WO2012160996A1 - 粘着フィルム - Google Patents
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- WO2012160996A1 WO2012160996A1 PCT/JP2012/062192 JP2012062192W WO2012160996A1 WO 2012160996 A1 WO2012160996 A1 WO 2012160996A1 JP 2012062192 W JP2012062192 W JP 2012062192W WO 2012160996 A1 WO2012160996 A1 WO 2012160996A1
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- sensitive adhesive
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
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- OAMHTTBNEJBIKA-UHFFFAOYSA-N 2,2,2-trichloro-1-phenylethanone Chemical class ClC(Cl)(Cl)C(=O)C1=CC=CC=C1 OAMHTTBNEJBIKA-UHFFFAOYSA-N 0.000 description 1
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- KQSMCAVKSJWMSI-UHFFFAOYSA-N 2,4-dimethyl-1-n,1-n,3-n,3-n-tetrakis(oxiran-2-ylmethyl)benzene-1,3-diamine Chemical compound CC1=C(N(CC2OC2)CC2OC2)C(C)=CC=C1N(CC1OC1)CC1CO1 KQSMCAVKSJWMSI-UHFFFAOYSA-N 0.000 description 1
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 1
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- FZUGPQWGEGAKET-UHFFFAOYSA-N parbenate Chemical compound CCOC(=O)C1=CC=C(N(C)C)C=C1 FZUGPQWGEGAKET-UHFFFAOYSA-N 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229940044654 phenolsulfonic acid Drugs 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical group 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 229920006264 polyurethane film Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- ADYYRXNLCZOUSU-UHFFFAOYSA-M potassium;propan-2-ol;hydroxide Chemical compound [OH-].[K+].CC(C)O ADYYRXNLCZOUSU-UHFFFAOYSA-M 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- AAYRWMCIKCRHIN-UHFFFAOYSA-N propane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CCCS(O)(=O)=O AAYRWMCIKCRHIN-UHFFFAOYSA-N 0.000 description 1
- KRIOVPPHQSLHCZ-UHFFFAOYSA-N propiophenone Chemical class CCC(=O)C1=CC=CC=C1 KRIOVPPHQSLHCZ-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003458 sulfonic acid derivatives Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical group 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/105—Compounds containing metals of Groups 1 to 3 or of Groups 11 to 13 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
-
- 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
- C09J2433/00—Presence of (meth)acrylic polymer
-
- 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
- C09J2471/00—Presence of polyether
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T428/2852—Adhesive compositions
- Y10T428/2878—Adhesive compositions including addition polymer from unsaturated monomer
- Y10T428/2891—Adhesive compositions including addition polymer from unsaturated monomer including addition polymer from alpha-beta unsaturated carboxylic acid [e.g., acrylic acid, methacrylic acid, etc.] Or derivative thereof
Definitions
- the present invention relates to an adhesive film having antistatic properties.
- the pressure-sensitive adhesive film of the present invention is used for plastic products and the like that easily generate static electricity.
- it is useful as a surface protective film used for the purpose of protecting the surface of optical members such as polarizing plates, wave plates, retardation plates, optical compensation films, reflection sheets, brightness enhancement films, and diffusion sheets used in liquid crystal displays. It is.
- the present invention relates to an adhesive film. More specifically, the present invention relates to an adhesive film excellent in adhesive properties (adhesiveness) to an adherend such as an optical member, for example, a diffusion sheet having irregularities on the surface (the surface is not smooth), and further suppressing the peeling voltage at the time of peeling. .
- the surface protective film is used for the purpose of sticking to an adherend (protected body) through an adhesive layer and preventing scratches and dirt generated during processing and transport of the adherend.
- adherend protected body
- surface protective films used for optical members such as diffusion sheets are used for the purpose of protecting shipments, processing adherends, and preventing scratches and dirt that occur during transportation after sticking. The protective film becomes unnecessary and is finally peeled off and removed.
- the base material, pressure-sensitive adhesive, and separator constituting the surface protective film are often made of plastic materials, they have high electrical insulation, and static electricity is generated during friction and peeling.
- the static electricity generated at the time of peeling causes dust and dirt to adhere to the surface protection film, contaminating the diffusion sheet and other optical members, or causing defects in the pasted state, such as contamination, or encapsulating inside the adherend.
- the liquid crystal and electronic circuits that are used may be damaged.
- the surface protective film peels off from the adherend when it is shipped or transported after the surface protective film is applied to the adherend having an uneven surface (the surface is not smooth) such as a diffusion sheet.
- the adhesive force is high, and high adhesive strength is required.
- An object of the present invention is to provide an antistatic adhesive film and a surface protective film exhibiting excellent adhesive properties.
- the pressure-sensitive adhesive layer is (meth) in a base material layer and a pressure-sensitive adhesive film having a pressure-sensitive adhesive layer on at least one side of the base material layer.
- a pressure-sensitive adhesive film having a pressure-sensitive adhesive layer on at least one side of the base material layer.
- the present inventors have found that an antistatic pressure-sensitive adhesive film can be obtained in which the antistatic to the adherend which is not prevented can be prevented and the contamination of the adherend is reduced, and the present invention has been completed.
- the pressure-sensitive adhesive film of the present invention is a pressure-sensitive adhesive film having a base material layer and a pressure-sensitive adhesive layer on at least one side of the base material layer, and the pressure-sensitive adhesive layer comprises a (meth) acrylic polymer, an alkali metal salt, and A crosslinking agent is contained, and the crosslinking agent is contained in an amount of 2 parts by weight or less with respect to 100 parts by weight of the (meth) acrylic polymer. 30 minutes after RH conditions) is 0.5 N / 25 mm or more at a tensile speed of 0.3 m / min.
- the (meth) acrylic polymer in the present invention refers to an acrylic polymer and / or a methacrylic polymer
- (meth) acrylate refers to an acrylate and / or methacrylate.
- the pressure-sensitive adhesive film of the present invention preferably has a peeling voltage (adhered body: acrylic panel, 23 ° C. ⁇ 50% RH condition) having an absolute value of 0.5 kV or less at a peeling speed of 10 m / min.
- the alkali metal salt is preferably a lithium salt.
- the pressure-sensitive adhesive layer preferably contains a polyether polyol compound.
- the adhesive film of the present invention is preferably a protective film for optical members.
- the adhesive film of the present invention is preferably a protective film for a diffusion sheet.
- the pressure-sensitive adhesive film of the present invention is excellent in pressure-sensitive adhesive properties, and can prevent charging to an adherend that is not antistatic when peeled.
- it has excellent adhesive properties (adhesiveness) to optical members (adherents) such as diffusion sheets with irregularities on the surface (surface is not smooth), further suppresses the stripping voltage during stripping, and is charged by static electricity.
- an antistatic adhesive film and a surface protective film can be obtained, which is very useful.
- the pressure-sensitive adhesive film of the present invention is a pressure-sensitive adhesive film having a base material layer and a pressure-sensitive adhesive layer on at least one side of the base material layer, wherein the pressure-sensitive adhesive layer comprises a (meth) acrylic polymer, an alkali metal salt, and a crosslinking agent. 2 parts by weight or less of the crosslinking agent with respect to 100 parts by weight of the (meth) acrylic polymer, and the adhesive strength of the adhesive film (adhered body: acrylic panel, 23 ° C. ⁇ 50% RH condition) (After 30 minutes elapses below) at a tensile speed of 0.3 m / min, it is 0.5 N / 25 mm or more.
- the pressure-sensitive adhesive layer in the present invention is characterized by containing a (meth) acrylic polymer.
- the (meth) acrylic polymer preferably contains a (meth) acrylic monomer having an alkyl group having 1 to 14 carbon atoms as a constituent component.
- Use of a (meth) acrylic polymer is preferable from the viewpoints of ease of handling, adhesive strength and removability.
- a (meth) acrylic monomer having an alkyl group having 1 to 14 carbon atoms in the present invention can be used, a (meth) acrylic monomer having an alkyl group having 4 to 14 carbon atoms is more preferable.
- examples thereof include methyl (meth) acrylate and ethyl (meth) acrylate.
- These acrylic monomers may be used alone or in combination of two or more.
- the amount of the (meth) acrylic monomer having an alkyl group having 1 to 14 carbon atoms is preferably 50% by weight or more, more preferably 60 to 100% by weight, and even more preferably 70 to 98% by weight in the monomer component. preferable. Within the above range, a favorable interaction with the alkali metal salt and a good adhesive property (adhesiveness) are appropriately adjusted, which is preferable.
- polymerizable monomers other than the (meth) acrylic monomer having an alkyl group having 1 to 14 carbon atoms include a polymerizable monomer for adjusting the glass transition point and peelability of the (meth) acrylic polymer, etc. Can be used as long as the effects of the present invention are not impaired. These monomers may be used alone or in combination, but the amount of other polymerizable monomers in the monomer component (whole) is preferably less than 50% by weight.
- Examples of the other polymerizable monomers include cohesive force / heat resistance improving components such as sulfonic acid group-containing monomers, phosphoric acid group-containing monomers, cyano group-containing monomers, vinyl ester monomers, aromatic vinyl monomers, and carboxyl group-containing monomers.
- cohesive force / heat resistance improving components such as sulfonic acid group-containing monomers, phosphoric acid group-containing monomers, cyano group-containing monomers, vinyl ester monomers, aromatic vinyl monomers, and carboxyl group-containing monomers.
- the acid value of the (meth) acrylic polymer is preferably adjusted to 40 or less, more preferably 29 or less, still more preferably 16 or less, particularly preferably 8 or less, and most preferably 1 or less.
- the acid value of the (meth) acrylic polymer exceeds 40, the charging characteristics are deteriorated.
- the acid value of the (meth) acrylic polymer in the present invention means the number of mg of potassium hydroxide necessary to neutralize free fatty acid, resin acid, etc. contained in 1 g of a sample.
- the (meth) acrylic polymer skeleton having a large acid value there are a large number of carboxyl groups and sulfonate groups having a large interaction with the alkali metal salt, and as a result, ion conduction by the alkali metal salt is hindered. Therefore, it is estimated that excellent antistatic ability cannot be obtained.
- Examples of the acid value of the (meth) acrylic polymer being 40 or less include, for example, an acrylic polymer obtained by copolymerizing 2-ethylhexyl acrylate and acrylic acid as a (meth) acrylic polymer having a carboxyl group.
- acrylic acid is 5.1 parts by weight or less with respect to 100 parts by weight of the total amount of 2-ethylhexyl acrylate and acrylic acid.
- the said acid value can be made into 29 or less by adjusting acrylic acid to 3.7 parts weight or less.
- sulfonic acid group-containing monomer examples include styrene sulfonic acid, allyl sulfonic acid, 2- (meth) acrylamide-2-methylpropane sulfonic acid, (meth) acrylamide propane sulfonic acid, sulfopropyl (meth) acrylate, (meth) And acryloyloxynaphthalene sulfonic acid.
- Examples of the phosphate group-containing monomer include 2-hydroxyethylacryloyl phosphate.
- Examples of the cyano group-containing monomer include acrylonitrile.
- Examples of the vinyl ester monomer include vinyl acetate, vinyl propionate, and vinyl laurate.
- aromatic vinyl monomer examples include styrene, chlorostyrene, chloromethylstyrene, ⁇ -methylstyrene, and the like.
- carboxyl group-containing monomer examples include (meth) acrylic acid, carboxyethyl (meth) acrylate, carboxypentyl (meth) acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid.
- Examples of the acid anhydride group-containing monomer include maleic anhydride and itaconic anhydride.
- hydroxyl group-containing monomer examples include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 6-hydroxyhexyl (meth) acrylate, and 8-hydroxyoctyl.
- hydroxyl group-containing monomer By using a hydroxyl group-containing monomer, it becomes easier to control the crosslinking of the pressure-sensitive adhesive composition, which is the raw material of the pressure-sensitive adhesive layer, and as a result, balance between improvement of wettability due to flow and reduction of adhesion (adhesion) force in peeling. It becomes easy to control. Furthermore, unlike carboxyl groups and sulfonate groups that can generally act as cross-linking sites, hydroxyl groups have a moderate interaction with alkali metal salts and polyether polyol compounds, so that they are also preferably used in terms of antistatic properties. Can do.
- amide group-containing monomer examples include acrylamide and diethyl acrylamide.
- amino group-containing monomer examples include N, N-dimethylaminoethyl (meth) acrylate, N, N-dimethylaminopropyl (meth) acrylate, and the like.
- epoxy group-containing monomer examples include glycidyl (meth) acrylate and allyl glycidyl ether.
- vinyl ether monomer examples include methyl vinyl ether, ethyl vinyl ether, isobutyl vinyl ether, and the like.
- the (meth) acrylic polymer used in the present invention preferably has a weight average molecular weight of 100,000 to 5,000,000, more preferably 200,000 to 4,000,000, and even more preferably 300,000 to 3,000,000. If the weight average molecular weight is less than 100,000, the wettability to the adherend will improve the adhesive strength (adhesive force) at the time of peeling, which may cause damage to the adherend in the peeling process (re-peeling). In addition, there is a tendency for adhesive residue to occur due to a decrease in the cohesive force of the pressure-sensitive adhesive layer.
- a weight average molecular weight means what was obtained by measuring by GPC (gel permeation chromatography).
- the glass transition temperature (Tg) of the (meth) acrylic polymer is preferably 0 ° C. or lower (usually ⁇ 100 ° C. or higher), more preferably ⁇ 10 ° C. or lower. More preferably, it is ⁇ 20 ° C. or lower.
- the glass transition temperature (Tg) of a (meth) acrylic-type polymer can be adjusted in the said range by changing the monomer component and composition ratio to be used suitably.
- the polymerization method of the (meth) acrylic polymer used in the present invention is not particularly limited, and can be polymerized by a known method such as solution polymerization, emulsion polymerization, bulk polymerization, suspension polymerization, etc. Therefore, solution polymerization is more preferable. Moreover, any of a random copolymer, a block copolymer, etc. may be sufficient as the obtained copolymer.
- the pressure-sensitive adhesive layer in the present invention contains an alkali metal salt.
- an alkali metal salt to obtain a compatible and well-balanced interaction with (meth) acrylic polymers, etc., an adhesive film that can be prevented from being charged to an adherend that is not antistatic when peeled off. (Surface protective film) can be obtained.
- Examples of the alkali metal salt used in the present invention include a metal salt composed of lithium, sodium and potassium. Specifically, a cation composed of Li + , Na + and K + , 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 ⁇ , C n F 2n + 1 SO 3 ⁇ (n is an integer), (CF 3 SO 2 ) 2 N ⁇ , (CF 3 SO 2 ) 3 C ⁇ , AsF 6 ⁇ , SbF 6 ⁇ , NbF 6 ⁇ , TaF 6 ⁇ , F (HF) n ⁇ , (CN) 2 N ⁇ , (C 2 F 5 SO 2 ) 2 N ⁇ , C 3 F 7 COO ⁇ , (CF 3 SO 2
- anion component the anion etc. which are represented with a following formula (A) can also be used.
- the blending amount of the alkali metal salt is preferably 0.01 to 3 parts by weight, more preferably 0.01 to 2 parts by weight with respect to 100 parts by weight of the (meth) acrylic polymer. It is particularly preferable to add 02 to 1 part by weight. If the amount is less than 0.01 parts by weight, sufficient charging characteristics may not be obtained. On the other hand, if the amount is more than 3 parts by weight, contamination of the adherend tends to increase, such being undesirable.
- the pressure-sensitive adhesive layer in the present invention preferably contains a polyether polyol compound.
- a polyether polyol compound By using a polyether polyol compound to obtain a compatible and well-balanced interaction with alkali metal salts and (meth) acrylic polymers, etc. Can be obtained, and an adhesive film (surface protective film) with reduced contamination of the adherend can be obtained.
- the polyether polyol compound is not particularly limited as long as it is a polymer polyol having an ether group.
- the molecular weight of the polyether polyol compound is preferably a number average molecular weight of 10,000 or less, more preferably 200 to 5,000. When the number average molecular weight exceeds 10,000, the contamination tends to deteriorate.
- the number average molecular weight is obtained by measuring by GPC (gel permeation chromatography).
- the blending amount of the polyether polyol compound is preferably 0.1 to 3 parts by weight, more preferably 0.2 to 2.5 parts by weight with respect to 100 parts by weight of the (meth) acrylic polymer. More preferably, it is 0.3 to 2 parts by weight. If it is less than 0.1 part by weight, it is difficult to obtain sufficient antistatic properties, and if it exceeds 3 parts by weight, the contamination of the adherend tends to increase or the adhesive properties tend to deteriorate, such being undesirable.
- the pressure-sensitive adhesive layer in the present invention is characterized by containing a crosslinking agent.
- An adhesive film (surface protective film) with more excellent heat resistance can be obtained by appropriately adjusting the structural unit, structural ratio, selection of the crosslinking agent, addition ratio, and the like of the (meth) acrylic polymer. .
- an isocyanate compound As the crosslinking agent used in the present invention, an isocyanate compound, an epoxy compound, a melamine resin, an aziridine derivative, a metal chelate compound, or the like is used.
- isocyanate compounds and epoxy compounds are particularly preferably used mainly from the viewpoint of obtaining an appropriate cohesive force. These compounds may be used alone or in combination of two or more.
- isocyanate compound examples include lower aliphatic polyisocyanates such as butylene diisocyanate and hexamethylene diisocyanate, alicyclic isocyanates such as cyclopentylene diisocyanate, cyclohexylene diisocyanate and isophorone diisocyanate, and 2,4-tolylene diisocyanate.
- lower aliphatic polyisocyanates such as butylene diisocyanate and hexamethylene diisocyanate
- alicyclic isocyanates such as cyclopentylene diisocyanate, cyclohexylene diisocyanate and isophorone diisocyanate
- 2,4-tolylene diisocyanate examples include 2,4-tolylene diisocyanate.
- aromatic isocyanates such as xylylene diisocyanate, trimethylolpropane / tolylene diisocyanate trimer adduct (trade name Coronate L, manufactured by Nippon Polyurethane Industry Co., Ltd.), trimethylolpropane / hexa Methylene diisocyanate trimer adduct (trade name Coronate HL, manufactured by Nippon Polyurethane Industry Co., Ltd.), Isocyanate of hexamethylene diisocyanate Rate body (trade name: Coronate HX, manufactured by Nippon Polyurethane Industry Co., Ltd.) and isocyanate adducts and the like. These compounds may be used alone or in combination of two or more.
- isocyanurate-modified isocyanate (trade name Coronate HX, manufactured by Nippon Polyurethane Industry Co., Ltd.) Isocyanate-modified isocyanate of tolylene diisocyanate
- An isocyanurate modified product (trade name Coronate 2030, manufactured by Nippon Polyurethane Industry Co., Ltd.) is a suitable example.
- Examples of the epoxy compound include N, N, N ′, N′-tetraglycidyl-m-xylenediamine (trade name: TETRAD-X, manufactured by Mitsubishi Gas Chemical Company) and 1,3-bis (N, N-dioxy). Glycidylaminomethyl) cyclohexane (trade name: TETRAD-C, manufactured by Mitsubishi Gas Chemical Company, Inc.). These compounds may be used alone or in combination of two or more.
- Examples of the melamine resin include hexamethylol melamine.
- Examples of the aziridine derivative include a commercially available product name HDU (manufactured by Mutual Pharmaceutical Company), a product name TAZM (manufactured by Mutual Pharmaceutical Company), and a product name TAZO (manufactured by Mutual Pharmaceutical Company). These compounds may be used alone or in combination of two or more.
- metal chelate compound examples include aluminum, iron, tin, titanium and nickel as metal components, and acetylene, methyl acetoacetate, ethyl lactate and acetylacetone as chelate components. These compounds may be used alone or in combination of two or more.
- a polyfunctional monomer having two or more radiation-reactive unsaturated bonds can be added as a crosslinking agent.
- the raw material (pressure-sensitive adhesive composition) for forming the pressure-sensitive adhesive layer is crosslinked by irradiating with radiation or the like.
- a polyfunctional monomer having two or more radiation-reactive unsaturated bonds in one molecule for example, it can be crosslinked (cured) by irradiation with radiation such as vinyl group, acryloyl group, methacryloyl group, vinylbenzyl group. Examples thereof include polyfunctional monomers having two or more radiation reactivity of one kind or two or more kinds.
- the polyfunctional monomer generally, those having 10 or less radiation-reactive unsaturated bonds are preferably used. These compounds may be used alone or in combination of two or more.
- polyfunctional monomer examples include, for example, ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, tetraethylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, and 1,6 hexane.
- examples include diol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tri (meth) acrylate, dipentaerythritol hexa (meth) acrylate, divinylbenzene, and N, N′-methylenebisacrylamide.
- the content of the crosslinking agent used in the present invention is 2 parts by weight or less, preferably 0.05 to 1.5 parts by weight, and 0.1 to 1 part by weight with respect to 100 parts by weight of the (meth) acrylic polymer. Is more preferable.
- the content is less than 0.05 parts by weight, the crosslinking formation by the crosslinking agent becomes insufficient, the cohesive force of the pressure-sensitive adhesive layer (pressure-sensitive adhesive composition) becomes small, and sufficient heat resistance may not be obtained. Yes, and tends to cause glue residue.
- Examples of the radiation include ultraviolet rays, laser rays, ⁇ rays, ⁇ rays, ⁇ rays, X rays, electron rays, and the like, and ultraviolet rays are preferably used from the viewpoints of controllability, ease of handling, and cost. . More preferably, ultraviolet rays having a wavelength of 200 to 400 nm are used. Ultraviolet rays can be irradiated using an appropriate light source such as a high-pressure mercury lamp, a microwave excitation lamp, or a chemical lamp. In addition, when using an ultraviolet-ray as a radiation, a photoinitiator is added to an acrylic adhesive.
- the photopolymerization initiator may be any substance that generates radicals or cations by irradiating ultraviolet rays having an appropriate wavelength that can trigger the polymerization reaction according to the type of the radiation-reactive component.
- radical photopolymerization initiators for example, benzoins such as benzoin, benzoin methyl ether, benzoin ethyl ether, o-benzoylbenzoic acid methyl-p-benzoin ethyl ether, benzoin isopropyl ether, ⁇ -methylbenzoin, benzyldimethyl ketal, trichloro Acetophenones such as acetophenone, 2,2-diethoxyacetophenone, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methylpropiophenone, 2-hydroxy-4'-isopropyl-2-methylpropiophenone, etc.
- benzoins such as benzoin, benzoin methyl ether, benzoin ethyl ether, o-benzoylbenzoic acid methyl-p-benzoin ethyl ether, benzoin isopropyl ether, ⁇ -methylbenzoin, benzyl
- Propiophenones benzophenone, methylbenzophenone, p-chlorobenzophenone, benzophenones such as p-dimethylaminobenzophenone, 2-chlorothioxanthone, 2-ethyl Thioxanthones such as oxanthone and 2-isopropylthioxanthone, bis (2,4,6-trimethylbenzoyl) -phenylphosphine oxide, 2,4,6-trimethylbenzoyldiphenylphosphine oxide, (2,4,6-trimethylbenzoyl)- And acylphosphine oxides such as (ethoxy) -phenylphosphine oxide, benzyl, dibenzosuberone, ⁇ -acyl oxime ester and the like. These compounds may be used alone or in combination of two or more.
- Examples of the cationic photopolymerization initiator include onium salts such as aromatic diazonium salts, aromatic iodonium salts, and aromatic sulfonium salts, organometallic complexes such as iron-allene complexes, titanocene complexes, and arylsilanol-aluminum complexes, nitro Examples thereof include benzyl ester, sulfonic acid derivative, phosphoric acid ester, phenol sulfonic acid ester, diazonaphthoquinone, and N-hydroxyimide sulfonate. These compounds may be used alone or in combination of two or more.
- the photopolymerization initiator is usually added in an amount of 0.1 to 10 parts by weight and preferably 0.2 to 7 parts by weight with respect to 100 parts by weight of the acrylic polymer.
- a photoinitiated polymerization aid such as amines in combination.
- the photoinitiator aid include 2-dimethylaminoethyl benzoate, dimethylaminoacetophenone, p-dimethylaminobenzoic acid ethyl ester, p-dimethylaminobenzoic acid isoamyl ester, and the like. These compounds may be used alone or in combination of two or more.
- the polymerization initiation assistant is preferably added in an amount of 0.05 to 10 parts by weight, more preferably 0.1 to 7 parts by weight, based on 100 parts by weight of the (meth) acrylic polymer.
- the pressure-sensitive adhesive layer (pressure-sensitive adhesive composition) of the present invention may contain other additives such as a crosslinking catalyst, a crosslinking retarder, a filler, a colorant, a pigment, a surfactant, and a plasticizer. , Tackifiers, low molecular weight polymers and the like can be used as appropriate.
- the pressure-sensitive adhesive film of the present invention is obtained by forming the pressure-sensitive adhesive layer on a base material layer (support). At that time, crosslinking of the pressure-sensitive adhesive composition, which is a raw material of the pressure-sensitive adhesive layer, is generally performed after application of the pressure-sensitive adhesive composition, but the pressure-sensitive adhesive layer after crosslinking is used as a base material layer (support). It is also possible to transfer.
- the pressure-sensitive adhesive composition (solution) is applied directly on the adherend, or a base layer (support, support base) ),
- the pressure-sensitive adhesive layer can be obtained by light irradiation.
- a pressure-sensitive adhesive film is obtained by photopolymerization by irradiating an ultraviolet ray having an illuminance of 1 to 200 mW / cm 2 at a wavelength of 300 to 400 nm with a light amount of about 400 to 4000 mJ / cm 2 .
- the method for forming the pressure-sensitive adhesive layer on the base material layer (support) is not particularly limited.
- the pressure-sensitive adhesive composition (solution) is applied to the base material layer, and the polymerization solvent or the like is removed by drying. It is produced by forming a layer on a substrate layer. Thereafter, curing may be performed for the purpose of adjusting the component transfer of the pressure-sensitive adhesive layer or adjusting the crosslinking reaction.
- a pressure-sensitive adhesive composition is applied on a base material layer to produce a pressure-sensitive adhesive film, one or more solvents other than the polymerization solvent are newly added to the composition so that the adhesive film can be uniformly applied on the base material layer. You may add to.
- a known method used for manufacturing a pressure-sensitive adhesive tape or the like is used as a method for forming the pressure-sensitive adhesive layer in the present invention. Specific examples include roll coating, gravure coating, reverse coating, roll brushing, spray coating, air knife coating, and the like.
- the pressure-sensitive adhesive composition used in the pressure-sensitive adhesive film of the present invention includes various conventionally known tackifiers, surface lubricants, leveling agents, antioxidants, corrosion inhibitors, light stabilizers, ultraviolet absorbers, polymerizations. Add appropriately according to the use of various conventionally known additives such as inhibitors, silane coupling agents, inorganic or organic fillers, powders such as metal powders and pigments, particles and foils. I can do it.
- the thickness of the pressure-sensitive adhesive is usually 3 to 100 ⁇ m, preferably about 5 to 50 ⁇ m.
- Various base material layers (supports) made of a plastic film such as a polyester film or a porous material such as paper or nonwoven fabric. ) Is applied and formed on one or both sides of the sheet to form a sheet or tape.
- the base material layer constituting the adhesive film is preferably a resin film having heat resistance and solvent resistance and flexibility.
- the pressure-sensitive adhesive composition solution
- Examples of the resin forming the base layer include polyethylene terephthalate, polyester, polyethylene, polypropylene, polystyrene, polyimide, polyvinyl alcohol, polyvinyl chloride, polyfluoroethylene, and other fluorine-containing resins, nylon, and cellulose. it can.
- the surface of the base material layer may be subjected to corona treatment or the like. Moreover, you may perform a back surface process to a base material layer.
- a plastic substrate is preferably used as the substrate layer (support).
- the plastic substrate is not particularly limited as long as it can be formed into a sheet shape or a film shape.
- polyethylene, polypropylene, poly-1-butene, poly-4-methyl-1-pentene, ethylene Polyolefin films such as propylene copolymer, ethylene / 1-butene copolymer, ethylene / vinyl acetate copolymer, ethylene / ethyl acrylate copolymer, ethylene / vinyl alcohol copolymer, polyethylene terephthalate, polyethylene naphthalate, poly Polyester film such as butylene terephthalate, polyacrylate film, polystyrene film, nylon 6, nylon 6,6, polyamide film such as partially aromatic polyamide, polyvinyl chloride film, polyvinylidene chloride film, polycarbonate Such as ball titanate film, and the like.
- the thickness of the base material layer is usually about 5 to 200 ⁇ m, preferably about 10 to 100 ⁇ m.
- the adhesive layer bonding surface of the base material layer may be appropriately treated with a release agent such as a silicone-based, fluorine-based, long-chain alkyl-based or fatty acid amide-based release agent, silica powder, or the like.
- a silicone, fluorine, long chain alkyl or fatty acid amide release agent, silica powder or the like if necessary, release by a silicone, fluorine, long chain alkyl or fatty acid amide release agent, silica powder or the like, antifouling treatment, acid treatment, alkali Easy adhesion treatment such as treatment, primer treatment, corona treatment, plasma treatment, and ultraviolet treatment can also be performed.
- the base material layer is more preferably one subjected to antistatic treatment.
- the antistatic treatment applied to the plastic substrate is not particularly limited, but there are a method of providing an antistatic layer on at least one side of a commonly used substrate and a method of kneading a type antistatic agent into a plastic substrate. Used.
- a method of providing an antistatic layer on at least one surface of the base material layer a method of applying an antistatic resin or a conductive polymer comprising an antistatic agent and a resin component described later, a conductive resin containing a conductive substance, Examples thereof include a method of depositing or plating a conductive substance.
- the pressure-sensitive adhesive film of the present invention can be bonded to the surface of the pressure-sensitive adhesive layer for the purpose of protecting the pressure-sensitive adhesive surface as necessary.
- a base material constituting the separator there are paper and plastic film, but a plastic film is preferably used from the viewpoint of excellent surface smoothness.
- the film is not particularly limited as long as it can protect the pressure-sensitive adhesive layer.
- examples thereof include a coalesced film, a polyethylene terephthalate film, a polybutylene terephthalate film, a polyurethane film, and an ethylene-vinyl acetate copolymer film.
- the separator (plastic base material) used in the present invention may be subjected to antistatic treatment. Although it does not specifically limit as an antistatic process given to a plastic base material, The method similar to the said base material layer is employable.
- Antistatic agents contained in the antistatic resin used in the base material layer and separator include cationic functional groups such as quaternary ammonium salts, pyridinium salts, primary, secondary, and tertiary amino groups.
- Cationic antistatic agents, anionic antistatic agents having anionic functional groups such as sulfonates, sulfates, phosphonates, phosphates, alkylbetaines and their derivatives, imidazolines and their derivatives, alanine and Amphoteric antistatic agents such as derivatives thereof, aminoalcohol and derivatives thereof, glycerin and derivatives thereof, nonionic antistatic agents such as polyethylene glycol and derivatives thereof, and the above cation type, anion type and zwitterionic type ionic conductivity Ion-conductivity obtained by polymerizing or copolymerizing monomers having a functional group Sex polymer and the like. These compounds may be used alone or in combination of two or more.
- a cationic type antistatic agent for example, it has a quaternary ammonium group such as alkyltrimethylammonium salt, acyloylamidopropyltrimethylammonium methosulfate, alkylbenzylmethylammonium salt, acylcholine chloride, polydimethylaminoethyl methacrylate (meth) Examples thereof include acrylate copolymers, styrene copolymers having quaternary ammonium groups such as polyvinylbenzyltrimethylammonium chloride, and diallylamine copolymers having quaternary ammonium groups such as polydiallyldimethylammonium chloride. These compounds may be used alone or in combination of two or more.
- anionic antistatic agent examples include alkyl sulfonate, alkyl benzene sulfonate, alkyl sulfate ester salt, alkyl ethoxy sulfate ester salt, alkyl phosphate ester salt, and sulfonic acid group-containing styrene copolymer. These compounds may be used alone or in combination of two or more.
- zwitterionic antistatic agents examples include alkylbetaines, alkylimidazolium betaines, and carbobetaine graft copolymers. These compounds may be used alone or in combination of two or more.
- Nonionic antistatic agents include, for example, fatty acid alkylolamide, di (2-hydroxyethyl) alkylamine, polyoxyethylene alkylamine, fatty acid glycerin ester, polyoxyethylene glycol fatty acid ester, sorbitan fatty acid ester, polyoxysorbitan fatty acid Examples thereof include esters, polyoxyethylene alkyl phenyl ethers, polyoxyethylene alkyl ethers, polyethylene glycols, polyoxyethylene diamines, copolymers composed of polyethers, polyesters and polyamides, and methoxypolyethylene glycol (meth) acrylates. These compounds may be used alone or in combination of two or more.
- Examples of the conductive polymer include polyaniline, polypyrrole, polythiophene and the like. These conductive polymers may be used alone or in combination of two or more.
- Examples of the conductive material include tin oxide, antimony oxide, indium oxide, cadmium oxide, titanium oxide, zinc oxide, indium, tin, antimony, gold, silver, copper, aluminum, nickel, chromium, titanium, iron, cobalt, Examples include copper iodide, and alloys or mixtures thereof.
- the resin component used for the antistatic resin and the conductive resin for example, general-purpose resins such as polyester, acrylic, polyvinyl, urethane, melamine, and epoxy are used.
- a polymer type antistatic agent it is not necessary to contain a resin component.
- the antistatic resin component may contain, for example, a methylol- or alkylol-containing melamine-based, urea-based, glyoxal-based, or acrylamide-based compound, an epoxy compound, or an isocyanate compound as a crosslinking agent.
- the above-mentioned antistatic resin, conductive polymer, or conductive resin is diluted with a solvent such as an organic solvent or water, and this coating solution is applied to a plastic substrate and dried. Formed with.
- organic solvent used for forming the antistatic layer examples include methyl ethyl ketone, acetone, ethyl acetate, tetrahydrofuran, dioxane, cyclohexanone, n-hexane, toluene, xylene, methanol, ethanol, n-propanol, and isopropanol. can give. These solvents may be used alone or in combination of two or more.
- a coating method in forming the antistatic layer a known coating method is appropriately used. Specific examples include roll coating, gravure coating, reverse coating, roll brushing, spray coating, air knife coating, impregnation and curtain coating methods.
- the thickness of the antistatic resin layer, the conductive polymer, and the conductive resin is usually about 0.01 to 5 ⁇ m, preferably about 0.03 to 1 ⁇ m.
- Examples of the method for depositing or plating the conductive material include vacuum deposition, sputtering, ion plating, chemical vapor deposition, spray pyrolysis, chemical plating, and electroplating.
- the thickness of the conductive material layer is usually preferably 20 to 10,000 mm (0.002 to 1 ⁇ m), more preferably 50 to 5000 mm (0.005 to 0.5 ⁇ m).
- the above antistatic agent is appropriately used.
- the mixing amount of the kneading type antistatic agent is 20% by weight or less, preferably 0.05 to 10% by weight, based on the total weight of the plastic substrate.
- the kneading method is not particularly limited as long as the antistatic agent can be uniformly mixed with the resin used for the plastic substrate. For example, a heating roll, a Banbury mixer, a pressure kneader, a biaxial kneader, etc. Used.
- the adhesive film of the present invention is used for plastic products that are particularly prone to generate static electricity, and in particular, a polarizing plate, a wave plate, a display device such as a liquid crystal display and an organic EL display, and a touch panel using the same, It can be used as a surface protective film used for the purpose of protecting the surface of an optical member such as a retardation plate, an optical compensation film, a reflection sheet, a brightness enhancement film, and a diffusion sheet.
- an optical member such as a retardation plate, an optical compensation film, a reflection sheet, a brightness enhancement film, and a diffusion sheet.
- HLC-8220GPC column Sample column: manufactured by Tosoh Corporation, TSK guard column Super HZ-H (1) + TSK gel Super HZM-H (2) Reference column: TSKgel Super H-RC (1 piece), manufactured by Tosoh Corporation Flow rate: 0.6 ml / min Sample injection volume: 10 ⁇ l Column temperature: 40 ° C Eluent: THF Injection sample concentration: 0.2% by weight Detector: differential refractometer The weight average molecular weight was calculated in terms of polystyrene.
- the glass transition temperature Tg (° C.) was determined by the following formula using the following literature values as the glass transition temperature Tg n (° C.) of the homopolymer of each monomer.
- Tg + 273 ⁇ [W n / (Tg n +273)] (Wherein, Tg (° C.) is the glass transition temperature of the copolymer, W n ( ⁇ ) is the weight fraction of each monomer, T g n (° C.) is the glass transition temperature of the homopolymer of each monomer, and n is each monomer.
- the acid value was measured using an automatic titration apparatus (COM-550, manufactured by Hiranuma Sangyo Co., Ltd.), and obtained from the following formula.
- Titration solution 2-propanol potassium hydroxide solution (0.1N, manufactured by Wako Pure Chemical Industries, Ltd., for petroleum product neutralization value test)
- Electrode Glass electrode; GE-101, Comparative electrode; RE-201 Measurement mode: Petroleum product neutralization number test 1
- An evaluation sample was prepared by laminating an adhesive film cut to a size of 25 mm width and 100 mm length on an acrylic panel (manufactured by Mitsubishi Rayon Co., Ltd.) under pressure bonding conditions of 0.25 MPa and a speed of 0.3 m / min. After leaving the laminate for 30 minutes, the adhesive strength when peeled at a peeling speed of 0.3 m / min and a peeling angle of 180 ° was measured with a universal tensile tester. The measurement was performed in an environment of 23 ° C. ⁇ 50% RH.
- the adhesive strength of the pressure-sensitive adhesive film of the present invention is 0.5 N / 25 mm or more, preferably 0.6 to 6 N / 25 mm, and more preferably 0.6 to 4 N / 25 mm. Within the above range, sufficient adhesive properties can be exhibited even for adherends having surface irregularities (not smooth) such as diffusion sheets.
- One end protruding 30 mm was fixed to an automatic winder and peeled so that the peeling angle was 150 ° and the peeling speed was 10 m / min.
- the peeled adhesive film was placed on a sample fixing base, and the potential of the adhesive surface was measured with a potential measuring device (KSD-0103, manufactured by Kasuga Denki Co., Ltd.) fixed at a predetermined position. The measurement was performed in an environment of 23 ° C. ⁇ 50% RH.
- the absolute value of the peel voltage of the pressure-sensitive adhesive film of the present invention is preferably 0.5 kV or less, more preferably 0.4 kV or less, and particularly preferably 0.3 kV or less. Within the above range, excellent charging characteristics can be exhibited.
- Antistatic agent solution (a) A four-necked flask equipped with a stirring blade, thermometer, condenser, and dropping funnel is charged with 20 parts by weight of lithium iodide and 80 parts by weight of ethyl acetate, and the mixture is stirred for 2 hours while maintaining the liquid temperature in the vicinity of 80 ° C. To prepare an antistatic agent solution (a) (20% by weight).
- Antistatic agent solution (b) A four-necked flask equipped with a stirring blade, thermometer, condenser, and dropping funnel is charged with 20 parts by weight of lithium perchlorate and 80 parts by weight of ethyl acetate, and the temperature in the flask is kept at around 80 ° C. for 2 hours. Stirring was performed to prepare an antistatic agent solution (b) (20% by weight).
- Antistatic agent solution (c) In a four-necked flask equipped with a stirring blade, a thermometer, a cooler, and a dropping funnel, 1 part by weight of LiN (C 2 F 5 SO 2 ) 2 , polypropylene glycol-polyethylene glycol-polypropylene glycol block copolymer (number average molecular weight 2000) , Ethylene glycol group ratio 50 wt%: PEP) 14 parts by weight, ethyl acetate 60 parts by weight, the liquid temperature in the flask was kept at around 80 ° C. and stirred for 2 hours, antistatic agent solution (c) ( 20% by weight) was prepared.
- Antistatic agent solution (d) In a four-necked flask equipped with a stirring blade, thermometer, condenser, and dropping funnel, 2 parts by weight of LiN (C 2 F 5 SO 2 ) 2 , polypropylene glycol (diol type, number average molecular weight 2000, ethylene glycol group ratio 0 weight) %: PPG) and 80 parts by weight of ethyl acetate were charged, and the mixture was stirred for 2 hours while maintaining the liquid temperature in the flask at around 80 ° C. to prepare an antistatic agent solution (d) (20% by weight). .
- Antistatic agent solution (e) In a four-necked flask equipped with a stirring blade, thermometer, condenser, and dropping funnel, 0.5 parts by weight of LiN (C 2 F 5 SO 2 ) 2 , polypropylene glycol-polyethylene glycol-polypropylene glycol block copolymer (number average) A molecular weight of 2000, an ethylene glycol group ratio of 50% by weight: 35 parts by weight of PEP and 142 parts by weight of ethyl acetate were charged, and the mixture was stirred for 2 hours while maintaining the liquid temperature in the flask at around 80 ° C. ) (20 wt%) was prepared.
- Antistatic agent by diluting 10 parts by weight of antistatic agent (manufactured by Solvex, Microsolver RMd-142, mainly composed of tin oxide and polyester resin) with a mixed solvent of 30 parts by weight of water and 70 parts by weight of methanol An agent solution was prepared. The obtained antistatic agent solution was applied onto a polyethylene terephthalate (PET) film (thickness 38 ⁇ m, base material layer) using a Mayer bar and dried at 130 ° C. for 1 minute to remove the solvent and charge An antistatic layer (thickness 0.2 ⁇ m) was formed to produce an antistatic-treated PET film.
- PET polyethylene terephthalate
- Example 1> (Preparation of adhesive solution) 0.5 parts by weight of the antistatic agent (a) with respect to 100 parts by weight of the solid content of the acrylic polymer (A), and a trimethylolpropane / tolylene diisocyanate trimer adduct as a crosslinking agent (Nippon Polyurethane) Kogyo Co., Ltd., Coronate: C / L) 0.5 parts by weight and 0.03 part by weight of dibutyltin dilaurate as a cross-linking catalyst were added, mixed and stirred, and diluted to 20% by weight with ethyl acetate.
- An acrylic pressure-sensitive adhesive solution (1) was prepared.
- the description in the said weight part has shown the weight of solid content. The same applies to the following.
- the acrylic pressure-sensitive adhesive solution (1) is applied to the surface opposite to the antistatic-treated surface of the antistatic-treated PET film prepared as described above, heated at 110 ° C. for 3 minutes, and has a thickness of 20 ⁇ m. An agent layer was formed. Next, a silicone-treated surface of a polyethylene terephthalate (PET) film (thickness: 25 ⁇ m) having a silicone treatment on one side was bonded to the surface of the pressure-sensitive adhesive layer to produce an adhesive film. When the adhesive film was used, the silicone-treated PET film was peeled off and used.
- PET polyethylene terephthalate
- Example 2 An adhesive film was prepared in the same manner as in Example 1 except that 1.0 part by weight of the antistatic agent (b) was used instead of the antistatic agent (a) in the adjustment of the adhesive of Example 1. .
- Example 3 An adhesive film was prepared in the same manner as in Example 1 except that 0.5 parts by weight of the antistatic agent (c) was used instead of the antistatic agent (a) in the adjustment of the adhesive of Example 1. .
- Example 4 An adhesive film was prepared in the same manner as in Example 1 except that 0.75 parts by weight of the antistatic agent (c) was used in place of the antistatic agent solution (a) in the adjustment of the adhesive of Example 1. did.
- Example 5 An adhesive film was prepared in the same manner as in Example 1 except that 1.0 part by weight of the antistatic agent (d) was used instead of the antistatic agent solution (a) in the adjustment of the adhesive of Example 1. did.
- Example 6> In the preparation of the pressure-sensitive adhesive of Example 1, 1.5 parts by weight of the above-mentioned antistatic agent (c) was used instead of the antistatic agent (a), and trimethylolpropane / tolylene diisocyanate trimer was used as a crosslinking agent. Except for using 0.2 parts by weight of isocyanurate of hexamethylene diisocyanate (manufactured by Nippon Polyurethane Industry Co., Ltd., Coronate: C / HX) instead of the adduct (Nihon Polyurethane Industry Co., Ltd., Coronate: C / L) Produced an adhesive film by the same method as in Example 1.
- Example 1 A pressure-sensitive adhesive film was produced in the same manner as in Example 1 except that the antistatic agent solution (a) was not used in the adjustment of the pressure-sensitive adhesive in Example 1.
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Abstract
Description
作製したポリマーの重量平均分子量は、GPC(ゲル・パーミエーション・クロマトグラフィー)により測定した。
カラム:
サンプルカラム;東ソー社製、TSKguardcolumn Super HZ-H(1 本)+TSKgel Super HZM-H(2本)
リファレンスカラム;東ソー社製、TSKgel Super H-RC(1本)
流量:0.6ml/分
サンプル注入量:10μl
カラム温度:40℃
溶離液:THF
注入試料濃度:0.2重量%
検出器:示差屈折計
なお、重量平均分子量はポリスチレン換算により算出した。
ガラス転移温度Tg(℃)は、各モノマーによるホモポリマーのガラス転移温度Tgn(℃)として下記の文献値を用い、下記の式により求めた。
(式中、Tg(℃)は共重合体のガラス転移温度、Wn(-)は各モノマーの重量分率、Tgn(℃)は各モノマーによるホモポリマーのガラス転移温度、nは各モノマーの種類を表す。)
2-エチルヘキシルアクリレート:-70℃
イソノニルアクリレート:-82℃
ブチルアクリレート:-55℃
エチルアクリレート:-22℃
2-ヒドロキシエチルアクリレート:-15℃
アクリル酸:106℃
なお、文献値として「アクリル樹脂の合成・設計と新用途開発」(中央経営開発センター出版部発行)を参照した。
酸価は、自動滴定装置(平沼産業社製、COM-550)を用いて測定を行い、下記式より求めた。
A;酸価
Y;サンプル溶液の滴定量(ml)
X;混合溶媒50gのみの溶液の滴定量(ml)
f;滴定溶液のファクター
M;ポリマーサンプルの重量(g)
なお、測定条件は下記の通りである。
電極:ガラス電極;GE-101、比較電極;RE-201
測定モード:石油製品中和価試験1
アクリルパネル(三菱レーヨン社製、アクリライト)に、幅25mm、長さ100mmのサイズにカットした粘着フィルムを0.25MPa、速度0.3m/分の圧着条件でラミネートし、評価サンプルを作製した。ラミネート後30分間放置した後、万能引張試験機にて剥離速度0.3m/分、剥離角度180°で剥離したときの粘着力を測定した。測定は23℃×50%RHの環境下で行った。
粘着フィルムを幅70mm、長さ130mmのサイズにカットし、セパレーターを剥離した後、あらかじめ除電しておいた厚み1mm、幅70mm、長さ100mmのアクリルパネル(三菱レーヨン社製、アクリライト)表面に片方の端部が30mmはみ出すようにハンドローラーにて圧着した。23℃×50%RHの環境下に1日放置した後、下記に示すように所定の位置にサンプルをセットした。30mmはみ出した片方の端部を自動巻取り機に固定し、剥離角度150°、剥離速度10m/分となるように剥離した。剥離した粘着フィルムをサンプル固定台に設置し、粘着剤表面の電位を、所定の位置に固定してある電位測定機(春日電機社製、KSD-0103)にて測定した。測定は、23℃×50%RHの環境下で行った。
〔アクリル系ポリマー(A)〕
攪拌羽根、温度計、窒素ガス導入管、冷却器、滴下ロートを備えた四つ口フラスコに2-エチルヘキシルアクリレート200重量部、2-ヒドロキシエチルアクリレート8重量部、重合開始剤として2,2’-アゾビスイソブチロニトリル0.4重量部、酢酸エチル312重量部を仕込み、緩やかに攪拌しながら窒素ガスを導入し、フラスコ内の液温を65℃付近に保って6時間重合反応を行い、アクリル系ポリマー(A)溶液(40重量%)を調製した。前記アクリル系ポリマー(A)の重量平均分子量は50万、ガラス転移温度(Tg)は-68℃、酸価は0.0であった。
〔帯電防止剤溶液(a)〕
攪拌羽根、温度計、冷却器、滴下ロートを備えた四つ口フラスコにヨウ化リチウム20重量部、酢酸エチル80重量部を仕込み、フラスコ内の液温を80℃付近に保って2時間混合攪拌を行い、帯電防止剤溶液(a)(20重量%)を調製した。
攪拌羽根、温度計、冷却器、滴下ロートを備えた四つ口フラスコに過塩素酸リチウム20重量部、酢酸エチル80重量部を仕込み、フラスコ内の液温を80℃付近に保って2時間混合攪拌を行い、帯電防止剤溶液(b)(20重量%)を調製した。
攪拌羽根、温度計、冷却器、滴下ロートを備えた四つ口フラスコにLiN(C2F5SO2)21重量部、ポリプロピレングリコール-ポリエチレングリコール-ポリプロピレングリコールブロック共重合体(数平均分子量2000、エチレングリコール基比率50重量%:PEP)14重量部、酢酸エチル60重量部を仕込み、フラスコ内の液温を80℃付近に保って2時間混合攪拌を行い、帯電防止剤溶液(c)(20重量%)を調製した。
攪拌羽根、温度計、冷却器、滴下ロートを備えた四つ口フラスコにLiN(C2F5SO2)22重量部、ポリプロピレングリコール(ジオール型、数平均分子量2000、エチレングリコール基比率0重量%:PPG)18重量部、酢酸エチル80重量部を仕込み、フラスコ内の液温を80℃付近に保って2時間混合攪拌を行い、帯電防止剤溶液(d)(20重量%)を調製した。
攪拌羽根、温度計、冷却器、滴下ロートを備えた四つ口フラスコにLiN(C2F5SO2)20.5重量部、ポリプロピレングリコール-ポリエチレングリコール-ポリプロピレングリコールブロック共重合体(数平均分子量2000、エチレングリコール基比率50重量%:PEP)35重量部、酢酸エチル142重量部を仕込み、フラスコ内の液温を80℃付近に保って2時間混合攪拌を行い、帯電防止剤溶液(e)(20重量%)を調製した。
帯電防止剤(ソルベックス社製、マイクロソルバーRMd-142、酸化スズとポリエステル樹脂を主成分とする)10重量部を、水30重量部とメタノール70重量部からなる混合溶媒で希釈することにより帯電防止剤溶液を調製した。得られた前記帯電防止剤溶液を、ポリエチレンテレフタレート(PET)フィルム(厚さ38μm、基材層)上にマイヤーバーを用いて塗布し、130℃で1分間乾燥することにより溶剤を除去して帯電防止層(厚さ0.2μm)を形成し、帯電防止処理PETフィルムを作製した。
〔粘着剤溶液の調製〕
上記アクリル系ポリマー(A)の固形分100重量部に対して上記帯電防止剤(a)0.5重量部、架橋剤としてトリメチロ-ルプロパン/トリレンジイソシアネ-ト3量体付加物(日本ポリウレタン工業社製、コロネ-ト:C/L)0.5重量部、架橋触媒としてジラウリン酸ジブチルスズ0.03重量部を、それぞれ加えて混合攪拌し、これを酢酸エチルで20重量%に希釈して、アクリル系粘着剤溶液(1)を調製した。なお、前記重量部での記載は、固形分の重量を示している。以下も同様である。
上記アクリル系粘着剤溶液(1)を、上述のように作製した帯電防止処理PETフィルムの帯電防止処理面とは反対の面に塗布し、110℃で3分間加熱して、厚さ20μmの粘着剤層を形成した。次いで、上記粘着剤層の表面に、片面にシリコーン処理を施したポリエチレンテレフタレート(PET)フィルム(厚さ25μm)のシリコーン処理面を貼り合わせ、粘着フィルムを作製した。なお、前記粘着フィルムの使用時には、前記シリコーン処理を施したPETフィルムを剥離して、使用した。
実施例1の粘着剤の調整で帯電防止剤(a)に代えて、上記帯電防止剤(b)1.0重量部を用いた以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤(a)に代えて、上記帯電防止剤(c)0.5重量部を用いた以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤溶液(a)に代えて、上記帯電防止剤(c)0.75重量部を用いた以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤溶液(a)に代えて、上記帯電防止剤(d)1.0重量部を用いた以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤(a)に代えて、上記帯電防止剤(c)1.5重量部を用い、架橋剤としてトリメチロ-ルプロパン/トリレンジイソシアネ-ト3量体付加物(日本ポリウレタン工業社製、コロネ-ト:C/L)に代えて、ヘキサメチレンジイソシアネートのイソシアヌレート体(日本ポリウレタン工業社製、コロネート:C/HX)0.2重量部を用いた以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤溶液(a)を用いないこと以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤(a)0.7重量部を用い、架橋剤としてトリメチロ-ルプロパン/トリレンジイソシアネ-ト3量体付加物(日本ポリウレタン工業社製、コロネ-ト:C/L)2.5重量部用いた以外は、実施例1と同様の方法により粘着フィルムを作製した。
実施例1の粘着剤の調整で帯電防止剤(a)に代えて、上記帯電防止剤(e)3.55重量部を用いたこと以外は、実施例1と同様の方法により粘着フィルムを作製した。
Claims (6)
- 基材層と、前記基材層の少なくとも片面に粘着剤層を有する粘着フィルムにおいて、
前記粘着剤層が、(メタ)アクリル系ポリマー、アルカリ金属塩、及び、架橋剤を含有し、
前記(メタ)アクリル系ポリマー100重量部に対して、前記架橋剤を2重量部以下含有し、
前記粘着フィルムの粘着力(被着体:アクリルパネル、23℃×50%RH条件下で30分経過後)が、引張速度0.3m/分において、0.5N/25mm以上であることを特徴とする粘着フィルム。 - 剥離帯電圧(被着体:アクリルパネル、23℃×50%RH条件下)が、剥離速度10m/分において、絶対値が0.5kV以下であることを特徴とする請求項1に記載の粘着フィルム。
- 前記アルカリ金属塩が、リチウム塩であることを特徴とする請求項1又は2に記載の粘着フィルム。
- 前記粘着剤層が、ポリエーテルポリオール化合物を含有することを特徴とする請求項1~3のいずれかに記載の粘着フィルム。
- 光学部材用保護フィルムであることを特徴とする請求項1~4のいずれかに記載の粘着フィルム。
- 拡散シート用保護フィルムであることを特徴とする請求項1~4のいずれかに記載の粘着フィルム。
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CN201280020111.8A CN103492513A (zh) | 2011-05-23 | 2012-05-11 | 粘合薄膜 |
KR1020137033999A KR20140035422A (ko) | 2011-05-23 | 2012-05-11 | 점착 필름 |
US14/119,530 US20140099504A1 (en) | 2011-05-23 | 2012-05-11 | Pressure-sensitive adhesive film |
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KR (1) | KR20140035422A (ja) |
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WO2014097719A1 (ja) * | 2012-12-19 | 2014-06-26 | 昭和電工株式会社 | 光学フィルム用粘着剤組成物及び表面保護フィルム |
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JP6285289B2 (ja) * | 2014-06-17 | 2018-02-28 | 日本カーバイド工業株式会社 | 粘着剤組成物、及び表示装置 |
CN104497902B (zh) * | 2014-12-31 | 2017-01-04 | 斯迪克新型材料(江苏)有限公司 | 用于显示屏的防蓝光光学胶带 |
JP6426071B2 (ja) * | 2015-09-14 | 2018-11-21 | 藤森工業株式会社 | 表面保護フィルム、及びそれが貼合された光学部品 |
KR101956547B1 (ko) * | 2016-03-09 | 2019-03-11 | 미쯔비시 케미컬 주식회사 | 점착 필름 및 그의 제조방법 |
KR102546280B1 (ko) * | 2016-07-22 | 2023-06-23 | 삼성디스플레이 주식회사 | 아크릴계 점착제 및 이를 포함하는 보호 필름 |
JP7080216B2 (ja) * | 2017-03-03 | 2022-06-03 | リンテック株式会社 | ガスバリア性接着フィルム、並びに、電子部材及び光学部材 |
JP6562488B2 (ja) * | 2018-10-23 | 2019-08-21 | 藤森工業株式会社 | 表面保護フィルム、及びそれが貼合された光学部品 |
JP2021006404A (ja) * | 2020-09-02 | 2021-01-21 | 藤森工業株式会社 | 帯電防止表面保護フィルム |
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JP2012241154A (ja) | 2012-12-10 |
KR20140035422A (ko) | 2014-03-21 |
US20140099504A1 (en) | 2014-04-10 |
JP5774375B2 (ja) | 2015-09-09 |
CN103492513A (zh) | 2014-01-01 |
TW201313867A (zh) | 2013-04-01 |
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