004014436 | 2004-01-22 | ||
| JP2004-014436 | 2004-01-22 | ||
| JP2004014436A JP4481020B2 (en) | 2004-01-22 | 2004-01-22 | Optical member adhesive composition, optical member adhesive layer, optical member adhesive sheet, and optical member |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1651540A true CN1651540A (en) | 2005-08-10 |
| CN100419037C CN100419037C (en) | 2008-09-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100062066A Active CN100419037C (en) | 2004-01-22 | 2005-01-21 | Adhesive composition, adhesive layer and adhesive sheet for optical element and optical element |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP4481020B2 (en) |
| KR (1) | KR101120295B1 (en) |
| CN (1) | CN100419037C (en) |
| TW (1) | TWI352728B (en) |
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| JP2646305B2 (en) * | 1991-12-16 | 1997-08-27 | 昭和高分子株式会社 | Base emulsion for adhesives |
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-
2004
- 2004-01-22 JP JP2004014436A patent/JP4481020B2/en not_active Expired - Lifetime
-
2005
- 2005-01-20 KR KR1020050005460A patent/KR101120295B1/en active IP Right Grant
- 2005-01-21 TW TW094101763A patent/TWI352728B/en active
- 2005-01-21 CN CNB2005100062066A patent/CN100419037C/en active Active
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| CN101586010B (en) * | 2008-05-23 | 2011-05-11 | 北京京都大成化工有限公司 | Preparation method of dry composite crylic acid resin aqueous adhesive |
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| CN104342073A (en) * | 2014-10-31 | 2015-02-11 | 中科院广州化学有限公司 | Organic silicon modified phenyl emulsion pressure-sensitive adhesive with high release force and low residue as well as preparation method thereof and application |
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Also Published As
| Publication number | Publication date |
|---|---|
| KR20050076819A (en) | 2005-07-28 |
| JP4481020B2 (en) | 2010-06-16 |
| TW200524998A (en) | 2005-08-01 |
| CN100419037C (en) | 2008-09-17 |
| KR101120295B1 (en) | 2012-03-07 |
| TWI352728B (en) | 2011-11-21 |
| JP2005206689A (en) | 2005-08-04 |
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