WO2023022029A1 - Adhesive layer-attached polarizing film having separator - Google Patents
Adhesive layer-attached polarizing film having separator Download PDFInfo
- Publication number
- WO2023022029A1 WO2023022029A1 PCT/JP2022/030131 JP2022030131W WO2023022029A1 WO 2023022029 A1 WO2023022029 A1 WO 2023022029A1 JP 2022030131 W JP2022030131 W JP 2022030131W WO 2023022029 A1 WO2023022029 A1 WO 2023022029A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- adhesive layer
- separator
- polarizing film
- sensitive adhesive
- pressure
- Prior art date
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- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 239000002683 reaction inhibitor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006268 silicone film Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 229940117986 sulfobetaine Drugs 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical class [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- PHBSBOANHONSDB-UHFFFAOYSA-N triethoxy(7-oxabicyclo[4.1.0]heptan-5-yl)silane Chemical compound CCO[Si](OCC)(OCC)C1CCCC2OC12 PHBSBOANHONSDB-UHFFFAOYSA-N 0.000 description 1
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 1
- 125000001889 triflyl group Chemical group FC(F)(F)S(*)(=O)=O 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical class O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- C09J201/00—Adhesives based on unspecified macromolecular compounds
- C09J201/02—Adhesives based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C09J201/06—Adhesives based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
- C09J201/08—Carboxyl groups
-
- 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
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
Definitions
- the present invention relates to a polarizing film with a pressure-sensitive adhesive layer having a separator.
- Polarizing films are used in image display devices such as liquid crystal display devices. When sticking a polarizing film on a display panel such as a liquid crystal panel, an adhesive is usually used.
- a polarizing film with an adhesive layer in which an adhesive is provided in advance as an adhesive layer on one side of the polarizing film, because it generally has the advantage of not requiring a drying process for attaching the polarizing film. is used.
- the pressure-sensitive adhesive layer-attached polarizing film is usually provided with a separator (also referred to as release film or release liner) on the surface of the pressure-sensitive adhesive layer in order to protect the pressure-sensitive adhesive layer before attachment.
- the polarizing film with an adhesive layer has become thinner, and there is a problem that it is difficult to peel off the separator from the adhesive layer because it does not have stiffness. Therefore, there is a demand for easy release of the separator.
- the adhesive layer is required to have functionality such as conductivity and durability, and development of a polarizing film with an adhesive layer that has a separator that achieves both easy release of the separator and the functionality of the adhesive layer is underway. is underway.
- a polyester film for a substrate-less double-sided pressure-sensitive adhesive sheet that can minimize peel speed dependency, has good releasability, and has low migration
- a polyester film characterized by having a reactive silicone resin having an alkenyl group and an alkyl group as functional groups, an unreactive silicone resin having a mass average molecular weight of 400,000 or more, and a silicone release layer containing a platinum catalyst is proposed. It is
- a release sheet that exhibits a very small release force and can be used as an ultra-light release sheet A base material and a release agent layer provided on at least one side of the base material,
- the substrate is made of a plastic film
- the release agent layer is formed from a release agent composition containing a polyorganosiloxane having a weight average molecular weight of 5000 or more and 100000 or less,
- a release sheet has been proposed in which the release agent layer has a thickness of 0.3 ⁇ m or more and 1.0 ⁇ m or less.
- An object of the present invention is to provide a polarizing film with a pressure-sensitive adhesive layer having a separator that achieves both easy peelability of the separator and high-temperature durability of the pressure-sensitive adhesive layer.
- the present invention is a polarizing film with a pressure-sensitive adhesive layer having a separator, wherein the pressure-sensitive adhesive layer with a separator having a pressure-sensitive adhesive layer on the separator is provided on one or both sides of the polarizing film,
- the separator has a release layer on the base film,
- the release layer contains a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more,
- the content of the reactive silicone resin is 50 to 70% by mass, and the content of the non-reactive silicone resin is 30 to 50% by mass, based on the total content of 100% by mass of the reactive silicone resin and the non-reactive silicone resin.
- the release layer has an elastic modulus of less than 1.5 MPa
- the adhesive layer is provided on the release layer
- the pressure-sensitive adhesive layer-attached polarizing film has a separator, wherein the pressure-sensitive adhesive layer contains a base polymer containing 0.5% by mass or more of a carboxy group-containing monomer as a monomer unit.
- the adhesive layer preferably contains a conductive agent.
- the surface resistance value of the pressure-sensitive adhesive layer is preferably 1.0 ⁇ 10 12 ⁇ / ⁇ or less.
- the peeling force when peeling the separator from the pressure-sensitive adhesive layer is preferably 0.12 N/50 mm or less.
- the thickness of the polarizing film is preferably 100 ⁇ m or less.
- the separator of the present invention contains a specific proportion of a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more, and has an elastic modulus of less than 1.5 MPa. Since the polarizing film with a pressure-sensitive adhesive layer is thinned, the separator can be easily peeled off from the pressure-sensitive adhesive layer due to the presence of the mold layer. Moreover, since the pressure-sensitive adhesive layer of the present invention contains a base polymer containing 0.5% by mass or more of a carboxy group-containing monomer as a monomer unit, it is excellent in high temperature durability. By using the separator and the pressure-sensitive adhesive layer in combination, a polarizing film with a pressure-sensitive adhesive layer having a separator that achieves both easy peelability of the separator and high-temperature durability of the pressure-sensitive adhesive layer can be obtained.
- the polarizing film with an adhesive layer having a separator of the present invention is a polarizing film in which an adhesive layer with a separator having an adhesive layer on a separator is provided on one or both sides of the polarizing film.
- the pressure-sensitive adhesive layer with a separator of the present invention has a pressure-sensitive adhesive layer on a separator, and the separator has a release layer on a base film.
- the adhesive layer is provided on the release layer.
- the separator may have an oligomer prevention layer between the base film and the release layer.
- a plastic film can be used as the base film.
- plastic films include polyolefin films such as polyethylene film, polypropylene film, polybutene film, polybutadiene film and polymethylpentene film; vinyl chloride films such as polyvinyl chloride film and vinyl chloride copolymer film; polyethylene terephthalate film and polybutylene.
- Polyester films such as terephthalate films and polynaphthylene terephthalate films; other examples include polyurethane films and ethylene-vinyl acetate copolymer films.
- the thickness of the base film is usually 5-200 ⁇ m, preferably 5-100 ⁇ m, more preferably 10-50 ⁇ m.
- the base film may be subjected to surface treatment such as corona treatment or plasma treatment.
- the release layer is provided to enhance releasability from the pressure-sensitive adhesive layer.
- the release layer is formed of a silicone-based release agent, and the silicone-based release agent includes a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more. contains
- a reactive silicone resin having a reactive functional group a crosslinked structure can be formed in the release layer via the reactive functional group by heating or irradiation with an active energy ray, and the elastic modulus of the release layer can be easily adjusted to the desired range.
- a non-reactive silicone resin having a weight average molecular weight of 400,000 or more it is possible to impart light releasability.
- the release layer can be formed as a coating layer on the base film or the oligomer prevention layer.
- the release layer can also be formed by transfer bonding.
- Examples of reactive silicone resins having reactive functional groups include polyorganosiloxanes having reactive functional groups.
- Examples of polyorganosiloxane include polydimethylsiloxane, polyphenylmethylsiloxane, polydiphenylsiloxane, and the like. One type of polyorganosiloxane may be used alone, or two or more types may be used in combination.
- the reactive functional group may be introduced to one end of the polyorganosiloxane, may be introduced to both ends, or may be introduced to a side chain.
- Examples of reactive functional groups include alkenyl groups having 2 to 10 carbon atoms, and examples of the alkenyl groups include vinyl, allyl, propenyl, butenyl, pentenyl, hexenyl, and heptenyl groups. , an octenyl group, and the like.
- Examples of reactive silicone resins having a reactive functional group include KS-774, KS-775, KS-778, KS-779H, KS-847H, KS-856 and X-62 manufactured by Shin-Etsu Chemical Co., Ltd. -2422, X-62-2461, X-62-1387, X-62-5039, X-62-5040, KNS-3051, X-62-1496, KNS320A, KNS316, X-62-1574A/B, X -62-7052, X-62-7028A/B, X-62-7619, X-62-7213; YSR-3022, TPR-6700, TPR-6720, TPR-6721, TPR6500 manufactured by Momentive Performance Materials , TPR6501, UV9300, UV9425, XS56-A2775, XS56-A2982, XS56-C6010, XS56-C4880, UV9430, TPR6600, T
- non-reactive silicone resins having a weight average molecular weight of 400,000 or more include polyorganosiloxanes having a weight average molecular weight of 400,000 or more, preferably polyorganosiloxanes represented by the following general formula (A). . R3SiO ( R2SiO ) nSiR3 ( A) (Wherein, each R is independently a hydrocarbon group having no aliphatic unsaturation, and n is a positive integer.)
- the weight-average molecular weight of the non-reactive silicone resin is preferably 500,000 or more, more preferably 600,000 or more, from the viewpoint of imparting easy release properties to the release layer, and increases the elastic modulus of the release layer. From the viewpoint of suppressing this, it is preferably 1,000,000 or less, more preferably 900,000 or less.
- the weight-average molecular weight is a value measured by GPC (gel permeation chromatography) and calculated by polystyrene conversion.
- the elastic modulus of the release layer is adjusted to less than 1.5 MPa, and from the viewpoint of imparting excellent light release properties to the release layer, the combination of the reactive silicone resin and the non-reactive silicone resin Of the total content of 100% by mass, the content of the reactive silicone resin is 50 to 70% by mass, and the content of the non-reactive silicone resin is 30 to 50% by mass.
- the reactive silicone resin is contained.
- the content of the non-reactive silicone resin is 55-65% by mass, and the content of the non-reactive silicone resin is 35-45% by mass, more preferably the content of the reactive silicone resin is 57-63% by mass, the non-reactive silicone resin
- the content of is 37 to 43% by mass.
- the release layer may contain a cross-linking agent, a catalyst, a reaction inhibitor, an adhesion improver, etc., in addition to the silicone resin.
- the release layer is usually 120 to 200 after coating a composition containing the above materials on a substrate film or oligomer prevention layer by a conventionally known coating method such as reverse gravure coating, bar coating, and die coating. C. for 30 seconds to 30 minutes for hardening. Further, if necessary, heat treatment and active energy ray irradiation such as ultraviolet irradiation may be used in combination.
- the thickness of the release layer is usually 10 to 2000 nm, preferably 10 to 1000 nm, more preferably 10 to 500 nm, still more preferably 50 to 300 nm.
- the elastic modulus of the release layer is less than 1.5 MPa, preferably 1.4 MPa or less, more preferably 1.3 MPa or less, still more preferably 1, from the viewpoint of imparting excellent easy release properties to the release layer. .2 MPa or less.
- the elastic modulus of the release layer is preferably 0.5 MPa or more, more preferably 0.75 MPa or more, and still more preferably 0.9 MPa or more, from the viewpoint of preventing the release layer from coming off.
- the elastic modulus of the release layer is measured by the method described in Examples.
- the oligomer-preventing layer is a functional layer for preventing the oligomer contained in the base film from eluting into the pressure-sensitive adhesive layer.
- a material for forming the oligomer-preventing layer an inorganic material, an organic material, or a composite material thereof can be used.
- inorganic substances include silica-based materials, metals such as gold, silver, platinum, palladium, copper, aluminum, nickel, chromium, titanium, iron, cobalt, tin, and alloys thereof, indium oxide, tin oxide, and titanium oxide. , metal oxides such as cadmium oxide or mixtures thereof, and other metal compounds such as steel iodide.
- organic substances include polyvinyl alcohol-based resins, acrylic-based resins, urethane-based resins, melamine-based resins, UV-curable resins, and epoxy-based resins.
- Composite materials include mixtures of the above organic matter and inorganic particles such as alumina, silica, and mica.
- the oligomer-preventing layer is preferably formed from a composition containing a silica-based material or a polyvinyl alcohol-based resin.
- silica-based material examples include organosiloxanes represented by the following general formula (I).
- R 1 and R 2 are each independently an epoxy group-containing organic group such as a ⁇ -glycidoxypropyl group, a 3,4-epoxycyclohexylethyl group, or It is an alkoxy group such as a methoxy group or an ethoxy group, and R3 is an alkoxy group such as a methoxy group or an ethoxy group, or a group represented by the following general formula (II).
- n and m are integers from 0 to 10;
- R4 is the same epoxy group-containing organic group or alkoxy group as R1 or R2 .
- organosiloxane examples include ⁇ -glycidoxypropyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 5 ,6-epoxycyclohexyltriethoxysilane, tetraethoxysilane and the like, and hydrolyzable products (oligomers) of these monomers or mixtures of these monomers.
- examples of the silica-based material include silane compounds having an amino group.
- an alkoxysilane represented by the following general formula (III) is preferable.
- Y—R—Si—(X) 3 (III) (In the general formula (III), Y is an amino group, R is an alkylene group such as methylene, ethylene, or propylene, X is an alkoxy group such as a methoxy group or an ethoxy group, an alkyl group, or an organic functional group having these groups. and at least one is an alkoxy group).
- silane compound having an amino group examples include N- ⁇ (aminoethyl) ⁇ -aminopropyltrimethoxysilane, N- ⁇ (aminoethyl) ⁇ -aminopropyltriethoxysilane, N- ⁇ (aminoethyl) ⁇ -aminopropylmethyldimethoxysilane, ⁇ -aminopropyltrimethoxysilane, N-phenyl- ⁇ -aminopropyltrimethoxysilane and the like.
- the silica-based materials include (meth)acryl group-containing silane compounds such as 3-acryloxypropyltrimethoxysilane and 3-methacryloxypropyltriethoxysilane, and isocyanate group-containing silanes such as 3-isocyanatopropyltriethoxysilane. compounds and the like.
- Specific products of the silica-based material include KR-401N, X-40-9227, X-40-9247, KR-510, KR-9218, KR-213, KR-217, and X manufactured by Shin-Etsu Chemical Co., Ltd. -41-1053, X-40-1056, X-41-1805, X-41-1810, X-40-2651, X-40-2652B, X-40-2655A, X-40-2761, X-40 -2672 and the like.
- silica-based material Only one type of the silica-based material may be used, or two or more types may be used.
- the oligomer-preventing layer formed of the silica-based material can contain, if necessary, an organic compound having a metal element (a metal compound such as a metal chelate), a catalyst, or the like. Only one metal organic compound having a metal element may be used, or two or more thereof may be used.
- an organic compound having a metal element a metal compound such as a metal chelate
- a catalyst or the like. Only one metal organic compound having a metal element may be used, or two or more thereof may be used.
- organic compounds containing an aluminum element having a chelate structure organic compounds containing a titanium element, and organic compounds containing a zirconium element are preferable in terms of particularly good performance in preventing the elution of oligomers.
- Such compounds are specifically described in "Crosslinking Agent Handbook” (edited by Shinzo Yamashita and Tosuke Kaneko, Taiseisha Co., Ltd., 1990 edition).
- the oligomer-preventing layer formed from the silica-based material can be formed by applying a solution of the silica-based material dissolved in a solvent such as alcohol to the substrate film and then drying.
- concentration of the solution in which the silica-based material is dissolved is not particularly limited, it is preferably about 0.1 to 40% by weight.
- drying temperature after coating is not particularly limited, it is preferably about 100 to 150°C.
- drying time after application is not particularly limited, it is preferably about 30 seconds to 30 minutes.
- polyvinyl alcohol-based resin examples include polyvinyl alcohol and derivatives thereof.
- Derivatives of polyvinyl alcohol include polyvinyl formal and polyvinyl acetal, as well as those modified with olefins such as ethylene and propylene, unsaturated carboxylic acids such as acrylic acid, methacrylic acid and crotonic acid, their alkyl esters, and acrylamide. are mentioned. Only one type of polyvinyl alcohol-based resin may be used, or two or more types may be used.
- the degree of polymerization of the polyvinyl alcohol resin is not particularly limited, it is usually 100 or more, preferably 300 to 40,000.
- the degree of saponification of the polyvinyl alcohol resin is not particularly limited, one having a degree of saponification of 70 mol % or more, preferably 80 mol % or more and 99.9 mol % or less is preferably used.
- the composition containing the polyvinyl alcohol-based resin can contain a binder polymer.
- Binder polymers include polyacrylamide, polyalkylene glycol, polyalkyleneimine, methylcellulose, hydroxycellulose, starches, polyurethane, polyester, polyacrylate, chlorine-based polymers (polyvinyl chloride, vinyl chloride vinyl acetate copolymer, etc.), polyolefin etc.
- nonionic, cationic, and amphoteric organic polymers that can be used as aqueous solutions or aqueous dispersions can be mentioned. Good adhesion is obtained when polyester or polyacrylate is used.
- By copolymerizing a nonionic, cationic, or amphoteric hydrophilic component as one component of the monomer these polymers are imparted with hydrophilicity and can be dispersed in water.
- the composition containing the polyvinyl alcohol-based resin may contain a cross-linking agent.
- cross-linking agents include methylolated or alkylolated urea-based, melamine-based, guanamine-based, acrylamide-based, polyamide-based compounds, epoxy compounds, aziridine compounds, blocked polyisocyanates, silane coupling agents, titanium coupling agents, Zirco An aluminate coupling agent etc. are mentioned. These cross-linking components may be pre-bonded with the binder polymer.
- the composition containing the polyvinyl alcohol-based resin may contain inorganic particles for the purpose of improving the adhesion and slipperiness of the oligomer-preventing layer.
- inorganic particles include silica, alumina, kaolin, calcium carbonate, titanium oxide, and barium salts.
- the formation of the oligomer-preventing layer can be carried out by applying a solution obtained by dissolving the composition containing the polyvinyl alcohol resin in a solvent such as water or alcohol to the substrate film and then drying the solution. Moreover, you may extend
- concentration of the solution in which the composition containing the polyvinyl alcohol resin is dissolved is not particularly limited, it is preferably about 0.1 to 40% by weight.
- the drying temperature after coating is not particularly limited, it is preferably about 60 to 200°C. Also, the drying time after coating is not particularly limited, but it is preferably about 3 to 60 seconds. Heat treatment and active energy ray irradiation such as ultraviolet irradiation may be used in combination as necessary.
- the content of the polyvinyl alcohol-based resin in the oligomer-preventing layer is not particularly limited, but is preferably 10 to 100% by weight, more preferably 20 to 90% by weight, and most preferably 30 to 80% by weight. good.
- the method for forming the oligomer-preventing layer is not particularly limited, and may be appropriately selected depending on the material for forming it, and a coating method, a spray method, a spin coating method, an in-line coating method, or the like is used. Also, a vacuum vapor deposition method, a sputtering method, an ion plating method, a spray pyrolysis method, a chemical plating method, an electroplating method, or the like can be used.
- the thickness of the oligomer-preventing layer is preferably set appropriately in the range of 5 to 100 nm, more preferably 10 to 70 nm.
- the adhesive layer is formed from an adhesive composition.
- adhesive compositions include rubber-based adhesive compositions, acrylic adhesive compositions, silicone-based adhesive compositions, urethane-based adhesive compositions, vinyl alkyl ether-based adhesive compositions, and polyvinyl alcohol-based adhesive compositions. products, polyvinylpyrrolidone-based pressure-sensitive adhesive compositions, polyacrylamide-based pressure-sensitive adhesive compositions, cellulose-based pressure-sensitive adhesive compositions, and the like.
- the adhesive composition preferably contains a base polymer.
- an adhesive base polymer is selected according to the type of the adhesive composition.
- the base polymer contains 0.5% by mass or more, preferably 1% by mass or more, more preferably 3% by mass or more of a carboxy group-containing monomer as a monomer unit. do.
- the base polymer preferably contains 10% by mass or less, more preferably 8% by mass or less of a carboxy group-containing monomer as a monomer unit. More preferably, it contains 5% by mass or less.
- the acrylic pressure-sensitive adhesive composition has excellent optical transparency, exhibits appropriate wettability, cohesiveness, and adhesive properties, and is excellent in weather resistance, heat resistance, etc. is preferably used.
- the acrylic pressure-sensitive adhesive composition preferably contains a (meth)acrylic polymer as an adhesive base polymer.
- a (meth)acrylic polymer usually contains alkyl (meth)acrylate as a main component as a monomer unit.
- (Meth)acrylate refers to acrylate and/or methacrylate, and has the same meaning as (meth) in the present invention.
- alkyl group examples include methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, amyl group, hexyl group, cyclohexyl group, heptyl group, 2-ethylhexyl group, isooctyl group, nonyl group, decyl group, Examples include isodecyl group, dodecyl group, isomyristyl group, lauryl group, tridecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, and the like. Only one type of alkyl (meth)acrylate may be used, or two or more types
- alkyl (meth) acrylate aromatic rings such as phenoxyethyl (meth) acrylate and benzyl (meth) acrylate are used from the viewpoint of adhesive properties, durability, adjustment of retardation, adjustment of refractive index, etc.
- Alkyl (meth)acrylate containing can be used.
- the (meth)acrylic polymer contains at least one polymerizable functional group having an unsaturated double bond such as a (meth)acryloyl group or a vinyl group for the purpose of improving adhesiveness and heat resistance. can be introduced by copolymerization.
- copolymerizable monomers include 2-hydroxyethyl (meth)acrylate, 3-hydroxypropyl (meth)acrylate, 4-hydroxybutyl (meth)acrylate, 6-hydroxyhexyl (meth)acrylate, ( Hydroxy group-containing monomers such as 8-hydroxyoctyl meth)acrylate, 10-hydroxydecyl (meth)acrylate, 12-hydroxylauryl (meth)acrylate and (4-hydroxymethylcyclohexyl)-methylacrylate; (meth)acrylic Carboxy group-containing monomers such as acids, carboxyethyl (meth)acrylate, carboxypentyl (meth)acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid; acid anhydride group-containing monomers such as maleic anhydride and itaconic anhydride; Caprolactone adducts of acrylic acid; styrenesulfonic acid, allylsulfonic acid, 2-(meth)
- the (meth)acrylic polymer contains 0.5% by mass or more of the carboxy group-containing monomer as a monomer unit from the viewpoint of improving the high-temperature durability of the pressure-sensitive adhesive layer. Preferred contents are as described above.
- the (meth)acrylic polymer is mainly composed of alkyl (meth)acrylate in the mass ratio of all constituent monomers, and the ratio of the copolymerization monomer is not particularly limited, but the mass ratio of all constituent monomers is 0 to 20. %, preferably about 0.1 to 15%, more preferably about 0.1 to 10%.
- the (meth)acrylic polymer usually used has a weight average molecular weight (Mw) in the range of 500,000 to 3,000,000. Considering durability, especially heat resistance, the weight average molecular weight (Mw) is preferably 700,000 to 2,700,000, more preferably 800,000 to 2,500,000. A weight-average molecular weight (Mw) of less than 500,000 is not preferable in terms of heat resistance. Further, if the weight average molecular weight (Mw) is more than 3,000,000, a large amount of diluent solvent is required to adjust the viscosity for coating, which is not preferable because it increases the cost.
- the weight average molecular weight (Mw) is a value measured by GPC (gel permeation chromatography) and calculated by polystyrene conversion.
- the (meth)acrylic polymer to be obtained may be a random copolymer, a block copolymer, a graft copolymer, or the like.
- the polymerization initiator, chain transfer agent, emulsifier, etc. used in the radical polymerization are not particularly limited and can be appropriately selected and used.
- the weight-average molecular weight (Mw) of the (meth)acrylic polymer can be controlled by the amount of the polymerization initiator and the chain transfer agent used and the reaction conditions, and the amount used is appropriately adjusted according to these types. be.
- solution polymerization ethyl acetate, toluene, or the like is used as a polymerization solvent.
- the reaction is carried out under an inert gas stream such as nitrogen, adding a polymerization initiator, and generally at a temperature of about 50 to 70° C. for about 5 to 30 hours.
- the adhesive composition preferably contains a conductive agent in addition to the base polymer.
- Conductive agents include ionic compounds, ionic surfactants, conductive polymers, metal oxides, and the like.
- an alkali metal salt and/or an organic cation-anion salt can be preferably used.
- alkali metal salts organic salts and inorganic salts of alkali metals can be used.
- organic cation-anion salt refers to an organic salt whose cation part is composed of an organic substance, and whose anion part may be an organic substance or an inorganic substance. It can be.
- Organic cation-anion salts are also referred to as ionic liquids, ionic solids. Only one kind of ionic compound may be used, or two or more kinds thereof may be used.
- alkali metal ions constituting the cation portion of the alkali metal salt include ions of lithium, sodium, and potassium. Among these alkali metal ions, lithium ions are preferred.
- the anion portion of the alkali metal salt may be composed of an organic substance or an inorganic substance.
- the anion moiety constituting the organic salt includes CH 3 COO ⁇ , CF 3 COO ⁇ , CH 3 SO 3 ⁇ , CF 3 SO 3 ⁇ , (CF 3 SO 2 ) 3 C ⁇ , C 4 F 9 SO 3 ⁇ , C 3 F 7 COO ⁇ , (CF 3 SO 2 )(CF 3 CO)N ⁇ , —O 3 S(CF 2 ) 3 SO 3 ⁇ , PF 6 ⁇ , CO 3 2 ⁇ , or the following general formula (1) through (4), (1): (C n F 2n+1 SO 2 ) 2 N ⁇ (where n is an integer of 1 to 10), (2): CF 2 (C m F 2m SO 2 ) 2 N ⁇ (where m is an integer of 1 to 10), (3): - O 3 S(CF 2 ) l SO 3 - (where l is an integer of 1 to 10),
- an anion moiety containing a fluorine atom is preferably used because an ionic compound having good ion dissociation properties can be obtained.
- the anion moiety constituting the inorganic salt include Cl ⁇ , Br ⁇ , I ⁇ , AlCl 4 ⁇ , Al 2 Cl 7 ⁇ , BF 4 ⁇ , PF 6 ⁇ , ClO 4 ⁇ , NO 3 ⁇ , AsF 6 ⁇ , SbF 6 ⁇ , NbF 6 ⁇ , TaF 6 ⁇ , (CN) 2 N ⁇ , etc. are used.
- (CF 3 SO 2 ) 2 N ⁇ , (C 2 F 5 SO 2 ) 2 N ⁇ , and the like (perfluoroalkylsulfonyl) imides represented by the general formula (1) are preferable, and ( (Trifluoromethanesulfonyl)imide represented by CF 3 SO 2 ) 2 N ⁇ is preferred.
- alkali metal organic salts include sodium acetate, sodium alginate, sodium ligninsulfonate, sodium toluenesulfonate, LiCF 3 SO 3 , Li(CF 3 SO 2 ) 2 N, Li(C 2 F 5 SO2 ) 2N , Li ( C4F9SO2 ) 2N , Li ( CF3SO2 ) 3C , KO3S ( CF2 ) 3SO3K , LiO3S ( CF2 ) 3SO3 K and the like, among which LiCF 3 SO 3 , Li(CF 3 SO 2 ) 2 N, Li(C 2 F 5 SO 2 ) 2 N, Li(C 4 F 9 SO 2 ) 2 N, Li( CF 3 SO 2 ) 3 C and the like are preferred, and fluorine-containing lithium imides such as Li(CF 3 SO 2 ) 2 N, Li(C 2 F 5 SO 2 ) 2 N and Li(C 4 F 9 SO 2 ) 2 N Salts are more preferred, especially (perfluorine
- Inorganic salts of alkali metals include lithium perchlorate and lithium iodide.
- the organic cation-anion salt is composed of a cation component and an anion component
- the cation component is composed of an organic substance.
- cationic components include pyridinium cations, piperidinium cations, pyrrolidinium cations, cations having a pyrroline skeleton, cations having a pyrrole skeleton, imidazolium cations, tetrahydropyrimidinium cations, dihydropyrimidinium cations, Examples include pyrazolium cations, pyrazolinium cations, tetraalkylammonium cations, trialkylsulfonium cations, tetraalkylphosphonium cations, and the like.
- anion component examples include Cl ⁇ , Br ⁇ , I ⁇ , AlCl 4 ⁇ , Al 2 Cl 7 ⁇ , BF 4 ⁇ , PF 6 ⁇ , ClO 4 ⁇ , NO 3 ⁇ , CH 3 COO ⁇ , CF 3 COO ⁇ , CH 3 SO 3 ⁇ , CF 3 SO 3 ⁇ , (CF 3 SO 2 ) 3 C ⁇ , AsF 6 ⁇ , SbF 6 ⁇ , NbF 6 ⁇ , TaF 6 ⁇ , (CN) 2 N ⁇ , C 4 F 9 SO 3 ⁇ , C 3 F 7 COO ⁇ , ((CF 3 SO 2 )(CF 3 CO)N ⁇ , —O 3 S(CF 2 ) 3 SO 3 ⁇ , or the following general formulas (1) to (4) , (1): (C n F 2n+1 SO 2 ) 2 N ⁇ (where n is an integer of 1 to 10), (2): CF 2 (C
- Examples of the ionic compound include inorganic salts such as ammonium chloride, aluminum chloride, copper chloride, ferrous chloride, ferric chloride, and ammonium sulfate, in addition to the alkali metal salts and organic cation-anion salts described above. be done.
- inorganic salts such as ammonium chloride, aluminum chloride, copper chloride, ferrous chloride, ferric chloride, and ammonium sulfate, in addition to the alkali metal salts and organic cation-anion salts described above. be done.
- ionic surfactant examples include cationic surfactants (quaternary ammonium salt type, phosphonium salt type, sulfonium salt type, etc.), anionic surfactants (carboxylic acid type, sulfonate type, sulfate type, phosphate type, phosphite type, etc.), Zwitterionic (sulfobetaine type, alkylbetaine type, alkylimidazolium betaine type, etc.) or nonionic (polyhydric alcohol derivative, ⁇ -cyclodextrin inclusion compound, sorbitan fatty acid monoester/diester, polyalkylene oxide derivative, amine oxide etc.). Only 1 type may be used for an ionic surfactant, and 2 or more types may be used for it.
- cationic surfactants quaternary ammonium salt type, phosphonium salt type, sulfonium salt type, etc.
- anionic surfactants carboxylic acid type, sulfonate
- Examples of the conductive polymer include polyaniline-based, polythiophene-based, polypyrrole-based, and polyquinoxaline-based polymers. Polythiophene and the like are preferably used. Polythiophene is particularly preferred. Only one type of conductive polymer may be used, or two or more types may be used.
- the metal oxide examples include tin oxide, antimony oxide, indium oxide, and zinc oxide.
- the tin oxide type is preferable.
- Tin oxides include, in addition to tin oxide, antimony-doped tin oxide, indium-doped tin oxide, aluminum-doped tin oxide, tungsten-doped tin oxide, titanium oxide-cerium oxide-tin oxide composite, titanium oxide- Composites of tin oxide and the like can be mentioned. Only one kind of metal oxide may be used, or two or more kinds thereof may be used.
- conductive agents other than the above acetylene black, ketjen black, natural graphite, artificial graphite, titanium black, cation type (quaternary ammonium salt, etc.), amphoteric ion type (betaine compound, etc.), anionic type (sulfonate etc.) or a homopolymer of a monomer having a nonionic (glycerin, etc.) ion-conductive group or a copolymer of the monomer with another monomer, an acrylate or methacrylate derived from a quaternary ammonium base and a permanent antistatic agent of the type in which a hydrophilic polymer such as a polyethylene methacrylate copolymer is alloyed with an acrylic resin or the like.
- a hydrophilic polymer such as a polyethylene methacrylate copolymer is alloyed with an acrylic resin or the like.
- an ionic compound as the conductive agent from the viewpoints of high conductive performance, excellent dispersibility and transparency in the adhesive, and storage stability in the adhesive.
- the mixing ratio of the conductive agent is preferably 0.0001 to 10 parts by mass with respect to 100 parts by mass of the base polymer. If the amount of the conductive agent is less than 0.0001 parts by mass, the effect of improving the antistatic performance may not be sufficient. On the other hand, if the conductive agent is more than 10 parts by mass, the durability may not be sufficient.
- the conductive agent is preferably 0.01 parts by mass or more, more preferably 0.1 parts by mass or more.
- the conductive agent is preferably 8 parts by mass or less, more preferably 6 parts by mass or less.
- the adhesive composition can contain a cross-linking agent.
- a cross-linking agent an organic cross-linking agent or a polyfunctional metal chelate can be used.
- organic cross-linking agents include isocyanate-based cross-linking agents, peroxide-based cross-linking agents, epoxy-based cross-linking agents, and imine-based cross-linking agents.
- Polyfunctional metal chelates are those in which polyvalent metals are covalently or coordinately bonded to organic compounds. Polyvalent metal atoms include Al, Cr, Zr, Co, Cu, Fe, Ni, V, Zn, In, Ca, Mg, Mn, Y, Ce, Sr, Ba, Mo, La, Sn, and Ti. mentioned. An oxygen atom etc.
- the cross-linking agent is preferably an isocyanate-based cross-linking agent or a peroxide-based cross-linking agent. Only one type of cross-linking agent may be used, or two or more types may be used.
- the mixing ratio of the cross-linking agent is preferably 0.01 to 20 parts by mass, more preferably 0.03 to 10 parts by mass, with respect to 100 parts by mass of the base polymer. If the amount of the cross-linking agent is less than 0.01 parts by mass, the cohesive force of the adhesive tends to be insufficient, and foaming may occur during heating. Peeling is likely to occur in a reliability test or the like.
- the adhesive composition can contain a silane coupling agent. Durability can be improved by using a silane coupling agent. Only one kind of silane coupling agent may be used, or two or more kinds thereof may be used.
- the mixing ratio of the silane coupling agent is preferably 0.001 to 5 parts by mass, more preferably 0.01 to 1 part by mass, and 0.02 to 1 part by mass with respect to 100 parts by mass of the base polymer. is more preferred, and 0.05 to 0.6 parts by mass is particularly preferred. It is appropriately selected within this range in order to improve durability and maintain an appropriate adhesive strength to optical members such as liquid crystal panels.
- the pressure-sensitive adhesive composition may contain other known additives, such as powders such as colorants and pigments, dyes, surfactants, plasticizers, tackifiers, surface lubricants. , leveling agents, softeners, antioxidants, anti-aging agents, light stabilizers, UV absorbers, polymerization inhibitors, inorganic or organic fillers, metal powders, particulates, foils, etc. can be added as appropriate. Also, a redox system with a reducing agent added may be employed within a controllable range.
- the pressure-sensitive adhesive layer with a separator can be produced by applying a solution containing the pressure-sensitive adhesive composition onto the release layer of the separator, followed by drying to form a pressure-sensitive adhesive layer.
- a solution containing the pressure-sensitive adhesive composition onto the release layer of the separator, followed by drying to form a pressure-sensitive adhesive layer.
- one or more solvents other than the polymerization solvent may be newly added as appropriate.
- Various methods are used as a method for applying the pressure-sensitive adhesive composition. Specifically, roll coating, kiss roll coating, gravure coating, reverse coating, roll brushing, spray coating, dip roll coating, bar coating, knife coating, air knife coating, curtain coating, lip coating, extrusion coating using a die coater, etc. method such as the law.
- the thickness of the adhesive layer is not particularly limited, and is about 1 to 100 ⁇ m. It is preferably 2 to 50 ⁇ m, more preferably 2 to 40 ⁇ m, even more preferably 5 to 35 ⁇ m.
- the surface resistance value of the pressure-sensitive adhesive layer is preferably 1.0 ⁇ 10 12 ⁇ / ⁇ or less from the viewpoint of imparting conductivity to the pressure-sensitive adhesive layer with separator and suppressing white unevenness of the liquid crystal panel. It is more preferably 0 ⁇ 10 11 ⁇ / ⁇ or less, and further preferably 1.0 ⁇ 10 10 ⁇ / ⁇ or less.
- the pressure-sensitive adhesive layer-attached polarizing film having the separator of the present invention is obtained by bonding the pressure-sensitive adhesive layer side of the separator-attached pressure-sensitive adhesive layer to one side or both sides of the polarizing film.
- the polarizing film generally used has a transparent protective film on one or both sides of a polarizer.
- the polarizer is not particularly limited, and various polarizers can be used.
- dichroic substances such as iodine and dichroic dyes are added to hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and partially saponified ethylene-vinyl acetate copolymer films.
- Polyene-based oriented films such as those obtained by adsorbing and uniaxially stretching, dehydrated polyvinyl alcohol and dehydrochlorinated polyvinyl chloride films, and the like can be mentioned.
- a polarizer composed of a polyvinyl alcohol film and a dichroic substance such as iodine is suitable.
- the thickness of these polarizers is not particularly limited, it is generally about 80 ⁇ m or less.
- a thin polarizer having a thickness of 10 ⁇ m or less can be used as the polarizer. From the viewpoint of thinning, the thickness is preferably 1 to 7 ⁇ m. Such a thin polarizer has less unevenness in thickness, is excellent in visibility, is excellent in durability due to little dimensional change, and is preferable in that the thickness of the polarizing film can be reduced.
- thermoplastic resin that is excellent in transparency, mechanical strength, thermal stability, water barrier properties, isotropy, etc. is used as the material constituting the transparent protective film.
- thermoplastic resins include cellulose resins such as triacetyl cellulose, polyester resins, polyethersulfone resins, polysulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, (meth)acrylic resins, cyclic Polyolefin resins (norbornene-based resins), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof.
- cellulose resins such as triacetyl cellulose, polyester resins, polyethersulfone resins, polysulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, (meth)acrylic resins, cyclic Polyolefin resins (norbornene-based resins
- a transparent protective film is attached to one side of the polarizer with an adhesive layer, and a transparent protective film such as (meth)acrylic, urethane, acrylic urethane, epoxy, or silicone film is attached to the other side of the polarizer.
- a transparent protective film such as (meth)acrylic, urethane, acrylic urethane, epoxy, or silicone film is attached to the other side of the polarizer.
- a thermosetting resin such as a system or a UV curable resin can be used.
- One or more of any suitable additives may be contained in the transparent protective film.
- the adhesive used for bonding the polarizer and the transparent protective film is not particularly limited as long as it is optically transparent. water-based adhesives or radical curing adhesives are preferred.
- the thickness of the polarizing film is preferably 100 ⁇ m or less, more preferably 90 ⁇ m or less, even more preferably 75 ⁇ m or less, and even more preferably 60 ⁇ m or less, from the viewpoint of thinning.
- the peel force when peeling the separator from the pressure-sensitive adhesive layer is preferably 0.12 N/50 mm or less, and more preferably 0.12 N/50 mm or less, from the viewpoint of easy peelability of the separator. is 0.10 N/50 mm or less, more preferably 0.08 N/50 mm or less.
- the polarizing film with an adhesive layer having the separator of the present invention has an adhesive layer with excellent high temperature durability, it is suitable for image display devices used in high temperature environments, such as in-vehicle image display devices. used for
- ⁇ Preparation of polarizer thickness 12 ⁇ m>
- the PVA-based resin film was stretched in an aqueous solution containing 4% by weight of hexaboric acid and 5% by weight of potassium iodide so that the length of the PVA-based resin film was 6 times its original length. Furthermore, after performing an iodine ion impregnation treatment with an aqueous solution of 3% by weight of potassium iodide (iodine impregnation bath), it was dried in an oven at 60° C. for 4 minutes to obtain a polarizer with a thickness of 12 ⁇ m.
- a saponified triacetyl cellulose film having a thickness of 25 ⁇ m was used as the base film.
- the moisture permeability of the base film was 1200 g/m 2 ⁇ 24 h.
- the resulting transparent protective film with a surface treatment layer had a thickness of 32 ⁇ m and a moisture permeability of 400 g/m 2 ⁇ 24 h.
- ⁇ Second transparent protective film> A cyclic polyolefin film (manufactured by Nippon Zeon Co., Ltd.: ZEONOR) having a thickness of 13 ⁇ m was subjected to corona treatment and used. The moisture permeability of the film was 12 g/m 2 ⁇ 24 h.
- polarizing film ⁇ Preparation of polarizing film> While applying a polyvinyl alcohol-based adhesive to both sides of the polarizer (thickness 12 ⁇ m) so that the thickness of the water-based adhesive layer is 0.1 ⁇ m, the first transparent protective film (no surface treatment layer is provided side) and the second transparent protective film, and dried at 50° C. for 5 minutes to prepare a polarizing film (thickness: 57 ⁇ m).
- a cross-linking agent based on a compound having an isocyanate group manufactured by Nippon Polyurethane Co., Ltd., trade name “Coronate L”
- KMB-403 ⁇ -glycidoxypropyltrimethoxysilane
- Lithium bis(trifluoromethanesulfonyl)imide manufactured by Mitsubishi Materials Electronic Chemicals Co., Ltd. was blended in this order to prepare an adhesive composition (A-1). Further, pressure-sensitive adhesive compositions (A-2) to (A-4) were prepared in the same manner as described above, except that the amount of the conductive agent was changed to 6 parts, 0.3 parts, and 0 parts.
- ⁇ Preparation of adhesive composition (B)> Per 100 parts of the solid content of the acrylic polymer solution (B), isocyanate cross-linking agent (Mitsui Chemical Takenate D160N, trimethylolpropane hexamethylene diisocyanate) 0.2 parts, benzoyl peroxide (NOF Co., Ltd. Nyper BMT) 0.2 parts, as a conductive agent, lithium bis (trifluoromethanesulfonyl) imide (manufactured by Mitsubishi Materials Electronic Chemicals Co., Ltd.) 6 parts, and an acetoacetyl group-containing silane coupling agent (trade name: A-100, Soken Chemical Co., Ltd.) was blended to prepare an adhesive composition (B).
- isocyanate cross-linking agent Mitsubishi Materials Electronic Chemicals Co., Ltd. Nyper BMT
- oligomer prevention layer As a silica-based material, organosiloxane (Ethyl Silicate 48: Colcoat Co.) was diluted with isopropyl alcohol to a solid concentration of 1% to prepare a coating liquid. The obtained coating solution was applied on a polyester film (thickness: 38 ⁇ m) as a base film by a gravure coater so that the thickness after drying was 50 nm, and then dried at 120° C. for 30 seconds to prevent oligomers. formed a layer.
- organosiloxane Ether Silicate 48: Colcoat Co.
- the obtained solution of the silicone-based release agent was applied on the oligomer-preventing layer by a gravure coater so that the thickness after drying was 120 nm, and then dried at 120°C for 30 seconds to form a release layer.
- a separator X having a configuration of polyester film/oligomer prevention layer/releasing layer was produced.
- the content of the reactive silicone resin is 60% by mass
- the content of the non-reactive silicone resin is 100% by mass in the total content of the reactive silicone resin and the non-reactive silicone resin. is 40% by mass.
- oligomer prevention layer As a silica-based material, organosiloxane (Ethyl Silicate 48: Colcoat Co.) was diluted with isopropyl alcohol to a solid concentration of 1% to prepare a coating liquid. The obtained coating solution was applied on a polyester film (thickness: 38 ⁇ m) as a base film by a gravure coater so that the thickness after drying was 50 nm, and then dried at 120° C. for 30 seconds to prevent oligomers. formed a layer.
- organosiloxane Ether Silicate 48: Colcoat Co.
- Example 1 Preparation of a polarizing film with a pressure-sensitive adhesive layer having a separator>
- the pressure-sensitive adhesive composition (A-1) is uniformly applied to the surface of the release layer of the separator X with a fountain coater, dried in an air circulation constant temperature oven at 155 ° C. for 2 minutes, and a pressure-sensitive adhesive layer having a thickness of 20 ⁇ m. was formed to prepare a pressure-sensitive adhesive layer with a separator. Then, the pressure-sensitive adhesive layer of the prepared pressure-sensitive adhesive layer with a separator was attached to the second transparent protective film of the prepared polarizing film to prepare a polarizing film with a pressure-sensitive adhesive layer having a separator.
- Examples 2-4, Comparative Examples 1-5 Preparation of a polarizing film with a pressure-sensitive adhesive layer having a separator> A polarizing film with a pressure-sensitive adhesive layer having a separator was produced in the same manner as in Example 1 except that the pressure-sensitive adhesive composition and separator shown in Table 1 were used.
- a sample was prepared by cutting the produced polarizing film with an adhesive layer into a size of 120 mm long ⁇ 25 mm wide.
- the sample was attached to an alkali-free glass plate (manufactured by Corning, EG-XG) with a thickness of 0.7 mm using a laminator, and then autoclaved at 50 ° C. and 5 atm for 15 minutes. , the adhesion of such samples was measured.
- the adhesive strength is measured by peeling off such a sample with a tensile tester (Autograph SHIMAZUAG-1 1OKN) at a peeling angle of 90 ° and a peeling speed of 300 mm / min (N / 25 mm, measuring length 80 mm). I asked for it.
- the measurement was sampled 200 times at an interval of 1 time/0.5 s, and the average value was used as the measured value.
- the number of samples was 3.
- the produced polarizing film with an adhesive layer having a separator was cut into a size of 50 mm ⁇ 100 mm to obtain a measurement sample. With the surface-treated side of the measurement sample facing downward, it was attached to a flat peeling jig via a double-sided adhesive tape. Next, the separator was peeled off 10 mm from the surface of the adhesive layer, the peeled separator was chucked, and pulled using a tensile tester, and the peel force (N / 50 mm) was measured (pulling direction: on the surface of the polarizing film 180°, tension speed: 300 mm/min).
- the surface resistance value ( ⁇ / ⁇ ) of the adhesive layer was measured using MCP-HT450 manufactured by Mitsubishi Chemical Analytic Tech. Moreover, it evaluated by the following reference
- the polarizing films with adhesive layers having the separators of Examples 1 to 4 have a low elastic modulus of the release layer, a low peeling force when peeling the separator from the adhesive layer, and easy release of the separator. and the high-temperature durability of the pressure-sensitive adhesive layer are both excellent.
- the adhesive layer-attached polarizing films having the separators of Comparative Examples 1 to 4 had a high elastic modulus of the release layer, a high peeling force when peeling the separator from the adhesive layer, and poor separator releasability. I know there is.
- the pressure-sensitive adhesive layer-attached polarizing film having the separator of Comparative Example 5 has a low content of the carboxy group-containing monomer contained in the base polymer of the pressure-sensitive adhesive layer, so that the high-temperature durability of the pressure-sensitive adhesive layer is inferior. Recognize.
- the pressure-sensitive adhesive layer-attached polarizing film having the separator of the present invention is suitably used for an image display device used in a high-temperature environment, for example, an in-vehicle image display device.
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Abstract
The purpose of the present invention is to provide an adhesive layer-attached polarizing film having a separator, whereby both easy peelability of the separator and high temperature durability of the adhesive layer are achieved. In the adhesive layer-attached polarizing film having a separator according to the present invention, an adhesive layer with a separator comprises an adhesive layer on the separator and is provided on one or both sides of a polarizing film. The separator has a release layer on a base material film. The release layer contains a reactive silicone resin having a reactive functional group, and a non-reactive silicone resin having a weight average molecular weight of 400,000 or greater. In 100 mass% of the total content of the reactive silicone resin and the non-reactive silicone resin, the content of the reactive silicone resin is 50-70 mass%, and the content of the non-reactive silicone resin is 30-50 mass%. The modulus of elasticity of the release layer is less than 1.5 MPa. The adhesive layer is provided on the release layer, and the adhesive layer is characterized in containing a base polymer that contains a carboxyl group-containing monomer 0.5 mass% or greater as a monomer unit.
Description
本発明は、セパレータを有する粘着剤層付き偏光フィルムに関する。
The present invention relates to a polarizing film with a pressure-sensitive adhesive layer having a separator.
液晶表示装置等の画像表示装置には、偏光フィルムが用いられる。偏光フィルムを液晶パネル等の表示パネルに貼着する際には、通常、粘着剤が使用される。一般的に、偏光フィルムを貼着させるのに乾燥工程を必要としないこと等のメリットを有することから、粘着剤が偏光フィルムの片側に予め粘着剤層として設けられた、粘着剤層付き偏光フィルムが用いられる。また、粘着剤層付き偏光フィルムは、通常、貼着前の粘着剤層を保護するために、粘着剤層表面にセパレータ（離型フィルム又は剥離ライナーともいう）が設けられる。
Polarizing films are used in image display devices such as liquid crystal display devices. When sticking a polarizing film on a display panel such as a liquid crystal panel, an adhesive is usually used. A polarizing film with an adhesive layer, in which an adhesive is provided in advance as an adhesive layer on one side of the polarizing film, because it generally has the advantage of not requiring a drying process for attaching the polarizing film. is used. In addition, the pressure-sensitive adhesive layer-attached polarizing film is usually provided with a separator (also referred to as release film or release liner) on the surface of the pressure-sensitive adhesive layer in order to protect the pressure-sensitive adhesive layer before attachment.
近年、粘着剤層付き偏光フィルムは薄型化しており、コシがないため、粘着剤層からセパレータを剥離し難いという問題が生じている。そのため、セパレータの軽剥離化が求められている。一方、粘着剤層は、導電性や耐久性などの機能性が要求されており、セパレータの軽剥離化と粘着剤層の機能性を両立した、セパレータを有する粘着剤層付き偏光フィルムの開発が進められている。
In recent years, the polarizing film with an adhesive layer has become thinner, and there is a problem that it is difficult to peel off the separator from the adhesive layer because it does not have stiffness. Therefore, there is a demand for easy release of the separator. On the other hand, the adhesive layer is required to have functionality such as conductivity and durability, and development of a polarizing film with an adhesive layer that has a separator that achieves both easy release of the separator and the functionality of the adhesive layer is underway. is underway.
例えば、特許文献１では、剥離速度依存性を最小限に抑えることを可能にし、離型性良好、かつ移行性の低い基材レス両面粘着シート用ポリエステルフィルムであって、
アルケニル基およびアルキル基を官能基として有する反応性シリコーン樹脂、質量平均分子量４０００００以上の未反応性シリコーン樹脂、および白金系触媒を含有するシリコーン系離型層を有することを特徴とするポリエステルフィルムが提案されている。 For example, in Patent Document 1, a polyester film for a substrate-less double-sided pressure-sensitive adhesive sheet that can minimize peel speed dependency, has good releasability, and has low migration,
A polyester film characterized by having a reactive silicone resin having an alkenyl group and an alkyl group as functional groups, an unreactive silicone resin having a mass average molecular weight of 400,000 or more, and a silicone release layer containing a platinum catalyst is proposed. It is
アルケニル基およびアルキル基を官能基として有する反応性シリコーン樹脂、質量平均分子量４０００００以上の未反応性シリコーン樹脂、および白金系触媒を含有するシリコーン系離型層を有することを特徴とするポリエステルフィルムが提案されている。 For example, in Patent Document 1, a polyester film for a substrate-less double-sided pressure-sensitive adhesive sheet that can minimize peel speed dependency, has good releasability, and has low migration,
A polyester film characterized by having a reactive silicone resin having an alkenyl group and an alkyl group as functional groups, an unreactive silicone resin having a mass average molecular weight of 400,000 or more, and a silicone release layer containing a platinum catalyst is proposed. It is
また、特許文献２では、非常に小さな剥離力を示し、超軽剥離シートとして使用することが可能な剥離シートであって、
基材と、前記基材の少なくとも一方の面側に設けられた剥離剤層とを備えており、
前記基材が、プラスチックフィルムから構成され、
前記剥離剤層が、重量平均分子量が５０００以上、１０００００以下であるポリオルガノシロキサンを含有する剥離剤組成物から形成され、
前記剥離剤層の厚さが、０．３μｍ以上、１．０μｍ以下であることを特徴とする剥離シートが提案されている。 Further, in Patent Document 2, a release sheet that exhibits a very small release force and can be used as an ultra-light release sheet,
A base material and a release agent layer provided on at least one side of the base material,
The substrate is made of a plastic film,
The release agent layer is formed from a release agent composition containing a polyorganosiloxane having a weight average molecular weight of 5000 or more and 100000 or less,
A release sheet has been proposed in which the release agent layer has a thickness of 0.3 μm or more and 1.0 μm or less.
基材と、前記基材の少なくとも一方の面側に設けられた剥離剤層とを備えており、
前記基材が、プラスチックフィルムから構成され、
前記剥離剤層が、重量平均分子量が５０００以上、１０００００以下であるポリオルガノシロキサンを含有する剥離剤組成物から形成され、
前記剥離剤層の厚さが、０．３μｍ以上、１．０μｍ以下であることを特徴とする剥離シートが提案されている。 Further, in Patent Document 2, a release sheet that exhibits a very small release force and can be used as an ultra-light release sheet,
A base material and a release agent layer provided on at least one side of the base material,
The substrate is made of a plastic film,
The release agent layer is formed from a release agent composition containing a polyorganosiloxane having a weight average molecular weight of 5000 or more and 100000 or less,
A release sheet has been proposed in which the release agent layer has a thickness of 0.3 μm or more and 1.0 μm or less.
しかし、特許文献１に記載のシリコーン系離型層又は特許文献２に記載の剥離剤層を有するセパレータを用いても、薄型化した粘着剤層付き偏光フィルムの粘着剤層からセパレータを剥離し難いという問題は解決できなかった。
However, even if a separator having a silicone-based release layer described in Patent Document 1 or a release agent layer described in Patent Document 2 is used, it is difficult to separate the separator from the adhesive layer of the thin polarizing film with an adhesive layer. problem could not be solved.
本発明は、セパレータの軽剥離性と粘着剤層の高温耐久性を両立した、セパレータを有する粘着剤層付き偏光フィルムを提供することを目的とする。
An object of the present invention is to provide a polarizing film with a pressure-sensitive adhesive layer having a separator that achieves both easy peelability of the separator and high-temperature durability of the pressure-sensitive adhesive layer.
本発明者らは前記課題を解決すべく鋭意検討を重ねた結果、下記のセパレータを有する粘着剤層付き偏光フィルムにより上記課題を解決できることを見出し、本発明を完成するに至った。
As a result of extensive studies aimed at solving the above problems, the present inventors found that the above problems can be solved by a polarizing film with an adhesive layer having the following separator, and completed the present invention.
本発明は、セパレータ上に粘着剤層を有するセパレータ付き粘着剤層が偏光フィルムの片面又は両面に設けられている、セパレータを有する粘着剤層付き偏光フィルムであって、
前記セパレータは、基材フィルム上に離型層を有し、
前記離型層は、反応性官能基を有する反応性シリコーン樹脂、及び重量平均分子量が４０万以上の非反応性シリコーン樹脂を含有し、
前記反応性シリコーン樹脂と前記非反応性シリコーン樹脂の合計含有量１００質量％中、前記反応性シリコーン樹脂の含有量が５０～７０質量％、前記非反応性シリコーン樹脂の含有量が３０～５０質量％であり、
前記離型層の弾性率が１．５ＭＰａ未満であり、
前記粘着剤層は、前記離型層上に設けられており、
前記粘着剤層は、モノマー単位としてカルボキシ基含有モノマーを０．５質量％以上含有するベースポリマーを含有することを特徴とするセパレータを有する粘着剤層付き偏光フィルム、に関する。 The present invention is a polarizing film with a pressure-sensitive adhesive layer having a separator, wherein the pressure-sensitive adhesive layer with a separator having a pressure-sensitive adhesive layer on the separator is provided on one or both sides of the polarizing film,
The separator has a release layer on the base film,
The release layer contains a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more,
The content of the reactive silicone resin is 50 to 70% by mass, and the content of the non-reactive silicone resin is 30 to 50% by mass, based on the total content of 100% by mass of the reactive silicone resin and the non-reactive silicone resin. % and
The release layer has an elastic modulus of less than 1.5 MPa,
The adhesive layer is provided on the release layer,
The pressure-sensitive adhesive layer-attached polarizing film has a separator, wherein the pressure-sensitive adhesive layer contains a base polymer containing 0.5% by mass or more of a carboxy group-containing monomer as a monomer unit.
前記セパレータは、基材フィルム上に離型層を有し、
前記離型層は、反応性官能基を有する反応性シリコーン樹脂、及び重量平均分子量が４０万以上の非反応性シリコーン樹脂を含有し、
前記反応性シリコーン樹脂と前記非反応性シリコーン樹脂の合計含有量１００質量％中、前記反応性シリコーン樹脂の含有量が５０～７０質量％、前記非反応性シリコーン樹脂の含有量が３０～５０質量％であり、
前記離型層の弾性率が１．５ＭＰａ未満であり、
前記粘着剤層は、前記離型層上に設けられており、
前記粘着剤層は、モノマー単位としてカルボキシ基含有モノマーを０．５質量％以上含有するベースポリマーを含有することを特徴とするセパレータを有する粘着剤層付き偏光フィルム、に関する。 The present invention is a polarizing film with a pressure-sensitive adhesive layer having a separator, wherein the pressure-sensitive adhesive layer with a separator having a pressure-sensitive adhesive layer on the separator is provided on one or both sides of the polarizing film,
The separator has a release layer on the base film,
The release layer contains a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more,
The content of the reactive silicone resin is 50 to 70% by mass, and the content of the non-reactive silicone resin is 30 to 50% by mass, based on the total content of 100% by mass of the reactive silicone resin and the non-reactive silicone resin. % and
The release layer has an elastic modulus of less than 1.5 MPa,
The adhesive layer is provided on the release layer,
The pressure-sensitive adhesive layer-attached polarizing film has a separator, wherein the pressure-sensitive adhesive layer contains a base polymer containing 0.5% by mass or more of a carboxy group-containing monomer as a monomer unit.
前記粘着剤層は、導電剤を含有することが好ましい。
The adhesive layer preferably contains a conductive agent.
また、前記粘着剤層の表面抵抗値は、１．０×１０１２Ω／□以下であることが好ましい。
Moreover, the surface resistance value of the pressure-sensitive adhesive layer is preferably 1.0×10 12 Ω/□ or less.
また、前記粘着剤層から前記セパレータを剥離する際の剥離力は、０．１２Ｎ／５０ｍｍ以下であることが好ましい。
Also, the peeling force when peeling the separator from the pressure-sensitive adhesive layer is preferably 0.12 N/50 mm or less.
また、前記偏光フィルムの厚みは、１００μｍ以下であることが好ましい。
Also, the thickness of the polarizing film is preferably 100 μm or less.
本発明のセパレータは、反応性官能基を有する反応性シリコーン樹脂、及び重量平均分子量が４０万以上の非反応性シリコーン樹脂を特定の割合で含有し、かつ弾性率が１．５ＭＰａ未満である離型層を有しているため、薄型化した粘着剤層付き偏光フィルムであっても、前記粘着剤層からセパレータを容易に剥離することができる。また、本発明の粘着剤層は、モノマー単位としてカルボキシ基含有モノマーを０．５質量％以上含有するベースポリマーを含有しているため、高温耐久性に優れている。前記セパレータと前記粘着剤層を併用することにより、セパレータの軽剥離性と粘着剤層の高温耐久性を両立した、セパレータを有する粘着剤層付き偏光フィルムが得られる。
The separator of the present invention contains a specific proportion of a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more, and has an elastic modulus of less than 1.5 MPa. Since the polarizing film with a pressure-sensitive adhesive layer is thinned, the separator can be easily peeled off from the pressure-sensitive adhesive layer due to the presence of the mold layer. Moreover, since the pressure-sensitive adhesive layer of the present invention contains a base polymer containing 0.5% by mass or more of a carboxy group-containing monomer as a monomer unit, it is excellent in high temperature durability. By using the separator and the pressure-sensitive adhesive layer in combination, a polarizing film with a pressure-sensitive adhesive layer having a separator that achieves both easy peelability of the separator and high-temperature durability of the pressure-sensitive adhesive layer can be obtained.
本発明のセパレータを有する粘着剤層付き偏光フィルムは、セパレータ上に粘着剤層を有するセパレータ付き粘着剤層が偏光フィルムの片面又は両面に設けられているものである。以下、各構成部材について詳細に説明する。
The polarizing film with an adhesive layer having a separator of the present invention is a polarizing film in which an adhesive layer with a separator having an adhesive layer on a separator is provided on one or both sides of the polarizing film. Each component will be described in detail below.
＜セパレータ付き粘着剤層＞
本発明のセパレータ付き粘着剤層は、セパレータ上に粘着剤層を有するものであり、前記セパレータは、基材フィルム上に離型層を有する。前記粘着剤層は、前記離型層上に設けられている。また、前記セパレータは、前記基材フィルムと前記離型層との間にオリゴマー防止層を有していてもよい。 <Adhesive layer with separator>
The pressure-sensitive adhesive layer with a separator of the present invention has a pressure-sensitive adhesive layer on a separator, and the separator has a release layer on a base film. The adhesive layer is provided on the release layer. Further, the separator may have an oligomer prevention layer between the base film and the release layer.
本発明のセパレータ付き粘着剤層は、セパレータ上に粘着剤層を有するものであり、前記セパレータは、基材フィルム上に離型層を有する。前記粘着剤層は、前記離型層上に設けられている。また、前記セパレータは、前記基材フィルムと前記離型層との間にオリゴマー防止層を有していてもよい。 <Adhesive layer with separator>
The pressure-sensitive adhesive layer with a separator of the present invention has a pressure-sensitive adhesive layer on a separator, and the separator has a release layer on a base film. The adhesive layer is provided on the release layer. Further, the separator may have an oligomer prevention layer between the base film and the release layer.
＜基材フィルム＞
前記基材フィルムとしては、プラスチックフィルムを用いることができる。プラスチックフィルムとしては、ポリエチレンフィルム、ポリプロピレンフィルム、ポリブテンフィルム、ポリブタジエンフィルム、ポリメチルペンテンフィルム等のポリオレフィンフィルム；ポリ塩化ビニルフィルム、塩化ビニル共重合体フィルム等の塩化ビニル系フィルム；ポリエチレンテレフタレートフィルム、ポリブチレンテレフタレートフィルム、ポリナフチレンテレフタレートフィルム等のポリエステルフィルム；その他、ポリウレタンフィルム、エチレン－酢酸ビニル共重合体フィルム等が挙げられる。前記プラスチックフィルムのうち、ポリエステルフィルムを用いることが好ましい。 <Base film>
A plastic film can be used as the base film. Examples of plastic films include polyolefin films such as polyethylene film, polypropylene film, polybutene film, polybutadiene film and polymethylpentene film; vinyl chloride films such as polyvinyl chloride film and vinyl chloride copolymer film; polyethylene terephthalate film and polybutylene. Polyester films such as terephthalate films and polynaphthylene terephthalate films; other examples include polyurethane films and ethylene-vinyl acetate copolymer films. Among the plastic films, it is preferable to use a polyester film.
前記基材フィルムとしては、プラスチックフィルムを用いることができる。プラスチックフィルムとしては、ポリエチレンフィルム、ポリプロピレンフィルム、ポリブテンフィルム、ポリブタジエンフィルム、ポリメチルペンテンフィルム等のポリオレフィンフィルム；ポリ塩化ビニルフィルム、塩化ビニル共重合体フィルム等の塩化ビニル系フィルム；ポリエチレンテレフタレートフィルム、ポリブチレンテレフタレートフィルム、ポリナフチレンテレフタレートフィルム等のポリエステルフィルム；その他、ポリウレタンフィルム、エチレン－酢酸ビニル共重合体フィルム等が挙げられる。前記プラスチックフィルムのうち、ポリエステルフィルムを用いることが好ましい。 <Base film>
A plastic film can be used as the base film. Examples of plastic films include polyolefin films such as polyethylene film, polypropylene film, polybutene film, polybutadiene film and polymethylpentene film; vinyl chloride films such as polyvinyl chloride film and vinyl chloride copolymer film; polyethylene terephthalate film and polybutylene. Polyester films such as terephthalate films and polynaphthylene terephthalate films; other examples include polyurethane films and ethylene-vinyl acetate copolymer films. Among the plastic films, it is preferable to use a polyester film.
前記基材フィルムの厚みは、通常、５～２００μｍであり、好ましくは５～１００μｍ、より好ましくは１０～５０μｍである。前記基材フィルムは、コロナ処理、プラズマ処理等の表面処理が施されていてもよい。
The thickness of the base film is usually 5-200 μm, preferably 5-100 μm, more preferably 10-50 μm. The base film may be subjected to surface treatment such as corona treatment or plasma treatment.
＜離型層＞
前記離型層は、粘着剤層からの剥離性を高めるために設けられる。前記離型層は、シリコーン系離型剤により形成されており、前記シリコーン系離型剤は、反応性官能基を有する反応性シリコーン樹脂、及び重量平均分子量が４０万以上の非反応性シリコーン樹脂を含有する。反応性官能基を有する反応性シリコーン樹脂を用いることにより、加熱又は活性エネルギー線照射により、離型層中に反応性官能基を介した架橋構造を形成することができ、離型層の弾性率を目的とする範囲に調整し易くなる。また、重量平均分子量が４０万以上の非反応性シリコーン樹脂を用いることにより、軽剥離性を付与することができる。前記離型層は、基材フィルム又はオリゴマー防止層の上に、塗布層として形成することができる。また、前記離型層は、転着によっても形成できる。 <Release layer>
The release layer is provided to enhance releasability from the pressure-sensitive adhesive layer. The release layer is formed of a silicone-based release agent, and the silicone-based release agent includes a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more. contains By using a reactive silicone resin having a reactive functional group, a crosslinked structure can be formed in the release layer via the reactive functional group by heating or irradiation with an active energy ray, and the elastic modulus of the release layer can be easily adjusted to the desired range. In addition, by using a non-reactive silicone resin having a weight average molecular weight of 400,000 or more, it is possible to impart light releasability. The release layer can be formed as a coating layer on the base film or the oligomer prevention layer. The release layer can also be formed by transfer bonding.
前記離型層は、粘着剤層からの剥離性を高めるために設けられる。前記離型層は、シリコーン系離型剤により形成されており、前記シリコーン系離型剤は、反応性官能基を有する反応性シリコーン樹脂、及び重量平均分子量が４０万以上の非反応性シリコーン樹脂を含有する。反応性官能基を有する反応性シリコーン樹脂を用いることにより、加熱又は活性エネルギー線照射により、離型層中に反応性官能基を介した架橋構造を形成することができ、離型層の弾性率を目的とする範囲に調整し易くなる。また、重量平均分子量が４０万以上の非反応性シリコーン樹脂を用いることにより、軽剥離性を付与することができる。前記離型層は、基材フィルム又はオリゴマー防止層の上に、塗布層として形成することができる。また、前記離型層は、転着によっても形成できる。 <Release layer>
The release layer is provided to enhance releasability from the pressure-sensitive adhesive layer. The release layer is formed of a silicone-based release agent, and the silicone-based release agent includes a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more. contains By using a reactive silicone resin having a reactive functional group, a crosslinked structure can be formed in the release layer via the reactive functional group by heating or irradiation with an active energy ray, and the elastic modulus of the release layer can be easily adjusted to the desired range. In addition, by using a non-reactive silicone resin having a weight average molecular weight of 400,000 or more, it is possible to impart light releasability. The release layer can be formed as a coating layer on the base film or the oligomer prevention layer. The release layer can also be formed by transfer bonding.
反応性官能基を有する反応性シリコーン樹脂としては、例えば、反応性官能基を有するポリオルガノシロキサンが挙げられる。ポリオルガノシロキサンとしては、例えば、ポリジメチルシロキサン、ポリフェニルメチルシロキサン、ポリジフェニルシロキサン等が挙げられる。ポリオルガノシロキサンは、１種を単独で用いてもよく、２種以上を併用してもよい。反応性官能基は、ポリオルガノシロキサンの片末端に導入されていてもよく、両末端に導入されていてもよく、側鎖に導入されていてもよい。反応性官能基としては、例えば、炭素数２～１０のアルケニル基等が挙げられ、前記アルケニル基としては、例えば、ビニル基、アリル基、プロペニル基、ブテニル基、ペンテニル基、ヘキセニル基、ヘプテニル基、オクテニル基等が挙げられる。
Examples of reactive silicone resins having reactive functional groups include polyorganosiloxanes having reactive functional groups. Examples of polyorganosiloxane include polydimethylsiloxane, polyphenylmethylsiloxane, polydiphenylsiloxane, and the like. One type of polyorganosiloxane may be used alone, or two or more types may be used in combination. The reactive functional group may be introduced to one end of the polyorganosiloxane, may be introduced to both ends, or may be introduced to a side chain. Examples of reactive functional groups include alkenyl groups having 2 to 10 carbon atoms, and examples of the alkenyl groups include vinyl, allyl, propenyl, butenyl, pentenyl, hexenyl, and heptenyl groups. , an octenyl group, and the like.
反応性官能基を有する反応性シリコーン樹脂としては、例えば、信越化学工業（株）製のＫＳ－７７４、ＫＳ－７７５、ＫＳ－７７８、ＫＳ－７７９Ｈ、ＫＳ－８４７Ｈ、ＫＳ－８５６、Ｘ－６２－２４２２、Ｘ－６２－２４６１、Ｘ－６２－１３８７、Ｘ－６２－５０３９、Ｘ－６２－５０４０、ＫＮＳ－３０５１、Ｘ－６２－１４９６、ＫＮＳ３２０Ａ、ＫＮＳ３１６、Ｘ－６２－１５７４Ａ／Ｂ、Ｘ－６２－７０５２、Ｘ－６２－７０２８Ａ／Ｂ、Ｘ－６２－７６１９、Ｘ－６２－７２１３；モメンティブ・パフォーマンス・マテリアルズ製のＹＳＲ－３０２２、ＴＰＲ－６７００、ＴＰＲ－６７２０、ＴＰＲ－６７２１、ＴＰＲ６５００、ＴＰＲ６５０１、ＵＶ９３００、ＵＶ９４２５、ＸＳ５６－Ａ２７７５、ＸＳ５６－Ａ２９８２、ＸＳ５６－Ｃ６０１０、ＸＳ５６－Ｃ４８８０、ＵＶ９４３０、ＴＰＲ６６００、ＴＰＲ６６０４、ＴＰＲ６６０５；東レ・ダウコ－ニング（株）製のＳＲＸ３５７、ＳＲＸ２１１、ＳＤ７２２０、ＳＤ７２９２、ＬＴＣ７５０Ａ、ＬＴＣ７６０Ａ、ＬＴＣ３０３Ｅ、ＬＴＣ３００Ｂ、ＬＴＣ８５６、ＳＰ７２５９、ＢＹ２４－４６８Ｃ、ＳＰ７２４８Ｓ、ＢＹ２４－４５２、ＤＫＱ３－２０２、ＤＫＱ３－２０３、ＤＫＱ３－２０４、ＤＫＱ３－２０５、ＤＫＱ３－２１０等が挙げられる。
Examples of reactive silicone resins having a reactive functional group include KS-774, KS-775, KS-778, KS-779H, KS-847H, KS-856 and X-62 manufactured by Shin-Etsu Chemical Co., Ltd. -2422, X-62-2461, X-62-1387, X-62-5039, X-62-5040, KNS-3051, X-62-1496, KNS320A, KNS316, X-62-1574A/B, X -62-7052, X-62-7028A/B, X-62-7619, X-62-7213; YSR-3022, TPR-6700, TPR-6720, TPR-6721, TPR6500 manufactured by Momentive Performance Materials , TPR6501, UV9300, UV9425, XS56-A2775, XS56-A2982, XS56-C6010, XS56-C4880, UV9430, TPR6600, TPR6604, TPR6605; , LTC760A, LTC303E, LTC300B, LTC856, SP7259, BY24-468C, SP7248S, BY24-452, DKQ3-202, DKQ3-203, DKQ3-204, DKQ3-205, DKQ3-210 and the like.
重量平均分子量が４０万以上の非反応性シリコーン樹脂としては、例えば、重量平均分子量が４０万以上のポリオルガノシロキサンが挙げられ、好ましくは下記一般式（Ａ）で表されるポリオルガノシロキサンである。
Ｒ３ＳｉＯ（Ｒ２ＳｉＯ）ｎＳｉＲ３ （Ａ）
（式中、Ｒはそれぞれ独立に脂肪族不飽和結合を有さない炭化水素基であり、ｎは正の整数である。） Examples of non-reactive silicone resins having a weight average molecular weight of 400,000 or more include polyorganosiloxanes having a weight average molecular weight of 400,000 or more, preferably polyorganosiloxanes represented by the following general formula (A). .
R3SiO ( R2SiO ) nSiR3 ( A)
(Wherein, each R is independently a hydrocarbon group having no aliphatic unsaturation, and n is a positive integer.)
Ｒ３ＳｉＯ（Ｒ２ＳｉＯ）ｎＳｉＲ３ （Ａ）
（式中、Ｒはそれぞれ独立に脂肪族不飽和結合を有さない炭化水素基であり、ｎは正の整数である。） Examples of non-reactive silicone resins having a weight average molecular weight of 400,000 or more include polyorganosiloxanes having a weight average molecular weight of 400,000 or more, preferably polyorganosiloxanes represented by the following general formula (A). .
R3SiO ( R2SiO ) nSiR3 ( A)
(Wherein, each R is independently a hydrocarbon group having no aliphatic unsaturation, and n is a positive integer.)
非反応性シリコーン樹脂の重量平均分子量は、離型層に軽剥離性を付与する観点から、好ましくは５０万以上、より好ましくは６０万以上であり、また、離型層の弾性率が高くなることを抑制する観点から、好ましくは１００万以下、より好ましくは９０万以下である。なお、前記重量平均分子量は、ＧＰＣ（ゲル・パーミエーション・クロマトグラフィー）により測定し、ポリスチレン換算により算出された値をいう。
The weight-average molecular weight of the non-reactive silicone resin is preferably 500,000 or more, more preferably 600,000 or more, from the viewpoint of imparting easy release properties to the release layer, and increases the elastic modulus of the release layer. From the viewpoint of suppressing this, it is preferably 1,000,000 or less, more preferably 900,000 or less. The weight-average molecular weight is a value measured by GPC (gel permeation chromatography) and calculated by polystyrene conversion.
前記離型層において、離型層の弾性率を１．５ＭＰａ未満に調整して、離型層に優れた軽剥離性を付与する観点から、前記反応性シリコーン樹脂と前記非反応性シリコーン樹脂の合計含有量１００質量％中、前記反応性シリコーン樹脂の含有量は５０～７０質量％、前記非反応性シリコーン樹脂の含有量は３０～５０質量％であり、好ましくは前記反応性シリコーン樹脂の含有量は５５～６５質量％、前記非反応性シリコーン樹脂の含有量は３５～４５質量％であり、より好ましくは前記反応性シリコーン樹脂の含有量は５７～６３質量％、前記非反応性シリコーン樹脂の含有量は３７～４３質量％である。
In the release layer, the elastic modulus of the release layer is adjusted to less than 1.5 MPa, and from the viewpoint of imparting excellent light release properties to the release layer, the combination of the reactive silicone resin and the non-reactive silicone resin Of the total content of 100% by mass, the content of the reactive silicone resin is 50 to 70% by mass, and the content of the non-reactive silicone resin is 30 to 50% by mass. Preferably, the reactive silicone resin is contained. the content of the non-reactive silicone resin is 55-65% by mass, and the content of the non-reactive silicone resin is 35-45% by mass, more preferably the content of the reactive silicone resin is 57-63% by mass, the non-reactive silicone resin The content of is 37 to 43% by mass.
前記離型層は、前記シリコーン樹脂の他に、架橋剤、触媒、反応抑制剤、密着向上剤等を含有していてもよい。
The release layer may contain a cross-linking agent, a catalyst, a reaction inhibitor, an adhesion improver, etc., in addition to the silicone resin.
前記離型層は、例えば、上記材料を含む組成物を基材フィルム又はオリゴマー防止層上に、リバースグラビアコート、バーコート、ダイコート等の従来公知の塗布方式により塗布した後、通常、１２０～２００℃程度で３０秒～３０分間熱処理を施して硬化させることにより形成することができる。また、必要に応じて、熱処理と紫外線照射等の活性エネルギー線照射とを併用してもよい。
The release layer is usually 120 to 200 after coating a composition containing the above materials on a substrate film or oligomer prevention layer by a conventionally known coating method such as reverse gravure coating, bar coating, and die coating. C. for 30 seconds to 30 minutes for hardening. Further, if necessary, heat treatment and active energy ray irradiation such as ultraviolet irradiation may be used in combination.
前記離型層の厚みは、通常、１０～２０００ｎｍであり、好ましくは１０～１０００ｎｍであり、より好ましくは１０～５００ｎｍであり、さらに好ましくは５０～３００ｎｍである。
The thickness of the release layer is usually 10 to 2000 nm, preferably 10 to 1000 nm, more preferably 10 to 500 nm, still more preferably 50 to 300 nm.
前記離型層の弾性率は、離型層に優れた軽剥離性を付与する観点から、１．５ＭＰａ未満であり、好ましくは１．４ＭＰａ以下、より好ましくは１．３ＭＰａ以下、さらに好ましくは１．２ＭＰａ以下である。また、前記離型層の弾性率は、離型層の脱落防止の観点から、好ましくは０．５ＭＰａ以上、より好ましくは０．７５ＭＰａ以上、さらに好ましくは０．９ＭＰａ以上である。離型層の弾性率は、実施例に記載の方法で測定する。
The elastic modulus of the release layer is less than 1.5 MPa, preferably 1.4 MPa or less, more preferably 1.3 MPa or less, still more preferably 1, from the viewpoint of imparting excellent easy release properties to the release layer. .2 MPa or less. In addition, the elastic modulus of the release layer is preferably 0.5 MPa or more, more preferably 0.75 MPa or more, and still more preferably 0.9 MPa or more, from the viewpoint of preventing the release layer from coming off. The elastic modulus of the release layer is measured by the method described in Examples.
＜オリゴマー防止層＞
前記オリゴマー防止層は、基材フィルムに含まれるオリゴマーが粘着剤層に溶出することを防止するため機能層である。オリゴマー防止層の形成材料としては、無機物もしくは有機物、又はそれらの複合材料を用いることができる。無機物としては、シリカ系材料、あるいは金、銀、白金、パラジウム、銅、アルミニウム、ニッケル、クロム、チタン、鉄、コバルト又はスズやこれらの合金等からなる金属、あるいは酸化インジウム、酸化スズ、酸化チタン、酸化カドミウム又はこれらの混合物からなる金属酸化物、ヨウ化鋼等からなる他の金属化合物等が挙げられる。有機物としては、ポリビニルアルコール系樹脂、アクリル系樹脂、ウレタン系樹脂、メラミン系樹脂、ＵＶ硬化型樹脂、エポキシ系樹脂が挙げられる。また複合材料としては、前記有機物と、アルミナ、シリカ、マイカ等の無機粒子との混合物が挙げられる。 <Oligomer prevention layer>
The oligomer-preventing layer is a functional layer for preventing the oligomer contained in the base film from eluting into the pressure-sensitive adhesive layer. As a material for forming the oligomer-preventing layer, an inorganic material, an organic material, or a composite material thereof can be used. Examples of inorganic substances include silica-based materials, metals such as gold, silver, platinum, palladium, copper, aluminum, nickel, chromium, titanium, iron, cobalt, tin, and alloys thereof, indium oxide, tin oxide, and titanium oxide. , metal oxides such as cadmium oxide or mixtures thereof, and other metal compounds such as steel iodide. Examples of organic substances include polyvinyl alcohol-based resins, acrylic-based resins, urethane-based resins, melamine-based resins, UV-curable resins, and epoxy-based resins. Composite materials include mixtures of the above organic matter and inorganic particles such as alumina, silica, and mica.
前記オリゴマー防止層は、基材フィルムに含まれるオリゴマーが粘着剤層に溶出することを防止するため機能層である。オリゴマー防止層の形成材料としては、無機物もしくは有機物、又はそれらの複合材料を用いることができる。無機物としては、シリカ系材料、あるいは金、銀、白金、パラジウム、銅、アルミニウム、ニッケル、クロム、チタン、鉄、コバルト又はスズやこれらの合金等からなる金属、あるいは酸化インジウム、酸化スズ、酸化チタン、酸化カドミウム又はこれらの混合物からなる金属酸化物、ヨウ化鋼等からなる他の金属化合物等が挙げられる。有機物としては、ポリビニルアルコール系樹脂、アクリル系樹脂、ウレタン系樹脂、メラミン系樹脂、ＵＶ硬化型樹脂、エポキシ系樹脂が挙げられる。また複合材料としては、前記有機物と、アルミナ、シリカ、マイカ等の無機粒子との混合物が挙げられる。 <Oligomer prevention layer>
The oligomer-preventing layer is a functional layer for preventing the oligomer contained in the base film from eluting into the pressure-sensitive adhesive layer. As a material for forming the oligomer-preventing layer, an inorganic material, an organic material, or a composite material thereof can be used. Examples of inorganic substances include silica-based materials, metals such as gold, silver, platinum, palladium, copper, aluminum, nickel, chromium, titanium, iron, cobalt, tin, and alloys thereof, indium oxide, tin oxide, and titanium oxide. , metal oxides such as cadmium oxide or mixtures thereof, and other metal compounds such as steel iodide. Examples of organic substances include polyvinyl alcohol-based resins, acrylic-based resins, urethane-based resins, melamine-based resins, UV-curable resins, and epoxy-based resins. Composite materials include mixtures of the above organic matter and inorganic particles such as alumina, silica, and mica.
前記オリゴマー防止層は、シリカ系材料やポリビニルアルコール系樹脂を含む組成物から形成されることが好ましい。
The oligomer-preventing layer is preferably formed from a composition containing a silica-based material or a polyvinyl alcohol-based resin.
＜シリカ系材料＞
前記シリカ系材料としては、例えば、下記一般式（Ｉ）で表わされるオルガノシロキサンが挙げられる。
<Silica material>
Examples of the silica-based material include organosiloxanes represented by the following general formula (I).
前記シリカ系材料としては、例えば、下記一般式（Ｉ）で表わされるオルガノシロキサンが挙げられる。
Examples of the silica-based material include organosiloxanes represented by the following general formula (I).
前記一般式（Ｉ）中、Ｒ１及びＲ２は、それぞれ独立して、γ－グリシドキシプロピル基、３，４－エポキシシクロヘキシルエチル基等のようなエポキシ基を含有する有機基、又は、メトキシ基、エトキシ基等のアルコキシ基であり、Ｒ３はメトキシ基、エトキシ基等のアルコキシ基、又は下記一般式（ＩＩ）で示される基である。ｎ及びｍは、０～１０の整数である。
In the general formula (I), R 1 and R 2 are each independently an epoxy group-containing organic group such as a γ-glycidoxypropyl group, a 3,4-epoxycyclohexylethyl group, or It is an alkoxy group such as a methoxy group or an ethoxy group, and R3 is an alkoxy group such as a methoxy group or an ethoxy group, or a group represented by the following general formula (II). n and m are integers from 0 to 10;
前記一般式（ＩＩ）中、Ｒ４はＲ１基又はＲ２基と同じエポキシ基含有有機基又はアルコキシ基である。
In general formula (II), R4 is the same epoxy group-containing organic group or alkoxy group as R1 or R2 .
前記オルガノシロキサンの具体例としては、γ－グリシドキシプロピルトリメトキシシラン、２－（３，４－エポキシシクロヘキシル）エチルトリメトキシシラン、２－（３，４－エポキシシクロヘキシル）エチルトリエトキシシラン、５，６－エポキシシクロヘキシルトリエトキシシラン、テトラエトキシシラン等の単量体、及びこれら単量体もしくはこれら単量体の混合物の加水分解性生物（オリゴマー）が例示される。
Specific examples of the organosiloxane include γ-glycidoxypropyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 5 ,6-epoxycyclohexyltriethoxysilane, tetraethoxysilane and the like, and hydrolyzable products (oligomers) of these monomers or mixtures of these monomers.
また前記シリカ系材料としては、アミノ基を有するシラン化合物が挙げられる。前記アミノ基を有するシラン化合物として、下記一般式（ＩＩＩ）で表されるアルコキシシランが好ましい。
Ｙ－Ｒ－Ｓｉ－（Ｘ）３ （ＩＩＩ）
（前記一般式（ＩＩＩ）中、Ｙはアミノ基、Ｒはメチレン、エチレン、プロピレン等のアルキレン基、Ｘはメトキシ基、エトキシ基等のアルコキシ基、アルキル基、又はこれらの基を有する有機官能基を表し、少なくとも１つ以上はアルコキシ基である）。 Further, examples of the silica-based material include silane compounds having an amino group. As the silane compound having an amino group, an alkoxysilane represented by the following general formula (III) is preferable.
Y—R—Si—(X) 3 (III)
(In the general formula (III), Y is an amino group, R is an alkylene group such as methylene, ethylene, or propylene, X is an alkoxy group such as a methoxy group or an ethoxy group, an alkyl group, or an organic functional group having these groups. and at least one is an alkoxy group).
Ｙ－Ｒ－Ｓｉ－（Ｘ）３ （ＩＩＩ）
（前記一般式（ＩＩＩ）中、Ｙはアミノ基、Ｒはメチレン、エチレン、プロピレン等のアルキレン基、Ｘはメトキシ基、エトキシ基等のアルコキシ基、アルキル基、又はこれらの基を有する有機官能基を表し、少なくとも１つ以上はアルコキシ基である）。 Further, examples of the silica-based material include silane compounds having an amino group. As the silane compound having an amino group, an alkoxysilane represented by the following general formula (III) is preferable.
Y—R—Si—(X) 3 (III)
(In the general formula (III), Y is an amino group, R is an alkylene group such as methylene, ethylene, or propylene, X is an alkoxy group such as a methoxy group or an ethoxy group, an alkyl group, or an organic functional group having these groups. and at least one is an alkoxy group).
前記アミノ基を有するシラン化合物の具体例としては、Ｎ－β（アミノエチル）γ－アミノプロピルトリメトキシシラン、Ｎ－β（アミノエチル）γ－アミノプロピルトリエトキシシラン、Ｎ－β（アミノエチル）γ－アミノプロピルメチルジメトキシシラン、γ－アミノプロピルトリメトキシシラン、Ｎ－フェニル－γ－アミノプロピルトリメトキシシラン等が挙げられる。
Specific examples of the silane compound having an amino group include N-β (aminoethyl)γ-aminopropyltrimethoxysilane, N-β (aminoethyl)γ-aminopropyltriethoxysilane, N-β (aminoethyl) γ-aminopropylmethyldimethoxysilane, γ-aminopropyltrimethoxysilane, N-phenyl-γ-aminopropyltrimethoxysilane and the like.
その他、前記シリカ系材料としては、３－アクリロキシプロピルトリメトキシシラン、３－メタクリロキシプロピルトリエトキシシラン等の（メタ）アクリル基含有シラン化合物、３－イソシアネートプロピルトリエトキシシラン等のイソシアネート基含有シラン化合物等が挙げられる。
In addition, the silica-based materials include (meth)acryl group-containing silane compounds such as 3-acryloxypropyltrimethoxysilane and 3-methacryloxypropyltriethoxysilane, and isocyanate group-containing silanes such as 3-isocyanatopropyltriethoxysilane. compounds and the like.
前記シリカ系材料の具体的製品としては、信越化学工業社製のＫＲ－４０１Ｎ、Ｘ－４０－９２２７、Ｘ－４０－９２４７、ＫＲ－５１０、ＫＲ－９２１８、ＫＲ－２１３、ＫＲ－２１７、Ｘ－４１－１０５３、Ｘ－４０－１０５６、Ｘ－４１－１８０５、Ｘ－４１－１８１０、Ｘ－４０－２６５１、Ｘ－４０－２６５２Ｂ、Ｘ－４０－２６５５Ａ、Ｘ－４０－２７６１、Ｘ－４０－２６７２等が挙げられる。
Specific products of the silica-based material include KR-401N, X-40-9227, X-40-9247, KR-510, KR-9218, KR-213, KR-217, and X manufactured by Shin-Etsu Chemical Co., Ltd. -41-1053, X-40-1056, X-41-1805, X-41-1810, X-40-2651, X-40-2652B, X-40-2655A, X-40-2761, X-40 -2672 and the like.
前記シリカ系材料は、１種のみを用いてもよく、２種以上を用いてもよい。
Only one type of the silica-based material may be used, or two or more types may be used.
前記シリカ系材料によって形成するオリゴマー防止層には、必要に応じて、金属元素を有する有機化合物（金属キレート等の金属化合物）、触媒等を含有することができる。金属元素を有する金属有機化合物は、１種のみを用いてもよく、２種以上を用いてもよい。
The oligomer-preventing layer formed of the silica-based material can contain, if necessary, an organic compound having a metal element (a metal compound such as a metal chelate), a catalyst, or the like. Only one metal organic compound having a metal element may be used, or two or more thereof may be used.
前記金属元素を有する金属有機化合物の中でも、特にオリゴマー溶出防止性能が良好となる点でキレート構造を有するアルミニウム元素を有する有機化合物、チタン元素を有する有機化合物、ジルコニウム元素を有する有機化合物が好ましい。かかる化合物は、「架橋剤ハンドブック」（山下晋三、金子東助編者（株）大成社平成２年版）に具体的に記載されている。
Among the metal organic compounds containing metal elements, organic compounds containing an aluminum element having a chelate structure, organic compounds containing a titanium element, and organic compounds containing a zirconium element are preferable in terms of particularly good performance in preventing the elution of oligomers. Such compounds are specifically described in "Crosslinking Agent Handbook" (edited by Shinzo Yamashita and Tosuke Kaneko, Taiseisha Co., Ltd., 1990 edition).
前記シリカ系材料によって形成するオリゴマー防止層の形成は、前記シリカ系材料を、アルコール等の溶媒に溶解した溶液を、基材フィルムに塗布後、乾燥することにより行うことができる。前記シリカ系材料を溶解した溶液の濃度は特に制限されるわけではないが、０．１～４０重量％程度であるのが好ましい。塗布後の乾燥温度は特に限定されるわけでないが、１００～１５０℃程度であるのが好ましい。また、塗布後の乾燥時間は特に限定されるわけでないが、３０秒～３０分程度であるのが好ましい。
The oligomer-preventing layer formed from the silica-based material can be formed by applying a solution of the silica-based material dissolved in a solvent such as alcohol to the substrate film and then drying. Although the concentration of the solution in which the silica-based material is dissolved is not particularly limited, it is preferably about 0.1 to 40% by weight. Although the drying temperature after coating is not particularly limited, it is preferably about 100 to 150°C. Although the drying time after application is not particularly limited, it is preferably about 30 seconds to 30 minutes.
＜ポリビニルアルコール系樹脂を含む組成物＞
前記ポリビニルアルコール系樹脂としては、ポリビニルアルコールまたはその誘導体が挙げられる。ポリビニルアルコールの誘導体としては、ポリビニルホルマール、ポリビニルアセタール等があげられる他、エチレン、プロピレン等のオレフィン、アクリル酸、メタクリル酸、クロトン酸等の不飽和カルボン酸及びそのアルキルエステル、アクリルアミド等で変性したものが挙げられる。ポリビニルアルコール系樹脂は、１種のみを用いてもよく、２種以上を用いてもよい。 <Composition containing polyvinyl alcohol-based resin>
Examples of the polyvinyl alcohol-based resin include polyvinyl alcohol and derivatives thereof. Derivatives of polyvinyl alcohol include polyvinyl formal and polyvinyl acetal, as well as those modified with olefins such as ethylene and propylene, unsaturated carboxylic acids such as acrylic acid, methacrylic acid and crotonic acid, their alkyl esters, and acrylamide. are mentioned. Only one type of polyvinyl alcohol-based resin may be used, or two or more types may be used.
前記ポリビニルアルコール系樹脂としては、ポリビニルアルコールまたはその誘導体が挙げられる。ポリビニルアルコールの誘導体としては、ポリビニルホルマール、ポリビニルアセタール等があげられる他、エチレン、プロピレン等のオレフィン、アクリル酸、メタクリル酸、クロトン酸等の不飽和カルボン酸及びそのアルキルエステル、アクリルアミド等で変性したものが挙げられる。ポリビニルアルコール系樹脂は、１種のみを用いてもよく、２種以上を用いてもよい。 <Composition containing polyvinyl alcohol-based resin>
Examples of the polyvinyl alcohol-based resin include polyvinyl alcohol and derivatives thereof. Derivatives of polyvinyl alcohol include polyvinyl formal and polyvinyl acetal, as well as those modified with olefins such as ethylene and propylene, unsaturated carboxylic acids such as acrylic acid, methacrylic acid and crotonic acid, their alkyl esters, and acrylamide. are mentioned. Only one type of polyvinyl alcohol-based resin may be used, or two or more types may be used.
前記ポリビニルアルコール系樹脂の重合度は特に限定されるわけではないが、通常１００以上、好ましくは３００～４００００のものが好適に用いられる。一方、ポリビニルアルコール系樹脂のけん化度は特に限定されるわけではないが、７０モル％以上、好ましくは８０モル％以上、９９．９モル％以下のものが好適に用いられる。
Although the degree of polymerization of the polyvinyl alcohol resin is not particularly limited, it is usually 100 or more, preferably 300 to 40,000. On the other hand, although the degree of saponification of the polyvinyl alcohol resin is not particularly limited, one having a degree of saponification of 70 mol % or more, preferably 80 mol % or more and 99.9 mol % or less is preferably used.
前記ポリビニルアルコール系樹脂を含む組成物には、バインダーポリマーを含むことができる。バインダーポリマーとしては、ポリアクリルアミド、ポリアルキレングリコール、ポリアルキレンイミン、メチルセルロース、ヒドロキシセルロース、でんぷん類、ポリウレタン、ポリエステル、ポリアクリレート、塩素系ポリマー（ポリ塩化ビニル、塩化ビニル酢酸ビニル共重合体等）、ポリオレフィン等が挙げられる。それらの中でも、オリゴマー防止層を塗布延伸法により塗設する場合には、ノニオン系、カチオン系、両性系の水溶液または水分散体として使用可能な有機ポリマーが挙げられ、また、それらの中でもポリウレタン、ポリエステル、ポリアクリレートを使用した場合には、接着性が良好となる。これらのポリマーはそのモノマーの一成分としてノニオン、カチオン、または両性系の親水性成分を共重合することにより、親水性を付与し、水に分散させることが可能となる。
The composition containing the polyvinyl alcohol-based resin can contain a binder polymer. Binder polymers include polyacrylamide, polyalkylene glycol, polyalkyleneimine, methylcellulose, hydroxycellulose, starches, polyurethane, polyester, polyacrylate, chlorine-based polymers (polyvinyl chloride, vinyl chloride vinyl acetate copolymer, etc.), polyolefin etc. Among them, when the oligomer-preventing layer is applied by a coating-stretching method, nonionic, cationic, and amphoteric organic polymers that can be used as aqueous solutions or aqueous dispersions can be mentioned. Good adhesion is obtained when polyester or polyacrylate is used. By copolymerizing a nonionic, cationic, or amphoteric hydrophilic component as one component of the monomer, these polymers are imparted with hydrophilicity and can be dispersed in water.
前記ポリビニルアルコール系樹脂を含む組成物には、架橋剤を含むことができる。架橋剤としては、メチロール化またはアルキロール化した尿素系、メラミン系、グアナミン系、アクリルアミド系、ポリアミド系化合物、エポキシ化合物、アジリジン化合物、ブロックポリイソシアネート、シランカップリング剤、チタンカップリング剤、ジルコーアルミネートカップリング剤等が挙げられる。これらの架橋成分は、バインダーポリマーと予め結合していてもよい。
The composition containing the polyvinyl alcohol-based resin may contain a cross-linking agent. Examples of cross-linking agents include methylolated or alkylolated urea-based, melamine-based, guanamine-based, acrylamide-based, polyamide-based compounds, epoxy compounds, aziridine compounds, blocked polyisocyanates, silane coupling agents, titanium coupling agents, Zirco An aluminate coupling agent etc. are mentioned. These cross-linking components may be pre-bonded with the binder polymer.
前記ポリビニルアルコール系樹脂を含む組成物には、オリゴマー防止層の固着性、滑り性改良を目的として、無機系粒子を含むことができる。無機系粒子としては、シリカ、アルミナ、カオリン、炭酸カルシウム、酸化チタン、バリウム塩等が挙げられる。
The composition containing the polyvinyl alcohol-based resin may contain inorganic particles for the purpose of improving the adhesion and slipperiness of the oligomer-preventing layer. Examples of inorganic particles include silica, alumina, kaolin, calcium carbonate, titanium oxide, and barium salts.
前記オリゴマー防止層の形成は、前記ポリビニルアルコール系樹脂を含む組成物を、水やアルコール等の溶媒に溶解した溶液を、基材フィルムに塗布後、乾燥することにより行うことができる。また、乾燥の際に、延伸してもよい。前記ポリビニルアルコール系樹脂を含む組成物を溶解した溶液の濃度は特に制限されるわけではないが、０．１～４０重量％程度であるのが好ましい。塗布後の乾燥温度は特に限定されるわけでないが、６０～２００℃程度であるのが好ましい。また、塗布後の乾燥時間は特に限定されるわけでないが、３～６０秒程度であるのが好ましい。必要に応じて熱処理と紫外線照射等の活性エネルギー線照射とを併用してもよい。
The formation of the oligomer-preventing layer can be carried out by applying a solution obtained by dissolving the composition containing the polyvinyl alcohol resin in a solvent such as water or alcohol to the substrate film and then drying the solution. Moreover, you may extend|stretch in the case of drying. Although the concentration of the solution in which the composition containing the polyvinyl alcohol resin is dissolved is not particularly limited, it is preferably about 0.1 to 40% by weight. Although the drying temperature after coating is not particularly limited, it is preferably about 60 to 200°C. Also, the drying time after coating is not particularly limited, but it is preferably about 3 to 60 seconds. Heat treatment and active energy ray irradiation such as ultraviolet irradiation may be used in combination as necessary.
前記オリゴマー防止層におけるポリビニルアルコール系樹脂の含有量は特に限定されるものではないが、好ましくは１０～１００重量％、さらに好ましくは２０～９０重量％、最も好ましくは３０～８０重量％の範囲がよい。
The content of the polyvinyl alcohol-based resin in the oligomer-preventing layer is not particularly limited, but is preferably 10 to 100% by weight, more preferably 20 to 90% by weight, and most preferably 30 to 80% by weight. good.
前記オリゴマー防止層の形成方法は、特に限定されず、その形成材料により適宜に選択すればよく、塗布法、スプレー法、スピンコート法、インラインコート法等が用いられる。また、真空蒸着法、スパッタリング法、イオンプレーティング法、スプレー熱分解法、化学メッキ法、電気メッキ法等も用いることができる。
The method for forming the oligomer-preventing layer is not particularly limited, and may be appropriately selected depending on the material for forming it, and a coating method, a spray method, a spin coating method, an in-line coating method, or the like is used. Also, a vacuum vapor deposition method, a sputtering method, an ion plating method, a spray pyrolysis method, a chemical plating method, an electroplating method, or the like can be used.
前記オリゴマー防止層の厚さは、５～１００ｎｍの範囲で適宜に設定することが好ましく、１０～７０ｎｍであるのがより好ましい。
The thickness of the oligomer-preventing layer is preferably set appropriately in the range of 5 to 100 nm, more preferably 10 to 70 nm.
＜粘着剤層＞
前記粘着剤層は、粘着剤組成物から形成される。粘着剤組成物としては、ゴム系粘着剤組成物、アクリル系粘着剤組成物、シリコーン系粘着剤組成物、ウレタン系粘着剤組成物、ビニルアルキルエーテル系粘着剤組成物、ポリビニルアルコール系粘着剤組成物、ポリビニルピロリドン系粘着剤組成物、ポリアクリルアミド系粘着剤組成物、セルロース系粘着剤組成物等が挙げられる。粘着剤組成物は、ベースポリマーを含むことが好ましい。 <Adhesive layer>
The adhesive layer is formed from an adhesive composition. Examples of adhesive compositions include rubber-based adhesive compositions, acrylic adhesive compositions, silicone-based adhesive compositions, urethane-based adhesive compositions, vinyl alkyl ether-based adhesive compositions, and polyvinyl alcohol-based adhesive compositions. products, polyvinylpyrrolidone-based pressure-sensitive adhesive compositions, polyacrylamide-based pressure-sensitive adhesive compositions, cellulose-based pressure-sensitive adhesive compositions, and the like. The adhesive composition preferably contains a base polymer.
前記粘着剤層は、粘着剤組成物から形成される。粘着剤組成物としては、ゴム系粘着剤組成物、アクリル系粘着剤組成物、シリコーン系粘着剤組成物、ウレタン系粘着剤組成物、ビニルアルキルエーテル系粘着剤組成物、ポリビニルアルコール系粘着剤組成物、ポリビニルピロリドン系粘着剤組成物、ポリアクリルアミド系粘着剤組成物、セルロース系粘着剤組成物等が挙げられる。粘着剤組成物は、ベースポリマーを含むことが好ましい。 <Adhesive layer>
The adhesive layer is formed from an adhesive composition. Examples of adhesive compositions include rubber-based adhesive compositions, acrylic adhesive compositions, silicone-based adhesive compositions, urethane-based adhesive compositions, vinyl alkyl ether-based adhesive compositions, and polyvinyl alcohol-based adhesive compositions. products, polyvinylpyrrolidone-based pressure-sensitive adhesive compositions, polyacrylamide-based pressure-sensitive adhesive compositions, cellulose-based pressure-sensitive adhesive compositions, and the like. The adhesive composition preferably contains a base polymer.
＜ベースポリマー＞
前記ベースポリマーは、前記粘着剤組成物の種類に応じて粘着性のベースポリマーが選択される。 <Base polymer>
As the base polymer, an adhesive base polymer is selected according to the type of the adhesive composition.
前記ベースポリマーは、前記粘着剤組成物の種類に応じて粘着性のベースポリマーが選択される。 <Base polymer>
As the base polymer, an adhesive base polymer is selected according to the type of the adhesive composition.
前記ベースポリマーは、粘着剤層の高温耐久性を向上させる観点から、モノマー単位としてカルボキシ基含有モノマーを０．５質量％以上含有し、好ましくは１質量％以上、より好ましくは３質量％以上含有する。一方、前記ベースポリマーは、粘着剤層からセパレータを剥離する際の剥離力を低下させる観点から、モノマー単位としてカルボキシ基含有モノマーを、好ましくは１０質量％以下、よりに好ましくは８質量％以下、さらに好ましくは５質量％以下含有する。
From the viewpoint of improving the high-temperature durability of the pressure-sensitive adhesive layer, the base polymer contains 0.5% by mass or more, preferably 1% by mass or more, more preferably 3% by mass or more of a carboxy group-containing monomer as a monomer unit. do. On the other hand, from the viewpoint of reducing the peeling force when peeling the separator from the pressure-sensitive adhesive layer, the base polymer preferably contains 10% by mass or less, more preferably 8% by mass or less of a carboxy group-containing monomer as a monomer unit. More preferably, it contains 5% by mass or less.
前記粘着剤組成物のなかでも、光学的透明性に優れ、適宜な濡れ性と凝集性と接着性の粘着特性を示して、耐候性や耐熱性等に優れる点から、アクリル系粘着剤組成物が好ましく使用される。アクリル系粘着剤組成物は、粘着性のベースポリマーとして（メタ）アクリル系ポリマーを含むことが好ましい。（メタ）アクリル系ポリマーは、通常、モノマー単位として、アルキル（メタ）アクリレートを主成分として含有する。なお、（メタ）アクリレートはアクリレート及び／又はメタクリレートをいい、本発明の（メタ）とは同様の意味である。
Among the pressure-sensitive adhesive compositions, the acrylic pressure-sensitive adhesive composition has excellent optical transparency, exhibits appropriate wettability, cohesiveness, and adhesive properties, and is excellent in weather resistance, heat resistance, etc. is preferably used. The acrylic pressure-sensitive adhesive composition preferably contains a (meth)acrylic polymer as an adhesive base polymer. A (meth)acrylic polymer usually contains alkyl (meth)acrylate as a main component as a monomer unit. (Meth)acrylate refers to acrylate and/or methacrylate, and has the same meaning as (meth) in the present invention.
前記（メタ）アクリル系ポリマーの主骨格を構成する、アルキル（メタ）アクリレートとしては、直鎖状又は分岐鎖状のアルキル基の炭素数１～１８のものを例示できる。前記アルキル基としては、メチル基、エチル基、プロピル基、イソプロピル基、ブチル基、イソブチル基、アミル基、ヘキシル基、シクロヘキシル基、ヘプチル基、２－エチルヘキシル基、イソオクチル基、ノニル基、デシル基、イソデシル基、ドデシル基、イソミリスチル基、ラウリル基、トリデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基、等を例示できる。アルキル（メタ）アクリレートは、１種のみを用いてもよく、２種以上を用いてもよい。これらアルキル基の平均炭素数は３～９であるのが好ましい。
Examples of the alkyl (meth)acrylate that constitutes the main skeleton of the (meth)acrylic polymer include linear or branched alkyl groups having 1 to 18 carbon atoms. Examples of the alkyl group include methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, amyl group, hexyl group, cyclohexyl group, heptyl group, 2-ethylhexyl group, isooctyl group, nonyl group, decyl group, Examples include isodecyl group, dodecyl group, isomyristyl group, lauryl group, tridecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, and the like. Only one type of alkyl (meth)acrylate may be used, or two or more types may be used. The average carbon number of these alkyl groups is preferably 3-9.
また、前記アルキル（メタ）アクリレートとしては、粘着特性、耐久性、位相差の調整、屈折率の調整等の点から、フェノキシエチル（メタ）アクリレート、ベンジル（メタ）アクリレートのような芳香族環を含有するアルキル（メタ）アクリレートを用いることができる。
In addition, as the alkyl (meth) acrylate, aromatic rings such as phenoxyethyl (meth) acrylate and benzyl (meth) acrylate are used from the viewpoint of adhesive properties, durability, adjustment of retardation, adjustment of refractive index, etc. Alkyl (meth)acrylate containing can be used.
前記（メタ）アクリル系ポリマー中には、接着性や耐熱性の改善を目的に、（メタ）アクリロイル基又はビニル基等の不飽和二重結合を有する重合性の官能基を有する、１種類以上の共重合モノマーを共重合により導入することができる。共重合モノマーの具体例としては、（メタ）アクリル酸２－ヒドロキシエチル、（メタ）アクリル酸３－ヒドロキシプロピル、（メタ）アクリル酸４－ヒドロキシブチル、（メタ）アクリル酸６－ヒドロキシヘキシル、（メタ）アクリル酸８－ヒドロキシオクチル、（メタ）アクリル酸１０－ヒドロキシデシル、（メタ）アクリル酸１２－ヒドロキシラウリルや（４－ヒドロキシメチルシクロヘキシル）－メチルアクリレート等のヒドロキシ基含有モノマー；（メタ）アクリル酸、カルボキシエチル（メタ）アクリレート、カルボキシペンチル（メタ）アクリレート、イタコン酸、マレイン酸、フマール酸、クロトン酸等のカルボキシ基含有モノマー；無水マレイン酸、無水イタコン酸等の酸無水物基含有モノマー；アクリル酸のカプロラクトン付加物；スチレンスルホン酸やアリルスルホン酸、２－（メタ）アクリルアミド－２－メチルプロパンスルホン酸、（メタ）アクリルアミドプロパンスルホン酸、スルホプロピル（メタ）アクリレート、（メタ）アクリロイルオキシナフタレンスルホン酸等のスルホン酸基含有モノマー；２－ヒドロキシエチルアクリロイルホスフェート等の燐酸基含有モノマー等が挙げられる。
The (meth)acrylic polymer contains at least one polymerizable functional group having an unsaturated double bond such as a (meth)acryloyl group or a vinyl group for the purpose of improving adhesiveness and heat resistance. can be introduced by copolymerization. Specific examples of copolymerizable monomers include 2-hydroxyethyl (meth)acrylate, 3-hydroxypropyl (meth)acrylate, 4-hydroxybutyl (meth)acrylate, 6-hydroxyhexyl (meth)acrylate, ( Hydroxy group-containing monomers such as 8-hydroxyoctyl meth)acrylate, 10-hydroxydecyl (meth)acrylate, 12-hydroxylauryl (meth)acrylate and (4-hydroxymethylcyclohexyl)-methylacrylate; (meth)acrylic Carboxy group-containing monomers such as acids, carboxyethyl (meth)acrylate, carboxypentyl (meth)acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid; acid anhydride group-containing monomers such as maleic anhydride and itaconic anhydride; Caprolactone adducts of acrylic acid; styrenesulfonic acid, allylsulfonic acid, 2-(meth)acrylamido-2-methylpropanesulfonic acid, (meth)acrylamidopropanesulfonic acid, sulfopropyl (meth)acrylate, (meth)acryloyloxynaphthalene sulfonic acid group-containing monomers such as sulfonic acid; and phosphoric acid group-containing monomers such as 2-hydroxyethyl acryloyl phosphate.
上記で述べたように、前記（メタ）アクリル系ポリマーは、粘着剤層の高温耐久性を向上させる観点から、モノマー単位として前記カルボキシ基含有モノマーを０．５質量％以上含有する。好ましい含有量は上記のとおりである。
As described above, the (meth)acrylic polymer contains 0.5% by mass or more of the carboxy group-containing monomer as a monomer unit from the viewpoint of improving the high-temperature durability of the pressure-sensitive adhesive layer. Preferred contents are as described above.
前記（メタ）アクリル系ポリマーは、全構成モノマーの質量比率において、アルキル（メタ）アクリレートを主成分とし、前記共重合モノマーの割合は特に制限されないが、全構成モノマーの質量比率において、０～２０％程度、０．１～１５％程度、さらには０．１～１０％程度であるのが好ましい。
The (meth)acrylic polymer is mainly composed of alkyl (meth)acrylate in the mass ratio of all constituent monomers, and the ratio of the copolymerization monomer is not particularly limited, but the mass ratio of all constituent monomers is 0 to 20. %, preferably about 0.1 to 15%, more preferably about 0.1 to 10%.
前記（メタ）アクリル系ポリマーは、通常、重量平均分子量（Ｍｗ）が５０万～３００万の範囲のものが用いられる。耐久性、特に耐熱性を考慮すれば、重量平均分子量（Ｍｗ）は７０万～２７０万であるものを用いることが好ましく、８０万～２５０万であることがより好ましい。重量平均分子量（Ｍｗ）が５０万よりも小さいと、耐熱性の点で好ましくない。また、重量平均分子量（Ｍｗ）が３００万よりも大きくなると、塗布するための粘度に調整するために多量の希釈溶剤が必要となり、コストアップとなることから好ましくない。なお、前記重量平均分子量（Ｍｗ）は、ＧＰＣ（ゲル・パーミエーション・クロマトグラフィー）により測定し、ポリスチレン換算により算出された値をいう。
The (meth)acrylic polymer usually used has a weight average molecular weight (Mw) in the range of 500,000 to 3,000,000. Considering durability, especially heat resistance, the weight average molecular weight (Mw) is preferably 700,000 to 2,700,000, more preferably 800,000 to 2,500,000. A weight-average molecular weight (Mw) of less than 500,000 is not preferable in terms of heat resistance. Further, if the weight average molecular weight (Mw) is more than 3,000,000, a large amount of diluent solvent is required to adjust the viscosity for coating, which is not preferable because it increases the cost. The weight average molecular weight (Mw) is a value measured by GPC (gel permeation chromatography) and calculated by polystyrene conversion.
前記（メタ）アクリル系ポリマーの製造は、溶液重合、塊状重合、乳化重合、各種ラジカル重合等の公知の製造方法を適宜選択できる。また、得られる（メタ）アクリル系ポリマーは、ランダム共重合体、ブロック共重合体、グラフト共重合体等いずれでもよい。
For the production of the (meth)acrylic polymer, known production methods such as solution polymerization, bulk polymerization, emulsion polymerization, and various radical polymerizations can be appropriately selected. The (meth)acrylic polymer to be obtained may be a random copolymer, a block copolymer, a graft copolymer, or the like.
前記ラジカル重合に用いられる重合開始剤、連鎖移動剤、乳化剤等は特に限定されず適宜選択して使用することができる。なお、（メタ）アクリル系ポリマーの重量平均分子量（Ｍｗ）は、重合開始剤、連鎖移動剤の使用量、反応条件により制御可能であり、これらの種類に応じて適宜のその使用量が調整される。
The polymerization initiator, chain transfer agent, emulsifier, etc. used in the radical polymerization are not particularly limited and can be appropriately selected and used. The weight-average molecular weight (Mw) of the (meth)acrylic polymer can be controlled by the amount of the polymerization initiator and the chain transfer agent used and the reaction conditions, and the amount used is appropriately adjusted according to these types. be.
なお、前記溶液重合においては、重合溶媒として、酢酸エチル、トルエン等が用いられる。具体的な溶液重合例としては、反応は窒素等の不活性ガス気流下で、重合開始剤を加え、通常、５０～７０℃程度で、５～３０時間程度の反応条件で行われる。
In addition, in the solution polymerization, ethyl acetate, toluene, or the like is used as a polymerization solvent. As a specific example of solution polymerization, the reaction is carried out under an inert gas stream such as nitrogen, adding a polymerization initiator, and generally at a temperature of about 50 to 70° C. for about 5 to 30 hours.
＜導電剤＞
前記粘着剤組成物は、前記ベースポリマーに加えて、導電剤を含有することが好ましい。導電剤としては、イオン性化合物、イオン性界面活性剤、導電性ポリマー、金属酸化物等が挙げられる。 <Conductive agent>
The adhesive composition preferably contains a conductive agent in addition to the base polymer. Conductive agents include ionic compounds, ionic surfactants, conductive polymers, metal oxides, and the like.
前記粘着剤組成物は、前記ベースポリマーに加えて、導電剤を含有することが好ましい。導電剤としては、イオン性化合物、イオン性界面活性剤、導電性ポリマー、金属酸化物等が挙げられる。 <Conductive agent>
The adhesive composition preferably contains a conductive agent in addition to the base polymer. Conductive agents include ionic compounds, ionic surfactants, conductive polymers, metal oxides, and the like.
前記イオン性化合物としては、アルカリ金属塩及び／または有機カチオン－アニオン塩を好ましく用いることができる。アルカリ金属塩は、アルカリ金属の有機塩および無機塩を用いることができる。なお、本発明でいう、「有機カチオン－アニオン塩」とは、有機塩であって、そのカチオン部が有機物で構成されているものを示し、アニオン部は有機物であっても良いし、無機物であっても良い。「有機カチオン－アニオン塩」は、イオン性液体、イオン性固体とも言われる。イオン性化合物は、１種のみを用いてもよく、２種以上を用いてもよい。
As the ionic compound, an alkali metal salt and/or an organic cation-anion salt can be preferably used. As alkali metal salts, organic salts and inorganic salts of alkali metals can be used. In the present invention, the term "organic cation-anion salt" refers to an organic salt whose cation part is composed of an organic substance, and whose anion part may be an organic substance or an inorganic substance. It can be. "Organic cation-anion salts" are also referred to as ionic liquids, ionic solids. Only one kind of ionic compound may be used, or two or more kinds thereof may be used.
前記アルカリ金属塩のカチオン部を構成するアルカリ金属イオンとしては、リチウム、ナトリウム、カリウムの各イオンが挙げられる。これらアルカリ金属イオンのなかでもリチウムイオンが好ましい。
Examples of the alkali metal ions constituting the cation portion of the alkali metal salt include ions of lithium, sodium, and potassium. Among these alkali metal ions, lithium ions are preferred.
前記アルカリ金属塩のアニオン部は有機物で構成されていてもよく、無機物で構成されていてもよい。有機塩を構成するアニオン部としては、ＣＨ３ＣＯＯ－、ＣＦ３ＣＯＯ－、ＣＨ３ＳＯ３
－、ＣＦ３ＳＯ３
－、（ＣＦ３ＳＯ２）３Ｃ－、Ｃ４Ｆ９ＳＯ３
－、Ｃ３Ｆ７ＣＯＯ－、（ＣＦ３ＳＯ２）（ＣＦ３ＣＯ）Ｎ－、－Ｏ３Ｓ（ＣＦ２）３ＳＯ３
－、ＰＦ６
－、ＣＯ３
２－、や下記一般式（１）乃至（４）、
（１）：（ＣｎＦ２ｎ＋１ＳＯ２）２Ｎ－ （但し、ｎは1～１０の整数）、
（２）：ＣＦ２（ＣｍＦ２ｍＳＯ２）２Ｎ－ （但し、ｍは１～１０の整数）、
（３）：－Ｏ３Ｓ（ＣＦ２）ｌＳＯ３ － （但し、ｌは１～１０の整数）、
（４）：（ＣｐＦ２ｐ＋１ＳＯ２）Ｎ－（ＣｑＦ２ｑ＋１ＳＯ２）、（但し、ｐ、ｑは１～１０の整数）、で表わされるもの等が用いられる。特に、フッ素原子を含むアニオン部は、イオン解離性の良いイオン化合物が得られることから好ましく用いられる。無機塩を構成するアニオン部としては、Ｃｌ－、Ｂｒ－、Ｉ－、ＡｌＣｌ４ －、Ａｌ２Ｃｌ７ －、ＢＦ４ －、ＰＦ６ －、ＣｌＯ４ －、ＮＯ３ －、ＡｓＦ６ －、ＳｂＦ６ －、ＮｂＦ６ －、ＴａＦ６ －、（ＣＮ）２Ｎ－、等が用いられる。アニオン部としては、（ＣＦ３ＳＯ２）２Ｎ－、（Ｃ２Ｆ５ＳＯ２）２Ｎ－、等の前記一般式（１）で表わされる、（ペルフルオロアルキルスルホニル）イミドが好ましく、特に（ＣＦ３ＳＯ２）２Ｎ－、で表わされる（トリフルオロメタンスルホニル）イミドが好ましい。 The anion portion of the alkali metal salt may be composed of an organic substance or an inorganic substance. The anion moiety constituting the organic salt includes CH 3 COO − , CF 3 COO − , CH 3 SO 3 − , CF 3 SO 3 − , (CF 3 SO 2 ) 3 C − , C 4 F 9 SO 3 − , C 3 F 7 COO − , (CF 3 SO 2 )(CF 3 CO)N − , —O 3 S(CF 2 ) 3 SO 3 − , PF 6 − , CO 3 2− , or the following general formula (1) through (4),
(1): (C n F 2n+1 SO 2 ) 2 N − (where n is an integer of 1 to 10),
(2): CF 2 (C m F 2m SO 2 ) 2 N − (where m is an integer of 1 to 10),
(3): - O 3 S(CF 2 ) l SO 3 - (where l is an integer of 1 to 10),
(4): (C p F 2p+1 SO 2 )N − (C q F 2q+1 SO 2 ), where p and q are integers of 1 to 10, and the like are used. In particular, an anion moiety containing a fluorine atom is preferably used because an ionic compound having good ion dissociation properties can be obtained. Examples of the anion moiety constituting the inorganic salt include Cl − , Br − , I − , AlCl 4 − , Al 2 Cl 7 − , BF 4 − , PF 6 − , ClO 4 − , NO 3 − , AsF 6 − , SbF 6 − , NbF 6 − , TaF 6 − , (CN) 2 N − , etc. are used. As the anion portion, (CF 3 SO 2 ) 2 N − , (C 2 F 5 SO 2 ) 2 N − , and the like (perfluoroalkylsulfonyl) imides represented by the general formula (1) are preferable, and ( (Trifluoromethanesulfonyl)imide represented by CF 3 SO 2 ) 2 N − is preferred.
（１）：（ＣｎＦ２ｎ＋１ＳＯ２）２Ｎ－ （但し、ｎは1～１０の整数）、
（２）：ＣＦ２（ＣｍＦ２ｍＳＯ２）２Ｎ－ （但し、ｍは１～１０の整数）、
（３）：－Ｏ３Ｓ（ＣＦ２）ｌＳＯ３ － （但し、ｌは１～１０の整数）、
（４）：（ＣｐＦ２ｐ＋１ＳＯ２）Ｎ－（ＣｑＦ２ｑ＋１ＳＯ２）、（但し、ｐ、ｑは１～１０の整数）、で表わされるもの等が用いられる。特に、フッ素原子を含むアニオン部は、イオン解離性の良いイオン化合物が得られることから好ましく用いられる。無機塩を構成するアニオン部としては、Ｃｌ－、Ｂｒ－、Ｉ－、ＡｌＣｌ４ －、Ａｌ２Ｃｌ７ －、ＢＦ４ －、ＰＦ６ －、ＣｌＯ４ －、ＮＯ３ －、ＡｓＦ６ －、ＳｂＦ６ －、ＮｂＦ６ －、ＴａＦ６ －、（ＣＮ）２Ｎ－、等が用いられる。アニオン部としては、（ＣＦ３ＳＯ２）２Ｎ－、（Ｃ２Ｆ５ＳＯ２）２Ｎ－、等の前記一般式（１）で表わされる、（ペルフルオロアルキルスルホニル）イミドが好ましく、特に（ＣＦ３ＳＯ２）２Ｎ－、で表わされる（トリフルオロメタンスルホニル）イミドが好ましい。 The anion portion of the alkali metal salt may be composed of an organic substance or an inorganic substance. The anion moiety constituting the organic salt includes CH 3 COO − , CF 3 COO − , CH 3 SO 3 − , CF 3 SO 3 − , (CF 3 SO 2 ) 3 C − , C 4 F 9 SO 3 − , C 3 F 7 COO − , (CF 3 SO 2 )(CF 3 CO)N − , —O 3 S(CF 2 ) 3 SO 3 − , PF 6 − , CO 3 2− , or the following general formula (1) through (4),
(1): (C n F 2n+1 SO 2 ) 2 N − (where n is an integer of 1 to 10),
(2): CF 2 (C m F 2m SO 2 ) 2 N − (where m is an integer of 1 to 10),
(3): - O 3 S(CF 2 ) l SO 3 - (where l is an integer of 1 to 10),
(4): (C p F 2p+1 SO 2 )N − (C q F 2q+1 SO 2 ), where p and q are integers of 1 to 10, and the like are used. In particular, an anion moiety containing a fluorine atom is preferably used because an ionic compound having good ion dissociation properties can be obtained. Examples of the anion moiety constituting the inorganic salt include Cl − , Br − , I − , AlCl 4 − , Al 2 Cl 7 − , BF 4 − , PF 6 − , ClO 4 − , NO 3 − , AsF 6 − , SbF 6 − , NbF 6 − , TaF 6 − , (CN) 2 N − , etc. are used. As the anion portion, (CF 3 SO 2 ) 2 N − , (C 2 F 5 SO 2 ) 2 N − , and the like (perfluoroalkylsulfonyl) imides represented by the general formula (1) are preferable, and ( (Trifluoromethanesulfonyl)imide represented by CF 3 SO 2 ) 2 N − is preferred.
アルカリ金属の有機塩としては、具体的には、酢酸ナトリウム、アルギン酸ナトリウム、リグニンスルホン酸ナトリウム、トルエンスルホン酸ナトリウム、ＬｉＣＦ３ＳＯ３、Ｌｉ（ＣＦ３ＳＯ２）２Ｎ、Ｌｉ（Ｃ２Ｆ５ＳＯ２）２Ｎ、Ｌｉ（Ｃ４Ｆ９ＳＯ２）２Ｎ、Ｌｉ（ＣＦ３ＳＯ２）３Ｃ、ＫＯ３Ｓ（ＣＦ２）３ＳＯ３Ｋ、ＬｉＯ３Ｓ（ＣＦ２）３ＳＯ３Ｋ等が挙げられ、これらのうちＬｉＣＦ３ＳＯ３、Ｌｉ（ＣＦ３ＳＯ２）２Ｎ、Ｌｉ（Ｃ２Ｆ５ＳＯ２）２Ｎ、Ｌｉ（Ｃ４Ｆ９ＳＯ２）２Ｎ、Ｌｉ（ＣＦ３ＳＯ２）３Ｃ等が好ましく、Ｌｉ（ＣＦ３ＳＯ２）２Ｎ、Ｌｉ（Ｃ２Ｆ５ＳＯ２）２Ｎ、Ｌｉ（Ｃ４Ｆ９ＳＯ２）２Ｎ等のフッ素含有リチウムイミド塩がより好ましく、特に（ペルフルオロアルキルスルホニル）イミドリチウム塩が好ましい。
Specific examples of alkali metal organic salts include sodium acetate, sodium alginate, sodium ligninsulfonate, sodium toluenesulfonate, LiCF 3 SO 3 , Li(CF 3 SO 2 ) 2 N, Li(C 2 F 5 SO2 ) 2N , Li ( C4F9SO2 ) 2N , Li ( CF3SO2 ) 3C , KO3S ( CF2 ) 3SO3K , LiO3S ( CF2 ) 3SO3 K and the like, among which LiCF 3 SO 3 , Li(CF 3 SO 2 ) 2 N, Li(C 2 F 5 SO 2 ) 2 N, Li(C 4 F 9 SO 2 ) 2 N, Li( CF 3 SO 2 ) 3 C and the like are preferred, and fluorine-containing lithium imides such as Li(CF 3 SO 2 ) 2 N, Li(C 2 F 5 SO 2 ) 2 N and Li(C 4 F 9 SO 2 ) 2 N Salts are more preferred, especially (perfluoroalkylsulfonyl)imide lithium salts.
また、アルカリ金属の無機塩としては、過塩素酸リチウム、ヨウ化リチウムが挙げられる。
Inorganic salts of alkali metals include lithium perchlorate and lithium iodide.
前記有機カチオン－アニオン塩は、カチオン成分とアニオン成分とから構成されており、前記カチオン成分は有機物からなるものである。カチオン成分として、具体的には、ピリジニウムカチオン、ピペリジニウムカチオン、ピロリジニウムカチオン、ピロリン骨格を有するカチオン、ピロール骨格を有するカチオン、イミダゾリウムカチオン、テトラヒドロピリミジニウムカチオン、ジヒドロピリミジニウムカチオン、ピラゾリウムカチオン、ピラゾリニウムカチオン、テトラアルキルアンモニウムカチオン、トリアルキルスルホニウムカチオン、テトラアルキルホスホニウムカチオン等が挙げられる。
The organic cation-anion salt is composed of a cation component and an anion component, and the cation component is composed of an organic substance. Specific examples of cationic components include pyridinium cations, piperidinium cations, pyrrolidinium cations, cations having a pyrroline skeleton, cations having a pyrrole skeleton, imidazolium cations, tetrahydropyrimidinium cations, dihydropyrimidinium cations, Examples include pyrazolium cations, pyrazolinium cations, tetraalkylammonium cations, trialkylsulfonium cations, tetraalkylphosphonium cations, and the like.
前記アニオン成分としては、Ｃｌ－、Ｂｒ－、Ｉ－、ＡｌＣｌ４
－、Ａｌ２Ｃｌ７
－、ＢＦ４
－、ＰＦ６
－、ＣｌＯ４
－、ＮＯ３
－、ＣＨ３ＣＯＯ－、ＣＦ３ＣＯＯ－、ＣＨ３ＳＯ３
－、ＣＦ３ＳＯ３
－、（ＣＦ３ＳＯ２）３Ｃ－、ＡｓＦ６
－、ＳｂＦ６
－、ＮｂＦ６
－、ＴａＦ６
－、（ＣＮ）２Ｎ－、Ｃ４Ｆ９ＳＯ３
－、Ｃ３Ｆ７ＣＯＯ－、（（ＣＦ３ＳＯ２）（ＣＦ３ＣＯ）Ｎ－、－Ｏ３Ｓ（ＣＦ２）３ＳＯ３
－、や下記一般式（１）乃至（４）、
（１）：（ＣｎＦ２ｎ＋１ＳＯ２）２Ｎ－ （但し、ｎは1～１０の整数）、
（２）：ＣＦ２（ＣｍＦ２ｍＳＯ２）２Ｎ－ （但し、ｍは１～１０の整数）、
（３）：－Ｏ３Ｓ（ＣＦ２）ｌＳＯ３ － （但し、ｌは１～１０の整数）、
（４）：（ＣｐＦ２ｐ＋１ＳＯ２）Ｎ－（ＣｑＦ２ｑ＋１ＳＯ２）、（但し、ｐ、ｑは１～１０の整数）、で表わされるもの等が用いられる。なかでも特に、フッ素原子を含むアニオン成分は、イオン解離性の良いイオン化合物が得られることから好ましく用いられる。 Examples of the anion component include Cl − , Br − , I − , AlCl 4 − , Al 2 Cl 7 − , BF 4 − , PF 6 − , ClO 4 − , NO 3 − , CH 3 COO − , CF 3 COO − , CH 3 SO 3 − , CF 3 SO 3 − , (CF 3 SO 2 ) 3 C − , AsF 6 − , SbF 6 − , NbF 6 − , TaF 6 − , (CN) 2 N − , C 4 F 9 SO 3 − , C 3 F 7 COO − , ((CF 3 SO 2 )(CF 3 CO)N − , —O 3 S(CF 2 ) 3 SO 3 − , or the following general formulas (1) to (4) ,
(1): (C n F 2n+1 SO 2 ) 2 N − (where n is an integer of 1 to 10),
(2): CF 2 (C m F 2m SO 2 ) 2 N − (where m is an integer of 1 to 10),
(3): - O 3 S(CF 2 ) l SO 3 - (where l is an integer of 1 to 10),
(4): (C p F 2p+1 SO 2 )N − (C q F 2q+1 SO 2 ), where p and q are integers of 1 to 10, and the like are used. Among them, an anion component containing a fluorine atom is particularly preferably used because an ionic compound having good ion dissociation properties can be obtained.
（１）：（ＣｎＦ２ｎ＋１ＳＯ２）２Ｎ－ （但し、ｎは1～１０の整数）、
（２）：ＣＦ２（ＣｍＦ２ｍＳＯ２）２Ｎ－ （但し、ｍは１～１０の整数）、
（３）：－Ｏ３Ｓ（ＣＦ２）ｌＳＯ３ － （但し、ｌは１～１０の整数）、
（４）：（ＣｐＦ２ｐ＋１ＳＯ２）Ｎ－（ＣｑＦ２ｑ＋１ＳＯ２）、（但し、ｐ、ｑは１～１０の整数）、で表わされるもの等が用いられる。なかでも特に、フッ素原子を含むアニオン成分は、イオン解離性の良いイオン化合物が得られることから好ましく用いられる。 Examples of the anion component include Cl − , Br − , I − , AlCl 4 − , Al 2 Cl 7 − , BF 4 − , PF 6 − , ClO 4 − , NO 3 − , CH 3 COO − , CF 3 COO − , CH 3 SO 3 − , CF 3 SO 3 − , (CF 3 SO 2 ) 3 C − , AsF 6 − , SbF 6 − , NbF 6 − , TaF 6 − , (CN) 2 N − , C 4 F 9 SO 3 − , C 3 F 7 COO − , ((CF 3 SO 2 )(CF 3 CO)N − , —O 3 S(CF 2 ) 3 SO 3 − , or the following general formulas (1) to (4) ,
(1): (C n F 2n+1 SO 2 ) 2 N − (where n is an integer of 1 to 10),
(2): CF 2 (C m F 2m SO 2 ) 2 N − (where m is an integer of 1 to 10),
(3): - O 3 S(CF 2 ) l SO 3 - (where l is an integer of 1 to 10),
(4): (C p F 2p+1 SO 2 )N − (C q F 2q+1 SO 2 ), where p and q are integers of 1 to 10, and the like are used. Among them, an anion component containing a fluorine atom is particularly preferably used because an ionic compound having good ion dissociation properties can be obtained.
また、前記イオン性化合物としては、前記のアルカリ金属塩、有機カチオン－アニオン塩の他に、塩化アンモニウム、塩化アルミニウム、塩化銅、塩化第一鉄、塩化第二鉄、硫酸アンモニウム等の無機塩が挙げられる。
Examples of the ionic compound include inorganic salts such as ammonium chloride, aluminum chloride, copper chloride, ferrous chloride, ferric chloride, and ammonium sulfate, in addition to the alkali metal salts and organic cation-anion salts described above. be done.
前記イオン性界面活性剤としては、カチオン系（４級アンモニウム塩型、ホスホニウム塩型、スルホニウム塩型等）、アニオン系（カルボン酸型、スルホネート型、サルフェート型、ホスフェート型、ホスファイト型等）、両性イオン系（スルホベタイン型、アルキルベタイン型、アルキルイミダゾリウムベタイン型等）またはノニオン系（多価アルコール誘導体、β－シクロデキストリン包接化合物、ソルビタン脂肪酸モノエステル・ジエステル、ポリアルキレンオキシド誘導体、アミンオキシド等）の各種界面活性剤が挙げられる。イオン性界面活性剤は、１種のみを用いてもよく、２種以上を用いてもよい。
Examples of the ionic surfactant include cationic surfactants (quaternary ammonium salt type, phosphonium salt type, sulfonium salt type, etc.), anionic surfactants (carboxylic acid type, sulfonate type, sulfate type, phosphate type, phosphite type, etc.), Zwitterionic (sulfobetaine type, alkylbetaine type, alkylimidazolium betaine type, etc.) or nonionic (polyhydric alcohol derivative, β-cyclodextrin inclusion compound, sorbitan fatty acid monoester/diester, polyalkylene oxide derivative, amine oxide etc.). Only 1 type may be used for an ionic surfactant, and 2 or more types may be used for it.
前記導電性ポリマーとしては、ポリアニリン系、ポリチオフェン系、ポリピロール系、ポリキノキサリン系等のポリマーがあげられるが、これらのなかでも、水溶性導電性ポリマーまたは水分散性導電性ポリマーになり易い、ポリアニリン、ポリチオフェン等が好ましく使用される。特にポリチオフェンが好ましい。導電性ポリマーは、１種のみを用いてもよく、２種以上を用いてもよい。
Examples of the conductive polymer include polyaniline-based, polythiophene-based, polypyrrole-based, and polyquinoxaline-based polymers. Polythiophene and the like are preferably used. Polythiophene is particularly preferred. Only one type of conductive polymer may be used, or two or more types may be used.
前記金属酸化物としては、酸化スズ系、酸化アンチモン系、酸化インジウム系、酸化亜鉛系等があげられる。これらのなかでも酸化スズ系が好ましい。酸化スズ系のものとしては、たとえば、酸化スズの他、アンチモンドープ酸化スズ、インジウムドープ酸化スズ、アルミニウムドープ酸化スズ、タングステンドープ酸化スズ、酸化チタン－酸化セリウム－酸化スズの複合体、酸化チタン－酸化スズの複合体等があげられる。金属酸化物は、１種のみを用いてもよく、２種以上を用いてもよい。
Examples of the metal oxide include tin oxide, antimony oxide, indium oxide, and zinc oxide. Among these, the tin oxide type is preferable. Tin oxides include, in addition to tin oxide, antimony-doped tin oxide, indium-doped tin oxide, aluminum-doped tin oxide, tungsten-doped tin oxide, titanium oxide-cerium oxide-tin oxide composite, titanium oxide- Composites of tin oxide and the like can be mentioned. Only one kind of metal oxide may be used, or two or more kinds thereof may be used.
さらに前記以外の導電剤として、アセチレンブラック、ケッチェンブラック、天然グラファイト、人造グラファイト、チタンブラックや、カチオン型（４級アンモニウム塩等）、両性イオン型（ベタイン化合物等）、アニオン型（スルホン酸塩等）またはノニオン型（グリセリン等）のイオン導電性基を有する単量体の単独重合体若しくは当該単量体と他の単量体との共重合体、４級アンモニウム塩基を有するアクリレートまたはメタクリレート由来の部位を有する重合体等のイオン導電性を有する重合体；ポリエチレンメタクリレート共重合体等の親水性ポリマーをアクリル系樹脂等にアロイ化させたタイプの永久帯電防止剤を例示できる。
Furthermore, as conductive agents other than the above, acetylene black, ketjen black, natural graphite, artificial graphite, titanium black, cation type (quaternary ammonium salt, etc.), amphoteric ion type (betaine compound, etc.), anionic type (sulfonate etc.) or a homopolymer of a monomer having a nonionic (glycerin, etc.) ion-conductive group or a copolymer of the monomer with another monomer, an acrylate or methacrylate derived from a quaternary ammonium base and a permanent antistatic agent of the type in which a hydrophilic polymer such as a polyethylene methacrylate copolymer is alloyed with an acrylic resin or the like.
前記導電剤は、導電性能が高い点、粘着剤中で分散性や透明性に優れている点、粘着剤中での保管安定性の観点から、イオン性化合物を用いることが好ましい。
It is preferable to use an ionic compound as the conductive agent from the viewpoints of high conductive performance, excellent dispersibility and transparency in the adhesive, and storage stability in the adhesive.
前記導電剤の配合割合は、ベースポリマー１００質量部に対して、０．０００１～１０質量部が好ましい。導電剤が０．０００１質量部未満では、帯電防止性能の向上効果が十分ではない場合がある。一方、導電剤は１０質量部より多いと、耐久性が十分ではなくなる場合がある。導電剤は、０．０１質量部以上が好ましく、０．１質量部以上であるのがより好ましい。また、導電剤は、８質量部以下が好ましく、６質量部以下であるのがより好ましい。
The mixing ratio of the conductive agent is preferably 0.0001 to 10 parts by mass with respect to 100 parts by mass of the base polymer. If the amount of the conductive agent is less than 0.0001 parts by mass, the effect of improving the antistatic performance may not be sufficient. On the other hand, if the conductive agent is more than 10 parts by mass, the durability may not be sufficient. The conductive agent is preferably 0.01 parts by mass or more, more preferably 0.1 parts by mass or more. The conductive agent is preferably 8 parts by mass or less, more preferably 6 parts by mass or less.
さらに、前記粘着剤組成物には、架橋剤を含有することできる。架橋剤としては、有機系架橋剤や多官能性金属キレートを用いることができる。有機系架橋剤としては、イソシアネート系架橋剤、過酸化物系架橋剤、エポキシ系架橋剤、イミン系架橋剤等が挙げられる。多官能性金属キレートは、多価金属が有機化合物と共有結合又は配位結合しているものである。多価金属原子としては、Ａｌ、Ｃｒ、Ｚｒ、Ｃｏ、Ｃｕ、Ｆｅ、Ｎｉ、Ｖ、Ｚｎ、Ｉｎ、Ｃａ、Ｍｇ、Ｍｎ、Ｙ、Ｃｅ、Ｓｒ、Ｂａ、Ｍｏ、Ｌａ、Ｓｎ、Ｔｉ等が挙げられる。共有結合又は配位結合する有機化合物中の原子としては酸素原子等が挙げられ、有機化合物としてはアルキルエステル、アルコール化合物、カルボン酸化合物、エーテル化合物、ケトン化合物等が挙げられる。架橋剤としては、イソシアネート系架橋剤、過酸化物系架橋剤が好ましい。架橋剤は、１種のみを用いてもよく、２種以上を用いてもよい。
Furthermore, the adhesive composition can contain a cross-linking agent. As the cross-linking agent, an organic cross-linking agent or a polyfunctional metal chelate can be used. Examples of organic cross-linking agents include isocyanate-based cross-linking agents, peroxide-based cross-linking agents, epoxy-based cross-linking agents, and imine-based cross-linking agents. Polyfunctional metal chelates are those in which polyvalent metals are covalently or coordinately bonded to organic compounds. Polyvalent metal atoms include Al, Cr, Zr, Co, Cu, Fe, Ni, V, Zn, In, Ca, Mg, Mn, Y, Ce, Sr, Ba, Mo, La, Sn, and Ti. mentioned. An oxygen atom etc. are mentioned as an atom in the organic compound which carries out a covalent bond or a coordinate bond, and an alkylester, an alcohol compound, a carboxylic acid compound, an ether compound, a ketone compound etc. are mentioned as an organic compound. The cross-linking agent is preferably an isocyanate-based cross-linking agent or a peroxide-based cross-linking agent. Only one type of cross-linking agent may be used, or two or more types may be used.
前記架橋剤の配合割合は、ベースポリマー１００質量部に対して、０．０１～２０質量部が好ましく、０．０３～１０質量部がより好ましい。なお、架橋剤が０．０１質量部未満では、粘着剤の凝集力が不足する傾向があり、加熱時に発泡が生じるおそれがあり、一方、２０質量部より多いと、耐湿性が十分ではなく、信頼性試験等で剥がれが生じやすくなる。
The mixing ratio of the cross-linking agent is preferably 0.01 to 20 parts by mass, more preferably 0.03 to 10 parts by mass, with respect to 100 parts by mass of the base polymer. If the amount of the cross-linking agent is less than 0.01 parts by mass, the cohesive force of the adhesive tends to be insufficient, and foaming may occur during heating. Peeling is likely to occur in a reliability test or the like.
さらに、前記粘着剤組成物には、シランカップリング剤を含有することできる。シランカップリング剤を用いることにより、耐久性を向上させることができる。シランカップリング剤は、１種のみを用いてもよく、２種以上を用いてもよい。
Furthermore, the adhesive composition can contain a silane coupling agent. Durability can be improved by using a silane coupling agent. Only one kind of silane coupling agent may be used, or two or more kinds thereof may be used.
前記シランカップリング剤の配合割合は、ベースポリマー１００質量部に対し、シランカップリング剤０．００１～５質量部が好ましく、０．０１～１質量部がより好ましく、０．０２～１質量部がさらに好ましく、０．０５～０．６質量部が特に好ましい。耐久性を向上させ、液晶パネル等の光学部材への接着力を適度に保持するために、この範囲内で適宜選択される。
The mixing ratio of the silane coupling agent is preferably 0.001 to 5 parts by mass, more preferably 0.01 to 1 part by mass, and 0.02 to 1 part by mass with respect to 100 parts by mass of the base polymer. is more preferred, and 0.05 to 0.6 parts by mass is particularly preferred. It is appropriately selected within this range in order to improve durability and maintain an appropriate adhesive strength to optical members such as liquid crystal panels.
さらに、前記粘着剤組成物には、その他の公知の添加剤を含有していてもよく、着色剤、顔料等の粉体、染料、界面活性剤、可塑剤、粘着性付与剤、表面潤滑剤、レベリング剤、軟化剤、酸化防止剤、老化防止剤、光安定剤、紫外線吸収剤、重合禁止剤、無機又は有機の充填剤、金属粉、粒子状、箔状物等を使用する用途に応じて適宜添加することができる。また、制御できる範囲内で、還元剤を加えてのレドックス系を採用してもよい。
Furthermore, the pressure-sensitive adhesive composition may contain other known additives, such as powders such as colorants and pigments, dyes, surfactants, plasticizers, tackifiers, surface lubricants. , leveling agents, softeners, antioxidants, anti-aging agents, light stabilizers, UV absorbers, polymerization inhibitors, inorganic or organic fillers, metal powders, particulates, foils, etc. can be added as appropriate. Also, a redox system with a reducing agent added may be employed within a controllable range.
前記セパレータ付き粘着剤層は、前記セパレータの離型層上に、前記粘着剤組成物を含有する溶液を塗布した後、乾燥して粘着剤層を形成することにより製造することができる。なお、粘着剤組成物の塗布にあたっては、適宜に、重合溶剤以外の一種以上の溶剤を新たに加えてもよい。
The pressure-sensitive adhesive layer with a separator can be produced by applying a solution containing the pressure-sensitive adhesive composition onto the release layer of the separator, followed by drying to form a pressure-sensitive adhesive layer. In applying the pressure-sensitive adhesive composition, one or more solvents other than the polymerization solvent may be newly added as appropriate.
前記粘着剤組成物の塗布方法としては、各種方法が用いられる。具体的には、ロールコート、キスロールコート、グラビアコート、リバースコート、ロールブラッシュ、スプレーコート、ディップロールコート、バーコート、ナイフコート、エアーナイフコート、カーテンコート、リップコート、ダイコーター等による押出しコート法等の方法が挙げられる。
Various methods are used as a method for applying the pressure-sensitive adhesive composition. Specifically, roll coating, kiss roll coating, gravure coating, reverse coating, roll brushing, spray coating, dip roll coating, bar coating, knife coating, air knife coating, curtain coating, lip coating, extrusion coating using a die coater, etc. method such as the law.
前記粘着剤層の厚さは、特に制限されず、１～１００μｍ程度である。好ましくは、２～５０μｍ、より好ましくは２～４０μｍであり、さらに好ましくは、５～３５μｍである。
The thickness of the adhesive layer is not particularly limited, and is about 1 to 100 μm. It is preferably 2 to 50 μm, more preferably 2 to 40 μm, even more preferably 5 to 35 μm.
前記粘着剤層の表面抵抗値は、セパレータ付き粘着剤層に導電性を付与し、液晶パネルの白色ムラを抑制する観点から、１．０×１０１２Ω／□以下であることが好ましく、１．０×１０１１Ω／□以下であることがより好ましく、１．０×１０１０Ω／□以下であることがさらに好ましい。
The surface resistance value of the pressure-sensitive adhesive layer is preferably 1.0×10 12 Ω/□ or less from the viewpoint of imparting conductivity to the pressure-sensitive adhesive layer with separator and suppressing white unevenness of the liquid crystal panel. It is more preferably 0×10 11 Ω/□ or less, and further preferably 1.0×10 10 Ω/□ or less.
＜セパレータを有する粘着剤層付き偏光フィルム＞
本発明のセパレータを有する粘着剤層付き偏光フィルムは、前記セパレータ付き粘着剤層の粘着剤層側が偏光フィルムの片面又は両面に貼り合わされたものである。 <Polarizing film with pressure-sensitive adhesive layer having a separator>
The pressure-sensitive adhesive layer-attached polarizing film having the separator of the present invention is obtained by bonding the pressure-sensitive adhesive layer side of the separator-attached pressure-sensitive adhesive layer to one side or both sides of the polarizing film.
本発明のセパレータを有する粘着剤層付き偏光フィルムは、前記セパレータ付き粘着剤層の粘着剤層側が偏光フィルムの片面又は両面に貼り合わされたものである。 <Polarizing film with pressure-sensitive adhesive layer having a separator>
The pressure-sensitive adhesive layer-attached polarizing film having the separator of the present invention is obtained by bonding the pressure-sensitive adhesive layer side of the separator-attached pressure-sensitive adhesive layer to one side or both sides of the polarizing film.
前記偏光フィルムは、偏光子の片面または両面に透明保護フィルムを有するものが一般に用いられる。偏光子は、特に限定されず、各種のものを使用できる。偏光子としては、ポリビニルアルコール系フィルム、部分ホルマール化ポリビニルアルコール系フィルム、エチレン・酢酸ビニル共重合体系部分ケン化フィルム等の親水性高分子フィルムに、ヨウ素や二色性染料の二色性物質を吸着させて一軸延伸したもの、ポリビニルアルコールの脱水処理物やポリ塩化ビニルの脱塩酸処理物等ポリエン系配向フィルム等が挙げられる。これらの中でも、ポリビニルアルコール系フィルムとヨウ素等の二色性物質からなる偏光子が好適である。これらの偏光子の厚さは特に制限されないが、一般的に８０μｍ程度以下である。
The polarizing film generally used has a transparent protective film on one or both sides of a polarizer. The polarizer is not particularly limited, and various polarizers can be used. As a polarizer, dichroic substances such as iodine and dichroic dyes are added to hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and partially saponified ethylene-vinyl acetate copolymer films. Polyene-based oriented films such as those obtained by adsorbing and uniaxially stretching, dehydrated polyvinyl alcohol and dehydrochlorinated polyvinyl chloride films, and the like can be mentioned. Among these, a polarizer composed of a polyvinyl alcohol film and a dichroic substance such as iodine is suitable. Although the thickness of these polarizers is not particularly limited, it is generally about 80 μm or less.
また前記偏光子としては厚みが１０μｍ以下の薄型の偏光子を用いることができる。薄型化の観点から言えば当該厚みは１～７μｍであるのが好ましい。このような薄型の偏光子は、厚みムラが少なく、視認性が優れており、また寸法変化が少ないため耐久性に優れ、さらには偏光フィルムとしての厚みも薄型化が図れる点が好ましい。
A thin polarizer having a thickness of 10 μm or less can be used as the polarizer. From the viewpoint of thinning, the thickness is preferably 1 to 7 μm. Such a thin polarizer has less unevenness in thickness, is excellent in visibility, is excellent in durability due to little dimensional change, and is preferable in that the thickness of the polarizing film can be reduced.
前記透明保護フィルムを構成する材料としては、透明性、機械的強度、熱安定性、水分遮断性、等方性等に優れる熱可塑性樹脂が用いられる。このような熱可塑性樹脂の具体例としては、トリアセチルセルロース等のセルロース樹脂、ポリエステル樹脂、ポリエーテルスルホン樹脂、ポリスルホン樹脂、ポリカーボネート樹脂、ポリアミド樹脂、ポリイミド樹脂、ポリオレフィン樹脂、（メタ）アクリル樹脂、環状ポリオレフィン樹脂（ノルボルネン系樹脂）、ポリアリレート樹脂、ポリスチレン樹脂、ポリビニルアルコール樹脂、およびこれらの混合物が挙げられる。なお、偏光子の片側には、透明保護フィルムが接着剤層により貼り合わされるが、他の片側には、透明保護フィルムとして、（メタ）アクリル系、ウレタン系、アクリルウレタン系、エポキシ系、シリコーン系等の熱硬化性樹脂または紫外線硬化型樹脂を用いることができる。透明保護フィルム中には任意の適切な添加剤が１種類以上含まれていてもよい。
A thermoplastic resin that is excellent in transparency, mechanical strength, thermal stability, water barrier properties, isotropy, etc. is used as the material constituting the transparent protective film. Specific examples of such thermoplastic resins include cellulose resins such as triacetyl cellulose, polyester resins, polyethersulfone resins, polysulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, (meth)acrylic resins, cyclic Polyolefin resins (norbornene-based resins), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof. A transparent protective film is attached to one side of the polarizer with an adhesive layer, and a transparent protective film such as (meth)acrylic, urethane, acrylic urethane, epoxy, or silicone film is attached to the other side of the polarizer. A thermosetting resin such as a system or a UV curable resin can be used. One or more of any suitable additives may be contained in the transparent protective film.
前記偏光子と透明保護フィルムの貼り合わせに用いる接着剤は光学的に透明であれば、特に制限されず水系、溶剤系、ホットメルト系、ラジカル硬化型、カチオン硬化型の各種形態のものが用いられるが、水系接着剤またはラジカル硬化型接着剤が好適である。
The adhesive used for bonding the polarizer and the transparent protective film is not particularly limited as long as it is optically transparent. water-based adhesives or radical curing adhesives are preferred.
前記偏光フィルムの厚みは、薄型化の観点から、好ましくは１００μｍ以下、より好ましくは９０μｍ以下、さらに好ましくは７５μｍ以下、さらに好ましくは６０μｍ以下である。
The thickness of the polarizing film is preferably 100 μm or less, more preferably 90 μm or less, even more preferably 75 μm or less, and even more preferably 60 μm or less, from the viewpoint of thinning.
本発明のセパレータを有する粘着剤層付き偏光フィルムにおいて、前記粘着剤層から前記セパレータを剥離する際の剥離力は、セパレータの軽剥離性の観点から、好ましくは０．１２Ｎ／５０ｍｍ以下、より好ましくは０．１０Ｎ／５０ｍｍ以下、さらに好ましくは０．０８Ｎ／５０ｍｍ以下である。
In the polarizing film with a pressure-sensitive adhesive layer having a separator of the present invention, the peel force when peeling the separator from the pressure-sensitive adhesive layer is preferably 0.12 N/50 mm or less, and more preferably 0.12 N/50 mm or less, from the viewpoint of easy peelability of the separator. is 0.10 N/50 mm or less, more preferably 0.08 N/50 mm or less.
本発明のセパレータを有する粘着剤層付き偏光フィルムは、高温耐久性に優れた粘着剤層を有しているため、高温環境下で用いられる画像表示装置、例えば、車載用画像表示装置などに好適に用いられる。
Since the polarizing film with an adhesive layer having the separator of the present invention has an adhesive layer with excellent high temperature durability, it is suitable for image display devices used in high temperature environments, such as in-vehicle image display devices. used for
以下に、本発明の実施例を記載するが、本発明の実施形態はこれらに限定されない。
Examples of the present invention are described below, but embodiments of the present invention are not limited to these.
＜偏光子の作製：厚み１２μｍ＞
平均重合度２４００、ケン化度９９．９モル％、厚さ３０μｍのポリビニルアルコールフィルムを、３０℃の温水中に浸漬し、膨潤させながらＰＶＡ系樹脂フィルムの長さが元長の２．０倍となるように一軸延伸を行った。次いで、０．３重量％（重量比：ヨウ素／ヨウ化カリウム＝０．５／８）の３０℃のヨウ素溶液中に浸漬し、ＰＶＡ系樹脂フィルムの長さが元長の３．０倍となるように一軸延伸しながら染色した。その後、６ホウ酸４重量％、ヨウ化カリウム５重量％の水溶液中で、ＰＶＡ系樹脂フィルムの長さが元長の６倍となるように延伸した。さらに、ヨウ化カリウム３重量％の水溶液（ヨウ素含浸浴）でヨウ素イオン含浸処理を行った後、６０℃のオーブンで４分間乾燥し、厚さ１２μｍの偏光子を得た。 <Preparation of polarizer: thickness 12 μm>
A polyvinyl alcohol film having an average degree of polymerization of 2,400, a degree of saponification of 99.9 mol%, and a thickness of 30 μm is immersed in warm water of 30° C., and while being swollen, the length of the PVA-based resin film becomes 2.0 times its original length. It was uniaxially stretched so as to be. Then, it is immersed in an iodine solution of 0.3% by weight (weight ratio: iodine/potassium iodide = 0.5/8) at 30°C, and the length of the PVA-based resin film becomes 3.0 times the original length. It was dyed while being uniaxially stretched. Thereafter, the PVA-based resin film was stretched in an aqueous solution containing 4% by weight of hexaboric acid and 5% by weight of potassium iodide so that the length of the PVA-based resin film was 6 times its original length. Furthermore, after performing an iodine ion impregnation treatment with an aqueous solution of 3% by weight of potassium iodide (iodine impregnation bath), it was dried in an oven at 60° C. for 4 minutes to obtain a polarizer with a thickness of 12 μm.
平均重合度２４００、ケン化度９９．９モル％、厚さ３０μｍのポリビニルアルコールフィルムを、３０℃の温水中に浸漬し、膨潤させながらＰＶＡ系樹脂フィルムの長さが元長の２．０倍となるように一軸延伸を行った。次いで、０．３重量％（重量比：ヨウ素／ヨウ化カリウム＝０．５／８）の３０℃のヨウ素溶液中に浸漬し、ＰＶＡ系樹脂フィルムの長さが元長の３．０倍となるように一軸延伸しながら染色した。その後、６ホウ酸４重量％、ヨウ化カリウム５重量％の水溶液中で、ＰＶＡ系樹脂フィルムの長さが元長の６倍となるように延伸した。さらに、ヨウ化カリウム３重量％の水溶液（ヨウ素含浸浴）でヨウ素イオン含浸処理を行った後、６０℃のオーブンで４分間乾燥し、厚さ１２μｍの偏光子を得た。 <Preparation of polarizer: thickness 12 μm>
A polyvinyl alcohol film having an average degree of polymerization of 2,400, a degree of saponification of 99.9 mol%, and a thickness of 30 μm is immersed in warm water of 30° C., and while being swollen, the length of the PVA-based resin film becomes 2.0 times its original length. It was uniaxially stretched so as to be. Then, it is immersed in an iodine solution of 0.3% by weight (weight ratio: iodine/potassium iodide = 0.5/8) at 30°C, and the length of the PVA-based resin film becomes 3.0 times the original length. It was dyed while being uniaxially stretched. Thereafter, the PVA-based resin film was stretched in an aqueous solution containing 4% by weight of hexaboric acid and 5% by weight of potassium iodide so that the length of the PVA-based resin film was 6 times its original length. Furthermore, after performing an iodine ion impregnation treatment with an aqueous solution of 3% by weight of potassium iodide (iodine impregnation bath), it was dried in an oven at 60° C. for 4 minutes to obtain a polarizer with a thickness of 12 μm.
＜第１透明保護フィルム＞
基材フィルムとして厚み２５μｍのトリアセチルセルロースフィルムにケン化処理を施したものを用いた。当該基材フィルムの透湿度は１２００ｇ／ｍ２・２４ｈであった。アクリル系ハードコート樹脂（大日本インキ化学工業（株）製、ユニディック１７－８１３）をイソプロピルアルコールに分散させた固形分濃度２５重量％の塗工液を前記基材フィルムの片面に塗布し、８０℃で２分間乾燥させ、さらに紫外線処理することにより、厚さ７μｍのハードコート層（鉛筆硬度３Ｈ）を形成し、ケン化処理を施して用いた。得られた表面処理層付き透明保護フィルムの厚みは３２μｍ、透湿度は４００ｇ／ｍ２・２４ｈであった。 <First transparent protective film>
A saponified triacetyl cellulose film having a thickness of 25 μm was used as the base film. The moisture permeability of the base film was 1200 g/m 2 ·24 h. A coating liquid having a solid content concentration of 25% by weight in which an acrylic hard coat resin (manufactured by Dainippon Ink and Chemicals Co., Ltd., Unidic 17-813) is dispersed in isopropyl alcohol is applied to one side of the base film, It was dried at 80° C. for 2 minutes and then treated with ultraviolet rays to form a 7 μm-thick hard coat layer (pencil hardness of 3H), which was saponified before use. The resulting transparent protective film with a surface treatment layer had a thickness of 32 μm and a moisture permeability of 400 g/m 2 ·24 h.
基材フィルムとして厚み２５μｍのトリアセチルセルロースフィルムにケン化処理を施したものを用いた。当該基材フィルムの透湿度は１２００ｇ／ｍ２・２４ｈであった。アクリル系ハードコート樹脂（大日本インキ化学工業（株）製、ユニディック１７－８１３）をイソプロピルアルコールに分散させた固形分濃度２５重量％の塗工液を前記基材フィルムの片面に塗布し、８０℃で２分間乾燥させ、さらに紫外線処理することにより、厚さ７μｍのハードコート層（鉛筆硬度３Ｈ）を形成し、ケン化処理を施して用いた。得られた表面処理層付き透明保護フィルムの厚みは３２μｍ、透湿度は４００ｇ／ｍ２・２４ｈであった。 <First transparent protective film>
A saponified triacetyl cellulose film having a thickness of 25 μm was used as the base film. The moisture permeability of the base film was 1200 g/m 2 ·24 h. A coating liquid having a solid content concentration of 25% by weight in which an acrylic hard coat resin (manufactured by Dainippon Ink and Chemicals Co., Ltd., Unidic 17-813) is dispersed in isopropyl alcohol is applied to one side of the base film, It was dried at 80° C. for 2 minutes and then treated with ultraviolet rays to form a 7 μm-thick hard coat layer (pencil hardness of 3H), which was saponified before use. The resulting transparent protective film with a surface treatment layer had a thickness of 32 μm and a moisture permeability of 400 g/m 2 ·24 h.
＜第２透明保護フィルム＞
厚さ１３μｍの環状ポリオレフィンフィルム（日本ゼオン社製：ＺＥＯＮＯＲ）にコロナ処理を施して用いた。当該フィルムの透湿度は１２ｇ／ｍ２・２４ｈであった。 <Second transparent protective film>
A cyclic polyolefin film (manufactured by Nippon Zeon Co., Ltd.: ZEONOR) having a thickness of 13 μm was subjected to corona treatment and used. The moisture permeability of the film was 12 g/m 2 ·24 h.
厚さ１３μｍの環状ポリオレフィンフィルム（日本ゼオン社製：ＺＥＯＮＯＲ）にコロナ処理を施して用いた。当該フィルムの透湿度は１２ｇ／ｍ２・２４ｈであった。 <Second transparent protective film>
A cyclic polyolefin film (manufactured by Nippon Zeon Co., Ltd.: ZEONOR) having a thickness of 13 μm was subjected to corona treatment and used. The moisture permeability of the film was 12 g/m 2 ·24 h.
＜透湿度＞
ＪＩＳ Ｚ０２０８に記載の防湿包装材料の透湿度試験方法（カップ法）に基づいて測定した。 <Moisture permeability>
It was measured based on the moisture permeability test method (cup method) for moisture-proof packaging materials described in JIS Z0208.
ＪＩＳ Ｚ０２０８に記載の防湿包装材料の透湿度試験方法（カップ法）に基づいて測定した。 <Moisture permeability>
It was measured based on the moisture permeability test method (cup method) for moisture-proof packaging materials described in JIS Z0208.
＜偏光フィルムの作製＞
上記偏光子（厚み１２μｍ）の両面に、水系接着剤層の厚さが０．１μｍになるようにポリビニルアルコール系接着剤を塗布しながら、上記第１透明保護フィルム（表面処理層を設けていない側）および第２透明保護フィルムを貼合せたのち、５０℃で５分間の乾燥を行って偏光フィルム（厚み：５７μｍ）を作製した。 <Preparation of polarizing film>
While applying a polyvinyl alcohol-based adhesive to both sides of the polarizer (thickness 12 μm) so that the thickness of the water-based adhesive layer is 0.1 μm, the first transparent protective film (no surface treatment layer is provided side) and the second transparent protective film, and dried at 50° C. for 5 minutes to prepare a polarizing film (thickness: 57 μm).
上記偏光子（厚み１２μｍ）の両面に、水系接着剤層の厚さが０．１μｍになるようにポリビニルアルコール系接着剤を塗布しながら、上記第１透明保護フィルム（表面処理層を設けていない側）および第２透明保護フィルムを貼合せたのち、５０℃で５分間の乾燥を行って偏光フィルム（厚み：５７μｍ）を作製した。 <Preparation of polarizing film>
While applying a polyvinyl alcohol-based adhesive to both sides of the polarizer (thickness 12 μm) so that the thickness of the water-based adhesive layer is 0.1 μm, the first transparent protective film (no surface treatment layer is provided side) and the second transparent protective film, and dried at 50° C. for 5 minutes to prepare a polarizing film (thickness: 57 μm).
＜アクリル系ポリマー溶液（Ａ）の調製＞
冷却管、窒素導入管、温度計及び撹拌装置を備えた反応容器に、アクリル酸ブチル１００部、アクリル酸５部、アクリル酸２－ヒドロキシエチル０．０７５部および２，２´－アゾビスイソブチロニトリル０．３部を酢酸エチルと共に加えて溶液を調製した。次いで、この溶液に窒素ガスを吹き込みながら撹拌して、６０℃で４時間反応させて、重量平均分子量２２０万のアクリル系ポリマーを含有する溶液を得た。さらに、このアクリル系ポリマーを含有する溶液に、酢酸エチルを加えて固形分濃度を３０％に調整したアクリル系ポリマー溶液（Ａ）を得た。 <Preparation of acrylic polymer solution (A)>
100 parts of butyl acrylate, 5 parts of acrylic acid, 0.075 parts of 2-hydroxyethyl acrylate and 2,2'-azobisisobutyl are added to a reaction vessel equipped with a condenser, nitrogen inlet, thermometer and stirrer. A solution was prepared by adding 0.3 parts of lonitrile along with ethyl acetate. Next, this solution was stirred while blowing nitrogen gas, and reacted at 60° C. for 4 hours to obtain a solution containing an acrylic polymer having a weight-average molecular weight of 2,200,000. Furthermore, an acrylic polymer solution (A) was obtained by adding ethyl acetate to the solution containing the acrylic polymer to adjust the solid content concentration to 30%.
冷却管、窒素導入管、温度計及び撹拌装置を備えた反応容器に、アクリル酸ブチル１００部、アクリル酸５部、アクリル酸２－ヒドロキシエチル０．０７５部および２，２´－アゾビスイソブチロニトリル０．３部を酢酸エチルと共に加えて溶液を調製した。次いで、この溶液に窒素ガスを吹き込みながら撹拌して、６０℃で４時間反応させて、重量平均分子量２２０万のアクリル系ポリマーを含有する溶液を得た。さらに、このアクリル系ポリマーを含有する溶液に、酢酸エチルを加えて固形分濃度を３０％に調整したアクリル系ポリマー溶液（Ａ）を得た。 <Preparation of acrylic polymer solution (A)>
100 parts of butyl acrylate, 5 parts of acrylic acid, 0.075 parts of 2-hydroxyethyl acrylate and 2,2'-azobisisobutyl are added to a reaction vessel equipped with a condenser, nitrogen inlet, thermometer and stirrer. A solution was prepared by adding 0.3 parts of lonitrile along with ethyl acetate. Next, this solution was stirred while blowing nitrogen gas, and reacted at 60° C. for 4 hours to obtain a solution containing an acrylic polymer having a weight-average molecular weight of 2,200,000. Furthermore, an acrylic polymer solution (A) was obtained by adding ethyl acetate to the solution containing the acrylic polymer to adjust the solid content concentration to 30%.
＜粘着剤組成物（Ａ－１）～（Ａ－４）の調製＞
前記アクリル系ポリマー溶液（Ａ）の固形分１００部に対して、架橋剤として、０．６部のイソシアネート基を有する化合物を主成分とする架橋剤（日本ポリウレタン（株）製、商品名「コロネートＬ」）と、シランカップリング剤として、０．０７５部のγ－グリシドキシプロピルトリメトキシシラン（信越化学工業（株）製、商品名「ＫＭＢ－４０３」）と、導電剤として、３部のリチウムビス（トリフルオロメタンスルホニル）イミド（三菱マテリアル電子化成（株）製）をこの順に配合して、粘着剤組成物（Ａ－１）を調製した。また、前記導電剤の配合量を６部、０．３部、０部に変更した以外は上記と同様の方法で粘着剤組成物（Ａ－２）～（Ａ－４）を調製した。 <Preparation of adhesive compositions (A-1) to (A-4)>
0.6 parts of a cross-linking agent based on a compound having an isocyanate group (manufactured by Nippon Polyurethane Co., Ltd., trade name "Coronate L”), 0.075 parts of γ-glycidoxypropyltrimethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd., trade name “KMB-403”) as a silane coupling agent, and 3 parts as a conductive agent. Lithium bis(trifluoromethanesulfonyl)imide (manufactured by Mitsubishi Materials Electronic Chemicals Co., Ltd.) was blended in this order to prepare an adhesive composition (A-1). Further, pressure-sensitive adhesive compositions (A-2) to (A-4) were prepared in the same manner as described above, except that the amount of the conductive agent was changed to 6 parts, 0.3 parts, and 0 parts.
前記アクリル系ポリマー溶液（Ａ）の固形分１００部に対して、架橋剤として、０．６部のイソシアネート基を有する化合物を主成分とする架橋剤（日本ポリウレタン（株）製、商品名「コロネートＬ」）と、シランカップリング剤として、０．０７５部のγ－グリシドキシプロピルトリメトキシシラン（信越化学工業（株）製、商品名「ＫＭＢ－４０３」）と、導電剤として、３部のリチウムビス（トリフルオロメタンスルホニル）イミド（三菱マテリアル電子化成（株）製）をこの順に配合して、粘着剤組成物（Ａ－１）を調製した。また、前記導電剤の配合量を６部、０．３部、０部に変更した以外は上記と同様の方法で粘着剤組成物（Ａ－２）～（Ａ－４）を調製した。 <Preparation of adhesive compositions (A-1) to (A-4)>
0.6 parts of a cross-linking agent based on a compound having an isocyanate group (manufactured by Nippon Polyurethane Co., Ltd., trade name "Coronate L”), 0.075 parts of γ-glycidoxypropyltrimethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd., trade name “KMB-403”) as a silane coupling agent, and 3 parts as a conductive agent. Lithium bis(trifluoromethanesulfonyl)imide (manufactured by Mitsubishi Materials Electronic Chemicals Co., Ltd.) was blended in this order to prepare an adhesive composition (A-1). Further, pressure-sensitive adhesive compositions (A-2) to (A-4) were prepared in the same manner as described above, except that the amount of the conductive agent was changed to 6 parts, 0.3 parts, and 0 parts.
＜アクリル系ポリマー溶液（Ｂ）の調製＞
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた４つ口フラスコに、ブチルアクリレート７９．７部、フェノキシエチルアクリレート１６部、Ｎ－ビニル－２－ピロリドン３部、アクリル酸０．３部、および４－ヒドロキシブチルアクリレート１部を含有するモノマー混合物を仕込んだ。さらに、前記モノマー混合物（固形分）１００部に対して、重合開始剤として２，２’－アゾビスイソブチロニトリル０．１部を酢酸エチル１００部と共に仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を５５℃付近に保って８時間重合反応を行って、重量平均分子量（Ｍｗ）１８０万のアクリル系ポリマーを含有する溶液（Ｂ）を調製した。 <Preparation of acrylic polymer solution (B)>
79.7 parts of butyl acrylate, 16 parts of phenoxyethyl acrylate, 3 parts of N-vinyl-2-pyrrolidone, and 0.3 parts of acrylic acid were placed in a four-necked flask equipped with a stirring blade, a thermometer, a nitrogen gas inlet tube, and a condenser. and 1 part of 4-hydroxybutyl acrylate were charged. Further, 0.1 part of 2,2′-azobisisobutyronitrile as a polymerization initiator was added to 100 parts of the monomer mixture (solid content) together with 100 parts of ethyl acetate, and nitrogen gas was introduced while gently stirring. After introducing and purging with nitrogen, the liquid temperature in the flask was maintained at around 55° C. and polymerization reaction was carried out for 8 hours to prepare a solution (B) containing an acrylic polymer having a weight average molecular weight (Mw) of 1,800,000. .
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた４つ口フラスコに、ブチルアクリレート７９．７部、フェノキシエチルアクリレート１６部、Ｎ－ビニル－２－ピロリドン３部、アクリル酸０．３部、および４－ヒドロキシブチルアクリレート１部を含有するモノマー混合物を仕込んだ。さらに、前記モノマー混合物（固形分）１００部に対して、重合開始剤として２，２’－アゾビスイソブチロニトリル０．１部を酢酸エチル１００部と共に仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を５５℃付近に保って８時間重合反応を行って、重量平均分子量（Ｍｗ）１８０万のアクリル系ポリマーを含有する溶液（Ｂ）を調製した。 <Preparation of acrylic polymer solution (B)>
79.7 parts of butyl acrylate, 16 parts of phenoxyethyl acrylate, 3 parts of N-vinyl-2-pyrrolidone, and 0.3 parts of acrylic acid were placed in a four-necked flask equipped with a stirring blade, a thermometer, a nitrogen gas inlet tube, and a condenser. and 1 part of 4-hydroxybutyl acrylate were charged. Further, 0.1 part of 2,2′-azobisisobutyronitrile as a polymerization initiator was added to 100 parts of the monomer mixture (solid content) together with 100 parts of ethyl acetate, and nitrogen gas was introduced while gently stirring. After introducing and purging with nitrogen, the liquid temperature in the flask was maintained at around 55° C. and polymerization reaction was carried out for 8 hours to prepare a solution (B) containing an acrylic polymer having a weight average molecular weight (Mw) of 1,800,000. .
＜粘着剤組成物（Ｂ）の調製＞
前記アクリル系ポリマー溶液（Ｂ）の固形分１００部に対して、イソシアネート架橋剤（三井化学社製のタケネートＤ１６０Ｎ、トリメチロールプロパンヘキサメチレンジイソシアネート）０．２部、ベンゾイルパーオキサイド（日本油脂社製のナイパーＢＭＴ）０．２部、導電剤として、リチウムビス（トリフルオロメタンスルホニル）イミド（三菱マテリアル電子化成（株）製）６部、およびアセトアセチル基含有シランカップリング剤（商品名：Ａ－１００、綜研化学（株）製）０．２部を配合して、粘着剤組成物（Ｂ）を調製した。 <Preparation of adhesive composition (B)>
Per 100 parts of the solid content of the acrylic polymer solution (B), isocyanate cross-linking agent (Mitsui Chemical Takenate D160N, trimethylolpropane hexamethylene diisocyanate) 0.2 parts, benzoyl peroxide (NOF Co., Ltd. Nyper BMT) 0.2 parts, as a conductive agent, lithium bis (trifluoromethanesulfonyl) imide (manufactured by Mitsubishi Materials Electronic Chemicals Co., Ltd.) 6 parts, and an acetoacetyl group-containing silane coupling agent (trade name: A-100, Soken Chemical Co., Ltd.) was blended to prepare an adhesive composition (B).
前記アクリル系ポリマー溶液（Ｂ）の固形分１００部に対して、イソシアネート架橋剤（三井化学社製のタケネートＤ１６０Ｎ、トリメチロールプロパンヘキサメチレンジイソシアネート）０．２部、ベンゾイルパーオキサイド（日本油脂社製のナイパーＢＭＴ）０．２部、導電剤として、リチウムビス（トリフルオロメタンスルホニル）イミド（三菱マテリアル電子化成（株）製）６部、およびアセトアセチル基含有シランカップリング剤（商品名：Ａ－１００、綜研化学（株）製）０．２部を配合して、粘着剤組成物（Ｂ）を調製した。 <Preparation of adhesive composition (B)>
Per 100 parts of the solid content of the acrylic polymer solution (B), isocyanate cross-linking agent (Mitsui Chemical Takenate D160N, trimethylolpropane hexamethylene diisocyanate) 0.2 parts, benzoyl peroxide (NOF Co., Ltd. Nyper BMT) 0.2 parts, as a conductive agent, lithium bis (trifluoromethanesulfonyl) imide (manufactured by Mitsubishi Materials Electronic Chemicals Co., Ltd.) 6 parts, and an acetoacetyl group-containing silane coupling agent (trade name: A-100, Soken Chemical Co., Ltd.) was blended to prepare an adhesive composition (B).
＜セパレータＸの作製＞
〔オリゴマー防止層の形成〕
シリカ系材料として、オルガノシロキサン（エチルシリケート４８：コルコート社）をイソプロピルアルコールで固形分濃度１％に希釈して塗布液を調製した。得られた塗布液を、基材フィルムとしてのポリエステルフィルム（厚み：３８μｍ）上に、乾燥後の厚みが５０ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、オリゴマー防止層を形成した。 <Preparation of Separator X>
[Formation of oligomer prevention layer]
As a silica-based material, organosiloxane (Ethyl Silicate 48: Colcoat Co.) was diluted with isopropyl alcohol to a solid concentration of 1% to prepare a coating liquid. The obtained coating solution was applied on a polyester film (thickness: 38 μm) as a base film by a gravure coater so that the thickness after drying was 50 nm, and then dried at 120° C. for 30 seconds to prevent oligomers. formed a layer.
〔オリゴマー防止層の形成〕
シリカ系材料として、オルガノシロキサン（エチルシリケート４８：コルコート社）をイソプロピルアルコールで固形分濃度１％に希釈して塗布液を調製した。得られた塗布液を、基材フィルムとしてのポリエステルフィルム（厚み：３８μｍ）上に、乾燥後の厚みが５０ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、オリゴマー防止層を形成した。 <Preparation of Separator X>
[Formation of oligomer prevention layer]
As a silica-based material, organosiloxane (Ethyl Silicate 48: Colcoat Co.) was diluted with isopropyl alcohol to a solid concentration of 1% to prepare a coating liquid. The obtained coating solution was applied on a polyester film (thickness: 38 μm) as a base film by a gravure coater so that the thickness after drying was 50 nm, and then dried at 120° C. for 30 seconds to prevent oligomers. formed a layer.
〔離型層の形成〕
反応性官能基を有する反応性シリコーン樹脂（ＬＴＣ８５６：東レ・ダウコーニング製）２０部、重量平均分子量４０００００の非反応性シリコーン樹脂（ＢＹ２４－８５０：東レ・ダウコーニング製）１３．５部、及び硬化剤（ＳＲＸ－２１２ｃａｔ：東レ・ダウコーニング製）０．２部を、メチルエチルケトン／トルエン混合溶媒（混合比率は１：１）３５０部で希釈して、シリコーン系離型剤の溶液を調製した。得られたシリコーン系離型剤の溶液を、オリゴマー防止層の上に、乾燥後の厚みが１２０ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、離型層を形成して、ポリエステルフィルム／オリゴマー防止層／離型層の構成を有するセパレータＸを作製した。形成した離型層において、前記反応性シリコーン樹脂と前記非反応性シリコーン樹脂の合計含有量１００質量％中、前記反応性シリコーン樹脂の含有量は６０質量％、前記非反応性シリコーン樹脂の含有量は４０質量％である。 [Formation of release layer]
20 parts of a reactive silicone resin having a reactive functional group (LTC856: Dow Corning Toray), 13.5 parts of a non-reactive silicone resin with a weight average molecular weight of 400000 (BY24-850: Dow Corning Toray), and curing 0.2 part of the release agent (SRX-212cat, manufactured by Dow Corning Toray) was diluted with 350 parts of a mixed solvent of methyl ethyl ketone/toluene (mixing ratio: 1:1) to prepare a solution of a silicone release agent. The obtained solution of the silicone-based release agent was applied on the oligomer-preventing layer by a gravure coater so that the thickness after drying was 120 nm, and then dried at 120°C for 30 seconds to form a release layer. Thus, a separator X having a configuration of polyester film/oligomer prevention layer/releasing layer was produced. In the formed release layer, the content of the reactive silicone resin is 60% by mass, and the content of the non-reactive silicone resin is 100% by mass in the total content of the reactive silicone resin and the non-reactive silicone resin. is 40% by mass.
反応性官能基を有する反応性シリコーン樹脂（ＬＴＣ８５６：東レ・ダウコーニング製）２０部、重量平均分子量４０００００の非反応性シリコーン樹脂（ＢＹ２４－８５０：東レ・ダウコーニング製）１３．５部、及び硬化剤（ＳＲＸ－２１２ｃａｔ：東レ・ダウコーニング製）０．２部を、メチルエチルケトン／トルエン混合溶媒（混合比率は１：１）３５０部で希釈して、シリコーン系離型剤の溶液を調製した。得られたシリコーン系離型剤の溶液を、オリゴマー防止層の上に、乾燥後の厚みが１２０ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、離型層を形成して、ポリエステルフィルム／オリゴマー防止層／離型層の構成を有するセパレータＸを作製した。形成した離型層において、前記反応性シリコーン樹脂と前記非反応性シリコーン樹脂の合計含有量１００質量％中、前記反応性シリコーン樹脂の含有量は６０質量％、前記非反応性シリコーン樹脂の含有量は４０質量％である。 [Formation of release layer]
20 parts of a reactive silicone resin having a reactive functional group (LTC856: Dow Corning Toray), 13.5 parts of a non-reactive silicone resin with a weight average molecular weight of 400000 (BY24-850: Dow Corning Toray), and curing 0.2 part of the release agent (SRX-212cat, manufactured by Dow Corning Toray) was diluted with 350 parts of a mixed solvent of methyl ethyl ketone/toluene (mixing ratio: 1:1) to prepare a solution of a silicone release agent. The obtained solution of the silicone-based release agent was applied on the oligomer-preventing layer by a gravure coater so that the thickness after drying was 120 nm, and then dried at 120°C for 30 seconds to form a release layer. Thus, a separator X having a configuration of polyester film/oligomer prevention layer/releasing layer was produced. In the formed release layer, the content of the reactive silicone resin is 60% by mass, and the content of the non-reactive silicone resin is 100% by mass in the total content of the reactive silicone resin and the non-reactive silicone resin. is 40% by mass.
＜セパレータＹの作製＞
〔オリゴマー防止層の形成〕
シリカ系材料として、オルガノシロキサン（エチルシリケート４８：コルコート社）をイソプロピルアルコールで固形分濃度１％に希釈して塗布液を調製した。得られた塗布液を、基材フィルムとしてのポリエステルフィルム（厚み：３８μｍ）上に、乾燥後の厚みが５０ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、オリゴマー防止層を形成した。 <Preparation of Separator Y>
[Formation of oligomer prevention layer]
As a silica-based material, organosiloxane (Ethyl Silicate 48: Colcoat Co.) was diluted with isopropyl alcohol to a solid concentration of 1% to prepare a coating liquid. The obtained coating solution was applied on a polyester film (thickness: 38 μm) as a base film by a gravure coater so that the thickness after drying was 50 nm, and then dried at 120° C. for 30 seconds to prevent oligomers. formed a layer.
〔オリゴマー防止層の形成〕
シリカ系材料として、オルガノシロキサン（エチルシリケート４８：コルコート社）をイソプロピルアルコールで固形分濃度１％に希釈して塗布液を調製した。得られた塗布液を、基材フィルムとしてのポリエステルフィルム（厚み：３８μｍ）上に、乾燥後の厚みが５０ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、オリゴマー防止層を形成した。 <Preparation of Separator Y>
[Formation of oligomer prevention layer]
As a silica-based material, organosiloxane (Ethyl Silicate 48: Colcoat Co.) was diluted with isopropyl alcohol to a solid concentration of 1% to prepare a coating liquid. The obtained coating solution was applied on a polyester film (thickness: 38 μm) as a base film by a gravure coater so that the thickness after drying was 50 nm, and then dried at 120° C. for 30 seconds to prevent oligomers. formed a layer.
〔離型層の形成〕
反応性官能基を有する反応性シリコーン樹脂（ＫＳ－８４７Ｈ：信越化学製）２０部及び硬化剤（ＰＬ－５０Ｔ：信越化学製）０．２部を、メチルエチルケトン／トルエン混合溶媒（混合比率は１：１）３５０部で希釈して、シリコーン系離型剤の溶液を調製した。得られたシリコーン系離型剤の溶液を、オリゴマー防止層の上に、乾燥後の厚みが１００ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、離型層を形成して、ポリエステルフィルム／オリゴマー防止層／離型層の構成を有するセパレータＹを作製した。 [Formation of release layer]
20 parts of a reactive silicone resin having a reactive functional group (KS-847H: manufactured by Shin-Etsu Chemical Co., Ltd.) and 0.2 parts of a curing agent (PL-50T: manufactured by Shin-Etsu Chemical Co., Ltd.) are added to a mixed solvent of methyl ethyl ketone / toluene (mixing ratio is 1: 1) Dilute with 350 parts to prepare a solution of a silicone release agent. The resulting solution of the silicone-based release agent is applied onto the oligomer-preventing layer by a gravure coater so that the thickness after drying becomes 100 nm, and then dried at 120° C. for 30 seconds to form a release layer. Thus, a separator Y having a configuration of polyester film/oligomer-preventing layer/releasing layer was produced.
反応性官能基を有する反応性シリコーン樹脂（ＫＳ－８４７Ｈ：信越化学製）２０部及び硬化剤（ＰＬ－５０Ｔ：信越化学製）０．２部を、メチルエチルケトン／トルエン混合溶媒（混合比率は１：１）３５０部で希釈して、シリコーン系離型剤の溶液を調製した。得られたシリコーン系離型剤の溶液を、オリゴマー防止層の上に、乾燥後の厚みが１００ｎｍになるようにグラビアコーターにより塗布した後、１２０℃で３０秒乾燥して、離型層を形成して、ポリエステルフィルム／オリゴマー防止層／離型層の構成を有するセパレータＹを作製した。 [Formation of release layer]
20 parts of a reactive silicone resin having a reactive functional group (KS-847H: manufactured by Shin-Etsu Chemical Co., Ltd.) and 0.2 parts of a curing agent (PL-50T: manufactured by Shin-Etsu Chemical Co., Ltd.) are added to a mixed solvent of methyl ethyl ketone / toluene (mixing ratio is 1: 1) Dilute with 350 parts to prepare a solution of a silicone release agent. The resulting solution of the silicone-based release agent is applied onto the oligomer-preventing layer by a gravure coater so that the thickness after drying becomes 100 nm, and then dried at 120° C. for 30 seconds to form a release layer. Thus, a separator Y having a configuration of polyester film/oligomer-preventing layer/releasing layer was produced.
実施例１
＜セパレータを有する粘着剤層付き偏光フィルムの作製＞
粘着剤組成物（Ａ－１）をセパレータＸの離型層の表面に、ファウンテンコータで均一に塗工し、１５５℃の空気循環式恒温オーブンで２分間乾燥し、厚さ２０μｍの粘着剤層を形成してセパレータ付き粘着剤層を作製した。次いで、作製した偏光フィルムの第２透明保護フィルムに、作製したセパレータ付き粘着剤層の粘着剤層を貼り合わせてセパレータを有する粘着剤層付き偏光フィルムを作製した。 Example 1
<Preparation of a polarizing film with a pressure-sensitive adhesive layer having a separator>
The pressure-sensitive adhesive composition (A-1) is uniformly applied to the surface of the release layer of the separator X with a fountain coater, dried in an air circulation constant temperature oven at 155 ° C. for 2 minutes, and a pressure-sensitive adhesive layer having a thickness of 20 μm. was formed to prepare a pressure-sensitive adhesive layer with a separator. Then, the pressure-sensitive adhesive layer of the prepared pressure-sensitive adhesive layer with a separator was attached to the second transparent protective film of the prepared polarizing film to prepare a polarizing film with a pressure-sensitive adhesive layer having a separator.
＜セパレータを有する粘着剤層付き偏光フィルムの作製＞
粘着剤組成物（Ａ－１）をセパレータＸの離型層の表面に、ファウンテンコータで均一に塗工し、１５５℃の空気循環式恒温オーブンで２分間乾燥し、厚さ２０μｍの粘着剤層を形成してセパレータ付き粘着剤層を作製した。次いで、作製した偏光フィルムの第２透明保護フィルムに、作製したセパレータ付き粘着剤層の粘着剤層を貼り合わせてセパレータを有する粘着剤層付き偏光フィルムを作製した。 Example 1
<Preparation of a polarizing film with a pressure-sensitive adhesive layer having a separator>
The pressure-sensitive adhesive composition (A-1) is uniformly applied to the surface of the release layer of the separator X with a fountain coater, dried in an air circulation constant temperature oven at 155 ° C. for 2 minutes, and a pressure-sensitive adhesive layer having a thickness of 20 μm. was formed to prepare a pressure-sensitive adhesive layer with a separator. Then, the pressure-sensitive adhesive layer of the prepared pressure-sensitive adhesive layer with a separator was attached to the second transparent protective film of the prepared polarizing film to prepare a polarizing film with a pressure-sensitive adhesive layer having a separator.
実施例２～４、比較例１～５
＜セパレータを有する粘着剤層付き偏光フィルムの作製＞
表１に記載の粘着剤組成物及びセパレータを用いた以外は、実施例１と同様の方法でセパレータを有する粘着剤層付き偏光フィルムを作製した。 Examples 2-4, Comparative Examples 1-5
<Preparation of a polarizing film with a pressure-sensitive adhesive layer having a separator>
A polarizing film with a pressure-sensitive adhesive layer having a separator was produced in the same manner as in Example 1 except that the pressure-sensitive adhesive composition and separator shown in Table 1 were used.
＜セパレータを有する粘着剤層付き偏光フィルムの作製＞
表１に記載の粘着剤組成物及びセパレータを用いた以外は、実施例１と同様の方法でセパレータを有する粘着剤層付き偏光フィルムを作製した。 Examples 2-4, Comparative Examples 1-5
<Preparation of a polarizing film with a pressure-sensitive adhesive layer having a separator>
A polarizing film with a pressure-sensitive adhesive layer having a separator was produced in the same manner as in Example 1 except that the pressure-sensitive adhesive composition and separator shown in Table 1 were used.
＜測定・評価方法＞
（離型層の弾性率）
作製したセパレータの基材フィルム側の面を、両面粘着テープを用いてステンレス製の試料台に貼り合せた。続いて、シリコンプローブ（オリンパス社製、製品名「ＡＣ２４０ＴＳ」、曲率半径：1０ｎｍ、バネ定数：３Ｎ／ｍ相当品）を装着したプローブ顕微鏡（オックスフォード・インストゥルメンツ株式会社製、製品名「アサイラムリサーチＭＦＰ－３Ｄ－ＳＡ」）を用いて、セパレータの離型層側の面を１Ｈｚでフォースカーブ測定を行い、荷重－変位曲線を得た。得られた荷重－変位曲線から、ＪＫＲ２点法により、離型層の弾性率（ＭＰａ）を算出した。 <Measurement/evaluation method>
(Elastic modulus of release layer)
The base film side surface of the produced separator was attached to a stainless steel sample table using a double-sided adhesive tape. Subsequently, a probe microscope (manufactured by Oxford Instruments Co., Ltd., product name "Asylum Research MFP-3D-SA”), force curve measurement was performed on the release layer side surface of the separator at 1 Hz to obtain a load-displacement curve. From the obtained load-displacement curve, the elastic modulus (MPa) of the release layer was calculated by the JKR two-point method.
（離型層の弾性率）
作製したセパレータの基材フィルム側の面を、両面粘着テープを用いてステンレス製の試料台に貼り合せた。続いて、シリコンプローブ（オリンパス社製、製品名「ＡＣ２４０ＴＳ」、曲率半径：1０ｎｍ、バネ定数：３Ｎ／ｍ相当品）を装着したプローブ顕微鏡（オックスフォード・インストゥルメンツ株式会社製、製品名「アサイラムリサーチＭＦＰ－３Ｄ－ＳＡ」）を用いて、セパレータの離型層側の面を１Ｈｚでフォースカーブ測定を行い、荷重－変位曲線を得た。得られた荷重－変位曲線から、ＪＫＲ２点法により、離型層の弾性率（ＭＰａ）を算出した。 <Measurement/evaluation method>
(Elastic modulus of release layer)
The base film side surface of the produced separator was attached to a stainless steel sample table using a double-sided adhesive tape. Subsequently, a probe microscope (manufactured by Oxford Instruments Co., Ltd., product name "Asylum Research MFP-3D-SA”), force curve measurement was performed on the release layer side surface of the separator at 1 Hz to obtain a load-displacement curve. From the obtained load-displacement curve, the elastic modulus (MPa) of the release layer was calculated by the JKR two-point method.
（粘着力）
作製した粘着剤層付き偏光フィルムを、縦１２０ｍｍ×横２５ｍｍに裁断したものをサンプルとした。当該サンプルを、厚さ０．７ｍｍの無アルカリガラス板（コーニング社製、ＥＧ－ＸＧ）に、ラミネーターを用いて貼り付け、次いで５０℃、５ａｔｍで１５分間オートクレーブ処理して完全に密着させた後、かかるサンプルの粘着力を測定した。粘着力は、かかるサンプルを引張り試験機（オートグラフＳＨＩＭＡＺＵＡＧ－１ １ＯＫＮ）にて、剥離角度９０°、剥離速度３００ｍｍ／ｍｉｎで引き剥がす際の粘着力（Ｎ／２５ｍｍ、測定長８０ｍｍ）を測定することにより求めた。測定は、１回／０．５ｓの間隔で２００回サンプリングし、その平均値を測定値とした。サンプル数は３とした。 (Adhesive force)
A sample was prepared by cutting the produced polarizing film with an adhesive layer into a size of 120 mm long×25 mm wide. The sample was attached to an alkali-free glass plate (manufactured by Corning, EG-XG) with a thickness of 0.7 mm using a laminator, and then autoclaved at 50 ° C. and 5 atm for 15 minutes. , the adhesion of such samples was measured. The adhesive strength is measured by peeling off such a sample with a tensile tester (Autograph SHIMAZUAG-1 1OKN) at a peeling angle of 90 ° and a peeling speed of 300 mm / min (N / 25 mm, measuring length 80 mm). I asked for it. The measurement was sampled 200 times at an interval of 1 time/0.5 s, and the average value was used as the measured value. The number of samples was 3.
作製した粘着剤層付き偏光フィルムを、縦１２０ｍｍ×横２５ｍｍに裁断したものをサンプルとした。当該サンプルを、厚さ０．７ｍｍの無アルカリガラス板（コーニング社製、ＥＧ－ＸＧ）に、ラミネーターを用いて貼り付け、次いで５０℃、５ａｔｍで１５分間オートクレーブ処理して完全に密着させた後、かかるサンプルの粘着力を測定した。粘着力は、かかるサンプルを引張り試験機（オートグラフＳＨＩＭＡＺＵＡＧ－１ １ＯＫＮ）にて、剥離角度９０°、剥離速度３００ｍｍ／ｍｉｎで引き剥がす際の粘着力（Ｎ／２５ｍｍ、測定長８０ｍｍ）を測定することにより求めた。測定は、１回／０．５ｓの間隔で２００回サンプリングし、その平均値を測定値とした。サンプル数は３とした。 (Adhesive force)
A sample was prepared by cutting the produced polarizing film with an adhesive layer into a size of 120 mm long×25 mm wide. The sample was attached to an alkali-free glass plate (manufactured by Corning, EG-XG) with a thickness of 0.7 mm using a laminator, and then autoclaved at 50 ° C. and 5 atm for 15 minutes. , the adhesion of such samples was measured. The adhesive strength is measured by peeling off such a sample with a tensile tester (Autograph SHIMAZUAG-1 1OKN) at a peeling angle of 90 ° and a peeling speed of 300 mm / min (N / 25 mm, measuring length 80 mm). I asked for it. The measurement was sampled 200 times at an interval of 1 time/0.5 s, and the average value was used as the measured value. The number of samples was 3.
（セパレータの剥離力）
作製したセパレータを有する粘着剤層付き偏光フィルムを５０ｍｍ×１００ｍｍの大きさに切断して測定用サンプルとした。測定用サンプルの表面処理側を下にして、両面粘着テープを介して平板状の剥離治具に貼り合せた。次いで、セパレータを粘着剤層の表面から１０ｍｍ剥離し、剥離したセパレータをチャックし、引張り試験機を用いて引張り、剥離力（Ｎ／５０ｍｍ）の測定を行った（引張方向：偏光フィルムの表面に対して１８０°、引張速度：３００ｍｍ／ｍｉｎ）。１回／０．５ｓの間隔で２００回サンプリングし、その平均値を測定値とした。サンプル数は３とした。また、下記基準で評価した。
◎：０．０８以下
〇：０．０８超０．１１以下
△：０．１１超０．１３未満
×：０．１３以上 (Peeling force of separator)
The produced polarizing film with an adhesive layer having a separator was cut into a size of 50 mm×100 mm to obtain a measurement sample. With the surface-treated side of the measurement sample facing downward, it was attached to a flat peeling jig via a double-sided adhesive tape. Next, the separator was peeled off 10 mm from the surface of the adhesive layer, the peeled separator was chucked, and pulled using a tensile tester, and the peel force (N / 50 mm) was measured (pulling direction: on the surface of the polarizing film 180°, tension speed: 300 mm/min). Sampling was performed 200 times at an interval of 1 time/0.5 s, and the average value was used as the measured value. The number of samples was 3. Moreover, it evaluated by the following reference|standard.
◎: 0.08 or less ○: 0.08 to 0.11 or less △: 0.11 to less than 0.13 ×: 0.13 or more
作製したセパレータを有する粘着剤層付き偏光フィルムを５０ｍｍ×１００ｍｍの大きさに切断して測定用サンプルとした。測定用サンプルの表面処理側を下にして、両面粘着テープを介して平板状の剥離治具に貼り合せた。次いで、セパレータを粘着剤層の表面から１０ｍｍ剥離し、剥離したセパレータをチャックし、引張り試験機を用いて引張り、剥離力（Ｎ／５０ｍｍ）の測定を行った（引張方向：偏光フィルムの表面に対して１８０°、引張速度：３００ｍｍ／ｍｉｎ）。１回／０．５ｓの間隔で２００回サンプリングし、その平均値を測定値とした。サンプル数は３とした。また、下記基準で評価した。
◎：０．０８以下
〇：０．０８超０．１１以下
△：０．１１超０．１３未満
×：０．１３以上 (Peeling force of separator)
The produced polarizing film with an adhesive layer having a separator was cut into a size of 50 mm×100 mm to obtain a measurement sample. With the surface-treated side of the measurement sample facing downward, it was attached to a flat peeling jig via a double-sided adhesive tape. Next, the separator was peeled off 10 mm from the surface of the adhesive layer, the peeled separator was chucked, and pulled using a tensile tester, and the peel force (N / 50 mm) was measured (pulling direction: on the surface of the polarizing film 180°, tension speed: 300 mm/min). Sampling was performed 200 times at an interval of 1 time/0.5 s, and the average value was used as the measured value. The number of samples was 3. Moreover, it evaluated by the following reference|standard.
◎: 0.08 or less ○: 0.08 to 0.11 or less △: 0.11 to less than 0.13 ×: 0.13 or more
（粘着剤層の表面抵抗値）
粘着剤層の表面抵抗値（Ω／□）は三菱化学アナリテック社製のＭＣＰ－ＨＴ４５０を用いて測定した。また、下記基準で評価した。
◎：１０１０以下
〇：１０１１～１０１２
×：Ｏｖｅｒ (Surface resistance value of adhesive layer)
The surface resistance value (Ω/□) of the adhesive layer was measured using MCP-HT450 manufactured by Mitsubishi Chemical Analytic Tech. Moreover, it evaluated by the following reference|standard.
◎: 10 10 or less ○: 10 11 to 10 12
×: Over
粘着剤層の表面抵抗値（Ω／□）は三菱化学アナリテック社製のＭＣＰ－ＨＴ４５０を用いて測定した。また、下記基準で評価した。
◎：１０１０以下
〇：１０１１～１０１２
×：Ｏｖｅｒ (Surface resistance value of adhesive layer)
The surface resistance value (Ω/□) of the adhesive layer was measured using MCP-HT450 manufactured by Mitsubishi Chemical Analytic Tech. Moreover, it evaluated by the following reference|standard.
◎: 10 10 or less ○: 10 11 to 10 12
×: Over
（耐久性）
作製したセパレータを有する粘着剤層付き偏光フィルム（１５インチ）のセパレータを剥がし、厚さ０．７ｍｍの無アルカリガラス（コーニング社製、ＥＧ－ＸＧ）にラミネーターを用いて貼着した。次いで、５０℃、０．５ＭＰaで、１５分間のオートクレーブ処理を行って、前記偏光フィルムを完全に無アクリルガラスに密着させた。次いで、これを、８０℃の加熱オーブン（通常耐久性）および９５℃の加熱オーブン（高温耐久性）にそれぞれ投入して、５００時間後の前記偏光フィルムの剥がれの有無を、下記基準で評価した。
〇：全く剥がれが認められなかった。
△：目視では確認できない程度の剥がれが認められた。
×：目視で確認できる小さな剥がれが認められた。 (durability)
The separator of the polarizing film (15 inches) with an adhesive layer having the separator was peeled off and adhered to non-alkaline glass (manufactured by Corning, EG-XG) having a thickness of 0.7 mm using a laminator. Then, autoclave treatment was performed at 50° C. and 0.5 MPa for 15 minutes to completely adhere the polarizing film to the non-acrylic glass. Next, this was placed in a heating oven at 80°C (normal durability) and a heating oven at 95°C (high temperature durability), respectively, and the presence or absence of peeling of the polarizing film after 500 hours was evaluated according to the following criteria. .
◯: No peeling was observed.
Δ: Peeling was observed to an extent that could not be visually confirmed.
x: Small peeling that can be visually confirmed was observed.
作製したセパレータを有する粘着剤層付き偏光フィルム（１５インチ）のセパレータを剥がし、厚さ０．７ｍｍの無アルカリガラス（コーニング社製、ＥＧ－ＸＧ）にラミネーターを用いて貼着した。次いで、５０℃、０．５ＭＰaで、１５分間のオートクレーブ処理を行って、前記偏光フィルムを完全に無アクリルガラスに密着させた。次いで、これを、８０℃の加熱オーブン（通常耐久性）および９５℃の加熱オーブン（高温耐久性）にそれぞれ投入して、５００時間後の前記偏光フィルムの剥がれの有無を、下記基準で評価した。
〇：全く剥がれが認められなかった。
△：目視では確認できない程度の剥がれが認められた。
×：目視で確認できる小さな剥がれが認められた。 (durability)
The separator of the polarizing film (15 inches) with an adhesive layer having the separator was peeled off and adhered to non-alkaline glass (manufactured by Corning, EG-XG) having a thickness of 0.7 mm using a laminator. Then, autoclave treatment was performed at 50° C. and 0.5 MPa for 15 minutes to completely adhere the polarizing film to the non-acrylic glass. Next, this was placed in a heating oven at 80°C (normal durability) and a heating oven at 95°C (high temperature durability), respectively, and the presence or absence of peeling of the polarizing film after 500 hours was evaluated according to the following criteria. .
◯: No peeling was observed.
Δ: Peeling was observed to an extent that could not be visually confirmed.
x: Small peeling that can be visually confirmed was observed.
表１から、実施例１～４のセパレータを有する粘着剤層付き偏光フィルムは、離型層の弾性率が低く、粘着剤層からセパレータを剥離する際の剥離力が低く、セパレータの軽剥離性と粘着剤層の高温耐久性がともに優れていることがわかる。一方、比較例１～４のセパレータを有する粘着剤層付き偏光フィルムは、離型層の弾性率が高く、粘着剤層からセパレータを剥離する際の剥離力が高く、セパレータの剥離性が劣っていることがわかる。また、比較例５のセパレータを有する粘着剤層付き偏光フィルムは、粘着剤層のベースポリマーに含まれるカルボキシ基含有モノマーの含有量が少ないため、粘着剤層の高温耐久性が劣っていることがわかる。
From Table 1, the polarizing films with adhesive layers having the separators of Examples 1 to 4 have a low elastic modulus of the release layer, a low peeling force when peeling the separator from the adhesive layer, and easy release of the separator. and the high-temperature durability of the pressure-sensitive adhesive layer are both excellent. On the other hand, the adhesive layer-attached polarizing films having the separators of Comparative Examples 1 to 4 had a high elastic modulus of the release layer, a high peeling force when peeling the separator from the adhesive layer, and poor separator releasability. I know there is. In addition, the pressure-sensitive adhesive layer-attached polarizing film having the separator of Comparative Example 5 has a low content of the carboxy group-containing monomer contained in the base polymer of the pressure-sensitive adhesive layer, so that the high-temperature durability of the pressure-sensitive adhesive layer is inferior. Recognize.
本発明のセパレータを有する粘着剤層付き偏光フィルムは、高温環境下で用いられる画像表示装置、例えば、車載用画像表示装置に好適に用いられる。
The pressure-sensitive adhesive layer-attached polarizing film having the separator of the present invention is suitably used for an image display device used in a high-temperature environment, for example, an in-vehicle image display device.
The pressure-sensitive adhesive layer-attached polarizing film having the separator of the present invention is suitably used for an image display device used in a high-temperature environment, for example, an in-vehicle image display device.
Claims (5)
- セパレータ上に粘着剤層を有するセパレータ付き粘着剤層が偏光フィルムの片面又は両面に設けられている、セパレータを有する粘着剤層付き偏光フィルムであって、
前記セパレータは、基材フィルム上に離型層を有し、
前記離型層は、反応性官能基を有する反応性シリコーン樹脂、及び重量平均分子量が４０万以上の非反応性シリコーン樹脂を含有し、
前記反応性シリコーン樹脂と前記非反応性シリコーン樹脂の合計含有量１００質量％中、前記反応性シリコーン樹脂の含有量が５０～７０質量％、前記非反応性シリコーン樹脂の含有量が３０～５０質量％であり、
前記離型層の弾性率が１．５ＭＰａ未満であり、
前記粘着剤層は、前記離型層上に設けられており、
前記粘着剤層は、モノマー単位としてカルボキシ基含有モノマーを０．５質量％以上含有するベースポリマーを含有することを特徴とするセパレータを有する粘着剤層付き偏光フィルム。 A polarizing film with an adhesive layer having a separator, wherein the adhesive layer with a separator having an adhesive layer on the separator is provided on one or both sides of the polarizing film,
The separator has a release layer on the base film,
The release layer contains a reactive silicone resin having a reactive functional group and a non-reactive silicone resin having a weight average molecular weight of 400,000 or more,
The content of the reactive silicone resin is 50 to 70% by mass, and the content of the non-reactive silicone resin is 30 to 50% by mass, based on the total content of 100% by mass of the reactive silicone resin and the non-reactive silicone resin. % and
The release layer has an elastic modulus of less than 1.5 MPa,
The adhesive layer is provided on the release layer,
A polarizing film with a pressure-sensitive adhesive layer having a separator, wherein the pressure-sensitive adhesive layer contains a base polymer containing 0.5% by mass or more of a carboxy group-containing monomer as a monomer unit. - 前記粘着剤層は、導電剤を含有する請求項１に記載のセパレータを有する粘着剤層付き偏光フィルム。 A polarizing film with an adhesive layer having the separator according to claim 1, wherein the adhesive layer contains a conductive agent.
- 前記粘着剤層の表面抵抗値が１．０×１０１２Ω／□以下である請求項１又は２に記載のセパレータを有する粘着剤層付き偏光フィルム。 The pressure-sensitive adhesive layer-attached polarizing film according to claim 1 or 2, wherein the pressure-sensitive adhesive layer has a surface resistance value of 1.0 × 10 12 Ω/□ or less.
- 前記粘着剤層から前記セパレータを剥離する際の剥離力が０．１２Ｎ／５０ｍｍ以下である請求項１～３のいずれかに記載のセパレータを有する粘着剤層付き偏光フィルム。 The polarizing film with a pressure-sensitive adhesive layer having a separator according to any one of claims 1 to 3, wherein the peel force when peeling the separator from the pressure-sensitive adhesive layer is 0.12 N/50 mm or less.
- 前記偏光フィルムの厚みが１００μｍ以下である請求項１～４のいずれかに記載のセパレータを有する粘着剤層付き偏光フィルム。
The pressure-sensitive adhesive layer-attached polarizing film having the separator according to any one of claims 1 to 4, wherein the polarizing film has a thickness of 100 µm or less.
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| KR1020237037771A KR20240042581A (en) | 2021-08-20 | 2022-08-05 | Polarizing film with adhesive layer and separator |
| CN202280056575.8A CN117836679A (en) | 2021-08-20 | 2022-08-05 | Polarizing film with adhesive layer having separator |
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| JP2021-134855 | 2021-08-20 | ||
| JP2021134855A JP2023028888A (en) | 2021-08-20 | 2021-08-20 | Polarization film with adhesive layer having separator |
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| CN (1) | CN117836679A (en) |
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|---|---|---|---|---|
| JP2008254207A (en) * | 2007-03-30 | 2008-10-23 | Lintec Corp | Release film and manufacturing method of the same |
| JP2012137567A (en) * | 2010-12-27 | 2012-07-19 | Mitsubishi Plastics Inc | Release polyester film for polarizing plate |
| JP2014129508A (en) * | 2012-11-30 | 2014-07-10 | Hitachi Maxell Ltd | Tacky tape for molding a plastic lens and method for molding a plastic lens molding |
| JP2017170672A (en) * | 2016-03-22 | 2017-09-28 | 東レフィルム加工株式会社 | Release film, and resin composition and coating composition used in the same |
| WO2020179509A1 (en) * | 2019-03-05 | 2020-09-10 | 日東電工株式会社 | Polarizing film with conductive layer and production method for polarizing film with conductive layer |
| JP2021080422A (en) * | 2019-11-22 | 2021-05-27 | 三菱ケミカル株式会社 | Adhesive composition, adhesive, adhesive for polarizing plate, and image display device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP6390149B2 (en) | 2014-04-24 | 2018-09-19 | 三菱ケミカル株式会社 | Polyester film |
| JP6714387B2 (en) | 2016-02-25 | 2020-06-24 | リンテック株式会社 | Release sheet |
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2022
- 2022-08-05 KR KR1020237037771A patent/KR20240042581A/en unknown
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- 2022-08-05 WO PCT/JP2022/030131 patent/WO2023022029A1/en active Application Filing
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008254207A (en) * | 2007-03-30 | 2008-10-23 | Lintec Corp | Release film and manufacturing method of the same |
| JP2012137567A (en) * | 2010-12-27 | 2012-07-19 | Mitsubishi Plastics Inc | Release polyester film for polarizing plate |
| JP2014129508A (en) * | 2012-11-30 | 2014-07-10 | Hitachi Maxell Ltd | Tacky tape for molding a plastic lens and method for molding a plastic lens molding |
| JP2017170672A (en) * | 2016-03-22 | 2017-09-28 | 東レフィルム加工株式会社 | Release film, and resin composition and coating composition used in the same |
| WO2020179509A1 (en) * | 2019-03-05 | 2020-09-10 | 日東電工株式会社 | Polarizing film with conductive layer and production method for polarizing film with conductive layer |
| JP2021080422A (en) * | 2019-11-22 | 2021-05-27 | 三菱ケミカル株式会社 | Adhesive composition, adhesive, adhesive for polarizing plate, and image display device |
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| KR20240042581A (en) | 2024-04-02 |
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