WO2018123688A1 - 表面保護フィルム - Google Patents
表面保護フィルム Download PDFInfo
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- WO2018123688A1 WO2018123688A1 PCT/JP2017/045320 JP2017045320W WO2018123688A1 WO 2018123688 A1 WO2018123688 A1 WO 2018123688A1 JP 2017045320 W JP2017045320 W JP 2017045320W WO 2018123688 A1 WO2018123688 A1 WO 2018123688A1
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- WIPO (PCT)
- Prior art keywords
- meth
- separator
- acrylate
- pressure
- sensitive adhesive
- Prior art date
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- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/023—Optical properties
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/06—Interconnection of layers permitting easy separation
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- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
Definitions
- the present invention relates to an optical surface protective film with a separator.
- an optical surface protection film with a separator used for protecting the surface of an optical member for example, a polarizing plate, a wave plate, a retardation plate, an optical compensation film, a reflection sheet, a brightness enhancement film, etc. used in a liquid crystal display
- the position of the optical member can be adjusted accurately with respect to the surface of the optical member. After the position adjustment, the separator is peeled off, so that the optical surface protective film can be bonded to the surface of the optical member at an accurate position, which is useful.
- the surface protective film generally has a configuration in which an adhesive layer is provided on a film-like base film (support). Such a surface protective film is bonded to an optical member as an adherend through the pressure-sensitive adhesive layer, and is used for the purpose of protecting the optical member from scratches and dirt on the surface during processing, transportation, inspection, and the like. It is done.
- a panel of a liquid crystal display is formed by bonding an optical member such as a polarizing plate or a wave plate to a liquid crystal cell via an adhesive layer.
- Such a pressure-sensitive adhesive layer is protected and stored by a release-treated separator or the like from the necessity of protection from drying or the like before being actually attached to an optical member (Patent Document 1).
- the surface protective film is peeled off and removed when it is no longer needed.
- the surface protective film with a separator is bonded to the optical member surface, only the surface protective film is cut to a desired size so as not to cut the separator in order to perform bonding at an accurate position.
- a hole is made in the outer edge, the perforated part is sensed by a sensor, the position is adjusted using an automatic laminating machine, and then the separator is peeled off, and then, it is bonded to the surface of the optical member.
- An object of the present invention is to provide an optical surface protective film with a separator that is excellent in position adjustability based on a separator and can be attached to an optical member surface at an accurate position when being bonded.
- the optical surface protective film with a separator of the present invention has an optical surface protective film having an adhesive layer on at least one side of the substrate film, and a surface opposite to the surface in contact with the adhesive layer of the substrate film.
- the base film is preferably a polyester film.
- the optical surface protective film with a separator of the present invention is formed from an adhesive composition in which the adhesive layer contains at least one selected from an acrylic adhesive, a urethane adhesive, and a silicone adhesive. It is preferred that
- the position of the optical surface protective film with a separator is adjusted with respect to the surface of the optical member by using an automatic laminator, and the surface of the optical member is separated after the separator is peeled off.
- an optical surface protective film with a separator that is excellent in positional adjustability based on the separator and can be applied to the surface of the optical member at an accurate position, and is useful.
- An optical surface protective film with a separator disclosed herein is generally a pressure-sensitive adhesive layer surface in a form called an adhesive tape, an adhesive label, an adhesive film, or the like. Is protected by a separator, and in particular, surface protection that protects the surface of optical components during processing, inspection, and transportation of optical components (for example, optical components used as liquid crystal display panel components such as polarizing plates and wave plates). Suitable as a film.
- the pressure-sensitive adhesive layer in the surface protective film is typically formed continuously, but is not limited to such a form, and is formed in a regular or random pattern such as a spot or stripe. It may be an adhesive layer.
- the surface protective film disclosed herein may be in the form of a roll or a single sheet.
- the optical surface protective film with a separator of the present invention has a base film.
- the resin material constituting the base film can be used without any particular limitation. For example, transparency, mechanical strength, thermal stability, moisture shielding property, isotropic property, It is preferable to use a material excellent in properties such as flexibility and dimensional stability.
- the pressure-sensitive adhesive composition can be applied by a roll coater or the like, and can be wound up into a roll shape, which is useful.
- the base film (support) examples include polyester polymers such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), and polybutylene terephthalate; cellulose polymers such as diacetyl cellulose and triacetyl cellulose; polycarbonate polymers; An acrylic polymer such as polymethyl methacrylate; and the like, a plastic film composed of a resin material having a main resin component (a main component of the resin component, typically a component occupying 50% by weight or more), It can be preferably used as a film.
- polyester polymers such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), and polybutylene terephthalate
- cellulose polymers such as diacetyl cellulose and triacetyl cellulose
- polycarbonate polymers An acrylic polymer such as polymethyl methacrylate
- An acrylic polymer such as polymethyl methacrylate; and the like
- the resin material examples include styrene polymers such as polystyrene and acrylonitrile-styrene copolymers; olefin polymers such as polyethylene, polypropylene, polyolefins having a cyclic or norbornene structure, and ethylene-propylene copolymers; Examples of the resin material include vinyl chloride polymers; amide polymers such as nylon 6, nylon 6,6, and aromatic polyamide. Still other examples of the resin material include imide polymers, sulfone polymers, polyether sulfone polymers, polyether ether ketone polymers, polyphenylene sulfide polymers, vinyl alcohol polymers, vinylidene chloride polymers, vinyl butyral polymers. , Arylate polymers, polyoxymethylene polymers, epoxy polymers and the like. A base film made of a blend of two or more of the above-described polymers may be used.
- the base film a plastic film made of a transparent thermoplastic resin material can be preferably used.
- the plastic films it is more preferable to use a polyester film.
- the polyester film includes a polyester polymer material (polyester resin) having a main skeleton based on an ester bond such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polybutylene terephthalate, or the like as a main resin component.
- PET polyethylene terephthalate
- PEN polyethylene naphthalate
- polybutylene terephthalate or the like as a main resin component.
- Such a polyester film has preferable characteristics as a base film for a surface protective film, such as excellent optical characteristics and dimensional stability.
- various additives such as an antioxidant, an ultraviolet absorber, a plasticizer, and a colorant (pigment, dye, etc.) may be blended as necessary.
- a known or conventional surface treatment such as corona discharge treatment, plasma treatment, ultraviolet irradiation treatment, acid treatment, alkali treatment, and application of a primer may be performed.
- Such surface treatment can be, for example, a treatment for improving the adhesion between the base film and the pressure-sensitive adhesive layer (the anchoring property of the pressure-sensitive adhesive layer).
- the substrate film It is also possible to use a plastic film that has been subjected to antistatic treatment as the substrate film.
- Use of the base film is preferable because charging of the surface protective film itself when peeled can be suppressed.
- the base film is a plastic film, and an antistatic treatment is performed on the plastic film, so that the surface protection film itself can be reduced in charge and can have an excellent antistatic ability on the adherend.
- a conventionally well-known method can be used, for example, antistatic resin which consists of an antistatic agent and a resin component, a conductive polymer, and a conductive substance. Examples thereof include a method of applying a conductive resin, a method of depositing or plating a conductive material, a method of kneading an antistatic agent, and the like.
- the thickness of the substrate film is usually about 5 to 200 ⁇ m, preferably about 10 to 100 ⁇ m.
- the thickness of the base film is within the above range, it is preferable because it is excellent in bonding workability to the adherend, peelability from the adherend and workability.
- the surface protective film disclosed herein may be implemented in an embodiment that further includes other layers in addition to the base film, the pressure-sensitive adhesive layer, and the separator.
- the other layer include an undercoat layer (anchor layer) that improves the anchoring property of the antistatic layer and the pressure-sensitive adhesive layer.
- the pressure-sensitive adhesive layer used in the present invention can be used without particular limitation as long as it is formed from a pressure-sensitive adhesive composition containing a pressure-sensitive adhesive polymer.
- the pressure-sensitive adhesive composition include acrylic pressure-sensitive adhesives, urethane-based pressure-sensitive adhesives, synthetic rubber-based pressure-sensitive adhesives, natural rubber-based pressure-sensitive adhesives, silicone-based pressure-sensitive adhesives, and polyester-based pressure-sensitive adhesives.
- the (meth) acrylic polymer which is a pressure-sensitive polymer constituting the acrylic pressure-sensitive adhesive
- the (meth) acrylic polymer is an alkyl having 1 to 14 carbon atoms as a raw material monomer constituting the pressure-sensitive adhesive layer.
- a (meth) acrylic monomer having a group can be used as the main monomer.
- As said (meth) acrylic-type monomer 1 type (s) or 2 or more types can be used.
- the (meth) acrylic polymer refers to an acrylic polymer and / or a methacrylic polymer
- the (meth) acrylate refers to acrylate and / or methacrylate.
- the (meth) acrylic monomer having an alkyl group having 1 to 14 carbon atoms include, for example, methyl (meth) acrylate, ethyl (meth) acrylate, n-butyl (meth) acrylate, s-butyl (meth) ) Acrylate, t-butyl (meth) acrylate, isobutyl (meth) acrylate, hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, isooctyl (meth) acrylate, n-nonyl ( (Meth) acrylate, isononyl (meth) acrylate, n-decyl (meth) acrylate, isodecyl (meth) acrylate, n-dodecyl (meth) acrylate, n-tridecyl (
- a (meth) acrylic monomer having an alkyl group having 4 to 14 carbon atoms, such as acrylate is preferred.
- by using a (meth) acrylic monomer having an alkyl group having 4 to 14 carbon atoms, such as acrylate is preferred.
- a (meth) acrylic monomer having an alkyl group having 1 to 14 carbon atoms with respect to 100% by weight of the total amount of monomer components constituting the (meth) acrylic polymer. More preferably, it is 75% by weight or more, more preferably 85 to 99.9% by weight, and most preferably 90 to 99% by weight. If it is less than 65% by weight, the appropriate wettability of the pressure-sensitive adhesive composition and the cohesive strength of the pressure-sensitive adhesive layer are inferior, which is not preferable.
- a hydroxyl group-containing (meth) acrylic monomer can be used as a raw material monomer.
- hydroxyl group containing (meth) acrylic-type monomer 1 type (s) or 2 or more types can be used.
- hydroxyl group-containing (meth) acrylic monomer examples include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, and 6-hydroxyhexyl (meth) acrylate. , 8-hydroxyoctyl (meth) acrylate, 10-hydroxydecyl (meth) acrylate, 12-hydroxylauryl (meth) acrylate, (4-hydroxymethylcyclohexyl) methyl acrylate, N-methylol (meth) acrylamide, etc. .
- the hydroxyl group-containing (meth) acrylic monomer is preferably contained in an amount of 25% by weight or less, more preferably 15% by weight or less, based on 100% by weight of the total amount of monomer components constituting the (meth) acrylic polymer. More preferably, the content is 0.1 to 10% by weight. Within the above range, the balance between the wettability of the pressure-sensitive adhesive composition and the cohesive force of the resulting pressure-sensitive adhesive layer can be easily controlled, which is preferable.
- the glass transition temperature and release of the (meth) acrylic polymer should be adjusted so that the Tg is 0 ° C. or lower (usually ⁇ 100 ° C. or higher) because the adhesive performance is easily balanced.
- a polymerizable monomer or the like for adjusting the property can be used as long as the effects of the present invention are not impaired.
- the (meth) acrylic polymer can use a carboxyl group-containing (meth) acrylic monomer as a raw material monomer.
- the pressure-sensitive adhesive layer surface protective film
- the pressure-sensitive adhesive layer can be prevented from increasing in adhesive strength over time, re-peelability, adhesive strength-increasing property, and work Excellent in properties.
- it is excellent in shearing force and is preferable.
- carboxyl group-containing (meth) acrylic monomer examples include (meth) acrylic acid, carboxylethyl (meth) acrylate, carboxylpentyl (meth) acrylate, and the like.
- the carboxyl group-containing (meth) acrylic monomer is preferably 10% by weight or less, preferably 0 to 8% by weight with respect to 100% by weight of the total amount of monomer components constituting the (meth) acrylic polymer. Is more preferably 0 to 6% by weight. Within the above range, the balance between the wettability of the pressure-sensitive adhesive composition and the cohesive force of the resulting pressure-sensitive adhesive layer can be easily controlled, which is preferable.
- the (meth) acrylic polymer can be used without any particular limitation as long as other polymerizable monomers other than the raw material monomer are within the range not impairing the characteristics of the present invention.
- a cohesive force / heat resistance improving component such as a cyano group-containing monomer, vinyl ester monomer, aromatic vinyl monomer, amide group-containing monomer, imide group-containing monomer, amino group-containing monomer, epoxy
- a component having a functional group that functions as a crosslinking base point can be used as appropriate, such as a group-containing monomer, N-acryloylmorpholine, vinyl ether monomer, and the like.
- a nitrogen-containing monomer such as a cyano group-containing monomer, an amide group-containing monomer, an imide group-containing monomer, an amino group-containing monomer, and N-acryloylmorpholine.
- a nitrogen-containing monomer is useful because it can ensure an appropriate peeling force (adhesive strength) that does not cause floating or peeling, and can provide a surface protective film having excellent shearing force.
- These polymerizable monomers can be used alone or in combination of two or more.
- Examples of the cyano group-containing monomer include acrylonitrile and methacrylonitrile.
- Examples of the amide group-containing monomer include acrylamide, methacrylamide, diethylacrylamide, N-vinylpyrrolidone, N, N-dimethylacrylamide, N, N-dimethylmethacrylamide, N, N-diethylacrylamide, and N, N-diethyl.
- Examples include methacrylamide, N, N′-methylenebisacrylamide, N, N-dimethylaminopropyl acrylamide, N, N-dimethylaminopropyl methacrylamide, and diacetone acrylamide.
- Examples of the imide group-containing monomer include cyclohexylmaleimide, isopropylmaleimide, N-cyclohexylmaleimide, and itaconimide.
- amino group-containing monomer examples include aminoethyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, N, N-dimethylaminopropyl (meth) acrylate, and the like.
- Examples of the vinyl ester monomer include vinyl acetate, vinyl propionate, and vinyl laurate.
- aromatic vinyl monomer examples include styrene, chlorostyrene, chloromethyl styrene, ⁇ -methyl styrene, and other substituted styrene.
- epoxy group-containing monomer examples include glycidyl (meth) acrylate, methyl 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 other polymerizable monomer is preferably 0 to 30% by weight, and preferably 0 to 10% by weight, based on 100% by weight of the total amount of monomer components constituting the (meth) acrylic polymer. It is more preferable.
- the other polymerizable monomers can be appropriately adjusted in order to obtain desired characteristics.
- the (meth) acrylic polymer may further contain an alkylene oxide group-containing reactive monomer as a monomer component.
- the average addition mole number of the oxyalkylene unit of the alkylene oxide group-containing reactive monomer is preferably 1 to 40, and preferably 3 to 40 from the viewpoint of compatibility with the oxyalkylene group-containing compound. Is more preferably 4 to 35, and particularly preferably 5 to 30.
- the average added mole number is 1 or more, the effect of reducing the contamination of the adherend (protected body) tends to be obtained efficiently.
- the said average added mole number is larger than 40, since interaction with an oxyalkylene group containing compound is large and there exists a tendency for the viscosity of an adhesive composition to rise and for coating to become difficult, it is unpreferable.
- the terminal of the oxyalkylene chain may be a hydroxyl group or may be substituted with another functional group.
- the alkylene oxide group-containing reactive monomer may be used alone or in combination of two or more, but the total content is the total amount of monomer components of the (meth) acrylic polymer. Among them, 0 to 20% by weight is preferable, and 0 to 10% by weight is more preferable. When the content of the alkylene oxide group-containing reactive monomer exceeds 20% by weight, the contamination on the adherend deteriorates, which is not preferable.
- Examples of the oxyalkylene unit of the alkylene oxide group-containing reactive monomer include those having an alkylene group having 1 to 6 carbon atoms, such as an oxymethylene group, an oxyethylene group, an oxypropylene group, and an oxybutylene group. It is done.
- the hydrocarbon group of the oxyalkylene chain may be linear or branched.
- the alkylene oxide group-containing reactive monomer is a reactive monomer having an ethylene oxide group.
- a reactive monomer-containing (meth) acrylic polymer having an ethylene oxide group as a base polymer, the compatibility between the base polymer and the oxyalkylene group-containing compound is improved, and bleeding to the adherend is suitably suppressed, A low-contamination pressure-sensitive adhesive composition is obtained.
- alkylene oxide group-containing reactive monomer examples include (meth) acrylic acid alkylene oxide adducts and reactive surfactants having reactive substituents such as acryloyl group, methacryloyl group, and allyl group in the molecule. can give.
- the (meth) acrylic acid alkylene oxide adduct include, for example, polyethylene glycol (meth) acrylate, polypropylene glycol (meth) acrylate, polyethylene glycol-polypropylene glycol (meth) acrylate, polyethylene glycol-polybutylene glycol (meth) ) Acrylate, polypropylene glycol-polybutylene glycol (meth) acrylate, methoxy polyethylene glycol (meth) acrylate, ethoxy polyethylene glycol (meth) acrylate, butoxy polyethylene glycol (meth) acrylate, octoxy polyethylene glycol (meth) acrylate, lauroxy polyethylene Glycol (meth) acrylate, stearoxy polyethylene glycol Lumpur (meth) acrylate, phenoxy polyethylene glycol (meth) acrylate, methoxy polypropylene glycol (meth) acrylate, octoxypolyethylene glycol - polyprop
- the reactive surfactant include, for example, an anionic reactive surfactant having a (meth) acryloyl group or an allyl group, a nonionic reactive surfactant, and a cationic reactive surfactant. Can be given.
- the (meth) acrylic polymer preferably has a weight average molecular weight (Mw) of 100,000 to 5,000,000, more preferably 200,000 to 4,000,000, still more preferably 300,000 to 3,000,000, and most preferably 300,000 to 1,200,000. It is.
- Mw weight average molecular weight
- the adhesive force tends to be generated due to the reduced cohesive force of the pressure-sensitive adhesive layer.
- the weight average molecular weight exceeds 5,000,000, the fluidity of the polymer is lowered, the wetness to the adherend (for example, polarizing plate) becomes insufficient, and the adherend and the pressure-sensitive adhesive layer of the surface protective film It tends to cause blisters that occur during the period.
- 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, more preferably ⁇ 10 ° C. or lower (usually ⁇ 100 ° C. or higher).
- the glass transition temperature is higher than 0 ° C., the polymer does not flow easily, for example, the wettability to the polarizing plate which is an optical member becomes insufficient, and the swelling generated between the polarizing plate and the pressure-sensitive adhesive layer of the surface protective film There is a tendency to cause.
- the glass transition temperature is preferably ⁇ 40 ° C. or less, and more preferably ⁇ 70 ° C. or less, whereby an adhesive layer excellent in wettability to the polarizing plate and light peelability can be easily obtained.
- the glass transition temperature 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 is not particularly limited, and can be polymerized by known methods such as solution polymerization, emulsion polymerization, bulk polymerization, suspension polymerization, etc. From the viewpoint of characteristics such as low contamination to the adherend (protected body), solution polymerization is a more preferable embodiment. Further, the polymer obtained may be any of a random copolymer, a block copolymer, an alternating copolymer, a graft copolymer, and the like.
- urethane-based pressure-sensitive adhesive can be adopted when a urethane-based pressure-sensitive adhesive is used for the pressure-sensitive adhesive layer.
- a urethane type adhesive Preferably, what consists of a urethane type polymer which is an adhesive polymer obtained by making a polyol and a polyisocyanate compound react is mentioned.
- the polyol include polyether polyol, polyester polyol, polycarbonate polyol, and polycaprolactone polyol.
- the polyisocyanate compound include diphenylmethane diisocyanate, tolylene diisocyanate, hexamethylene diisocyanate, and the like.
- any appropriate silicone-based pressure-sensitive adhesive can be adopted.
- a silicone-based pressure-sensitive adhesive one obtained by blending or agglomerating a silicone-based polymer that is a pressure-sensitive polymer can be preferably used.
- silicone pressure-sensitive adhesive examples include addition reaction curable silicone pressure-sensitive adhesives and peroxide curable silicone pressure-sensitive adhesives.
- peroxides benzoyl peroxide and the like
- an addition reaction curable silicone pressure-sensitive adhesive is preferable.
- the curing reaction of the addition reaction curable silicone pressure-sensitive adhesive for example, when obtaining a polyalkyl silicone pressure-sensitive adhesive, generally, a method of curing a polyalkylhydrogensiloxane composition with a platinum catalyst can be mentioned.
- the pressure-sensitive adhesive composition used in the present invention can also contain an oxyalkylene group-containing compound.
- an oxyalkylene group-containing compound By containing the oxyalkylene group-containing compound, it is possible to further develop light peelability.
- the oxyalkylene group-containing compound include an organopolysiloxane having an oxyalkylene chain and an oxyalkylene group-containing compound not containing an organopolysiloxane.
- organopolysiloxane having an oxyalkylene chain examples include specific examples of the organopolysiloxane having an oxyalkylene chain in the main chain, such as a commercial product, and trade names of X-22-4952, X-22. -4272, X-22-6266, KF-6004, KF-889 (above, manufactured by Shin-Etsu Chemical Co., Ltd.), BY16-201, SF8427 (above, made by Toray Dow Corning), IM22 (made by Asahi Kasei Wacker), etc. Is given.
- organosiloxane having an oxyalkylene chain in the side chain examples include, for example, trade names KF-351A, KF-352A, KF-353, KF-354L, KF-355A, KF-615A, KF-945.
- oxyalkylene group-containing compound not containing the organopolysiloxane examples include, for example, polyoxyalkylene alkylamine, polyoxyalkylene diamine, polyoxyalkylene fatty acid ester, polyoxyalkylene sorbitan fatty acid ester, polyoxyalkylene alkyl phenyl ether.
- Nonionic surfactants such as polyoxyalkylene alkyl ether, polyoxyalkylene alkyl allyl ether, polyoxyalkylene alkyl phenyl allyl ether; polyoxyalkylene alkyl ether sulfate ester salt, polyoxyalkylene alkyl ether phosphate ester salt, Oxyalkylene alkylphenyl ether sulfate ester salt, polyoxyalkylene alkylphenyl ether phosphate Anionic surfactants such as salt of salts; other cationic surfactants having polyoxyalkylene chains (polyalkylene oxide chains), amphoteric surfactants, polyether compounds having polyoxyalkylene chains (and their Derivatives), acrylic compounds having a polyoxyalkylene chain (and derivatives thereof), and the like. Moreover, you may mix
- Such polyoxyalkylene chain-containing compounds may
- polyether compound (polyether component) having a polyoxyalkylene chain examples include a block copolymer of polypropylene glycol (PPG) -polyethylene glycol (PEG), a block copolymer of PPG-PEG-PPG, Examples thereof include a block copolymer of PEG-PPG-PEG.
- the derivative of the polyether compound having a polyoxyalkylene chain include an oxypropylene group-containing compound (PPG monoalkyl ether, PEG-PPG monoalkyl ether, etc.) whose terminal is etherified, and oxypropylene whose terminal is acetylated Group-containing compounds (terminal acetylated PPG and the like), and the like.
- the acrylic compound having a polyoxyalkylene chain include a (meth) acrylate polymer having an oxyalkylene group.
- the oxyalkylene group has an addition mole number of oxyalkylene units of preferably 1 to 50, more preferably 2 to 30, and further preferably 2 to 20.
- the terminal of the oxyalkylene chain may be a hydroxyl group, or may be substituted with an alkyl group, a phenyl group or the like.
- the (meth) acrylate polymer having an oxyalkylene group is preferably a polymer containing (meth) acrylic acid alkylene oxide as a monomer component, and specific examples of the (meth) acrylic acid alkylene oxide include ethylene.
- glycol group-containing (meth) acrylates include methoxy-polyethylene glycol (meth) acrylate types such as methoxy-diethylene glycol (meth) acrylate and methoxy-triethylene glycol (meth) acrylate, ethoxy-diethylene glycol (meth) acrylate, ethoxy -Ethoxy-polyethylene glycol (meth) acrylate type such as triethylene glycol (meth) acrylate, butoxy-diethylene glycol (meth) acrylate, buto Butoxy-polyethylene glycol (meth) acrylate type such as cy-triethylene glycol (meth) acrylate, phenoxy-polyethylene glycol (meth) acrylate type
- the monomer component other monomer components other than the (meth) acrylic acid alkylene oxide can also be used.
- specific examples of other monomer components include methyl (meth) acrylate, ethyl (meth) acrylate, n-butyl (meth) acrylate, s-butyl (meth) acrylate, t-butyl (meth) acrylate, and isobutyl (meth) acrylate.
- the polyoxyalkylene chain-containing compound not containing the organopolysiloxane is a compound having at least a part of a (poly) ethylene oxide chain.
- compatibility with the base polymer is improved, bleeding to the adherend is suitably suppressed, and a low-staining adhesive composition is obtained.
- a PPG-PEG-PPG block copolymer is used, a pressure-sensitive adhesive excellent in low contamination can be obtained.
- the weight of the (poly) ethylene oxide chain in the total polyoxyalkylene chain-containing compound not containing the organopolysiloxane is preferably 5 to 90% by weight, more preferably 5 to 85%. % By weight, more preferably 5 to 80% by weight, most preferably 5 to 75% by weight.
- Examples of commercially available polyoxyalkylene chain-containing compounds that do not contain the organopolysiloxane include, for example, Adekapluronic 17R-4, Adekapluronic 25R-2 (all of which are manufactured by ADEKA), Latemul PD-420, LaterumPD -420, Latemul PD-450, Emulgen 120 (manufactured by Kao), Aqualon HS-10, KH-10, Neugen EA-87, EA-137, EA-157, EA-167, EA-177 (above, first Manufactured by Kogyo Seiyaku Co., Ltd.).
- the content of the oxyalkylene group-containing compound is 100 parts by weight of an adhesive polymer (main polymer, for example, (meth) acrylic polymer, urethane polymer, silicone polymer, etc.) constituting the adhesive composition.
- an adhesive polymer main polymer, for example, (meth) acrylic polymer, urethane polymer, silicone polymer, etc.
- the pressure-sensitive adhesive composition preferably contains a crosslinking agent. Moreover, in this invention, it can be set as an adhesive layer using the said adhesive composition.
- the pressure-sensitive adhesive composition is an acrylic pressure-sensitive adhesive containing the (meth) acrylic polymer
- the constitutional unit, the structural ratio, the selection and addition ratio of the cross-linking agent, etc. are appropriately determined. By adjusting and crosslinking, a pressure-sensitive adhesive layer (surface protective film) having more excellent heat resistance can be obtained.
- 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 may be used.
- an isocyanate compound or an epoxy compound is a preferred embodiment.
- these compounds may be used independently and may be used in mixture of 2 or more types.
- isocyanate compounds include aliphatic polyisocyanates such as trimethylene diisocyanate, butylene diisocyanate, hexamethylene diisocyanate (HDI), dimer acid diisocyanate, cyclopentylene diisocyanate, cyclohexylene diisocyanate, isophorone diisocyanate (IPDI), 1, Alicyclic isocyanates such as 3-bis (isocyanatomethyl) cyclohexane, aromatic isocyanates such as 2,4-tolylene diisocyanate, 4,4′-diphenylmethane diisocyanate, xylylene diisocyanate (XDI), and the isocyanate compound Allophanate bond, biuret bond, isocyanurate bond, uretdione bond, urea bond, carbodiimide bond Uretonimine bond, polyisocynate modified products thereof obtained by modifying the like oxadiazinetrione bond
- These isocyanate compounds may be used alone, or may be used in combination of two or more, and a bifunctional isocyanate compound and a trifunctional or higher isocyanate compound may be used in combination.
- a cross-linking agent in combination, it is possible to achieve both tackiness and rebound resistance (adhesion to curved surfaces), and a pressure-sensitive adhesive layer (surface protective film) with better adhesion reliability can be obtained.
- epoxy compound examples include N, N, N ′, N′-tetraglycidyl-m-xylenediamine (trade name: TETRAD-X, manufactured by Mitsubishi Gas Chemical Co., Ltd.) and 1,3-bis (N, N-dioxy). Glycidylaminomethyl) cyclohexane (trade name: TETRAD-C, manufactured by Mitsubishi Gas Chemical Company, Inc.).
- Examples of the melamine resin include hexamethylol melamine.
- Examples of the aziridine derivative include commercially available product names HDU, TAZM, TAZO (manufactured by Mutual Yakugyo Co., Ltd.) and the like.
- metal chelate compound examples include aluminum, iron, tin, titanium, and nickel as metal components, and acetylene, methyl acetoacetate, and ethyl lactate as chelate components.
- the content of the crosslinking agent used in the present invention is, for example, preferably 0.01 to 20 parts by weight, and 0.1 to 15 parts by weight with respect to 100 parts by weight of the (meth) acrylic polymer. More preferred is 0.5 to 10 parts by weight, still more preferred is 1 to 8 parts by weight.
- the content is less than 0.01 parts by weight, the crosslinking formation by the crosslinking agent becomes insufficient, the cohesive force of the resulting pressure-sensitive adhesive layer becomes small, and sufficient heat resistance may not be obtained, It tends to cause glue residue.
- the pressure-sensitive adhesive composition may further contain a cross-linking catalyst for causing any of the above-described cross-linking reactions to proceed more effectively.
- cross-linking catalysts include tin-based catalysts such as dibutyltin dilaurate and dioctyltin dilaurate, tris (acetylacetonato) iron, tris (hexane-2,4-dionato) iron, tris (heptane-2,4-dionato).
- Iron tris (heptane-3,5-dionato) iron, tris (5-methylhexane-2,4-dionato) iron, tris (octane-2,4-dionato) iron, tris (6-methylheptane-2) , 4-Dionato) iron, tris (2,6-dimethylheptane-3,5-dionato) iron, tris (nonane-2,4-dionato) iron, tris (nonane-4,6-dionato) iron, tris ( 2,2,6,6-tetramethylheptane-3,5-dionato) iron, tris (tridecan-6,8-dionato) iron, tris (1-phenylbutane-1, -Dionato) iron, tris (hexafluoroacetylacetonato) iron, tris (ethyl acetoacetate) iron, tris (acetoacetate-n-propyl) iron, tris (isopropy
- the content of the crosslinking catalyst is not particularly limited, but is preferably about 0.0001 to 1 part by weight, for example, 0.001 to 0.5 parts per 100 parts by weight of the (meth) acrylic polymer. Part by weight is more preferred. Within the above range, when the pressure-sensitive adhesive layer is formed, the speed of the cross-linking reaction is high, and the pot life of the pressure-sensitive adhesive composition is lengthened.
- the pressure-sensitive adhesive composition may contain other known additives, for example, powders such as lubricants, colorants, pigments, plasticizers, tackifiers, low molecular weight polymers, surface lubrication.
- powders such as lubricants, colorants, pigments, plasticizers, tackifiers, low molecular weight polymers, surface lubrication.
- optical surface protective film with separator is formed by forming the pressure-sensitive adhesive layer on at least one surface of a base film, and in that case, the pressure-sensitive adhesive composition is crosslinked. Although it is generally performed after application of the adhesive composition, it is also possible to transfer the adhesive layer comprising the crosslinked adhesive composition to a substrate film or the like.
- the method for forming the pressure-sensitive adhesive layer on the base film is not particularly limited.
- the pressure-sensitive adhesive layer is formed by applying the pressure-sensitive adhesive composition (solution) to the base film and removing the polymerization solvent by drying. It is produced by forming on a base film. Thereafter, curing may be performed for the purpose of adjusting the component transfer of the pressure-sensitive adhesive layer or adjusting the crosslinking reaction.
- the pressure-sensitive adhesive composition contains at least one polymerization solvent other than the polymerization solvent so that the surface protective film can be uniformly applied. A new solvent may be added.
- a known method used for producing pressure-sensitive adhesive tapes is used as a method for forming the pressure-sensitive adhesive layer when producing the surface protective film of the present invention. Specific examples include roll coating, gravure coating, reverse coating, roll brushing, spray coating, air knife coating, extrusion coating using a die coater, and the like.
- the surface protective film of the present invention is usually prepared so that the thickness of the pressure-sensitive adhesive layer is 3 to 100 ⁇ m, preferably about 5 to 50 ⁇ m. It is preferable for the thickness of the pressure-sensitive adhesive layer to be within the above range because it is easy to obtain an appropriate balance between removability and adhesiveness.
- the total thickness of the surface protective film of the present invention is preferably 8 to 300 ⁇ m, more preferably 10 to 200 ⁇ m, and most preferably 20 to 100 ⁇ m. Within the above range, the adhesive properties (removability, adhesiveness, etc.), workability, and appearance properties are excellent and a preferred embodiment is obtained.
- the said total thickness means the sum total of the thickness containing all layers, such as a base film, an adhesive layer, a separator, and another layer.
- the surface protective film of the present invention has a pressure-sensitive adhesive layer on at least one surface of the base film, and has a separator on the surface opposite to the surface in contact with the pressure-sensitive adhesive layer of the base film.
- the separator has a release layer and a base material, and the haze of the separator is 90% or more, and the total light transmittance is 50% or less.
- the separator is to bond the separator to the surface of the pressure-sensitive adhesive layer, and in particular, the separator has optical characteristics such as specific haze and total light transmittance,
- the optical surface protective film with a separator is accurately adjusted on the optical member, and after adjusting the position, the optical surface protective film from which the separator has been peeled off can be stuck (laminated) on the optical member surface, which is a preferred embodiment. .
- the separator has a haze of 90% or more and a total light transmittance of 50% or less (0 to 50%), preferably a haze of 92% or more and a total light transmittance of 5 to 50%, more preferably haze. Is 94% or more and the total light transmittance is 8 to 48%, and more preferably, the haze is 96% or more and the total light transmittance is 10 to 45%.
- the haze of the separator is 90% or more and the total light transmittance is 50% or less, it is excellent in position adjustability with respect to the optical member surface of the optical surface protective film with a separator, and after the position adjustment, the separator is peeled off.
- the total light transmittance is 50% or less (0 to 50%), preferably 48% or less, more preferably 45% or less, and still more preferably 40% or less. Particularly preferably, it is 30% or less. Since the total light transmittance is low, it is easy to adjust the position relative to the surface of the optical member of the optical surface protective film with a separator, which is preferable because of excellent position adjustability and workability.
- paper or plastic film is preferably used as the substrate.
- the film is not particularly limited as long as it can protect the pressure-sensitive adhesive layer.
- polyethylene film, polypropylene film, polybutene film, polybutadiene film, polymethylpentene film, polyvinyl chloride film, vinyl chloride copolymer examples thereof include a coalesced film, a polyethylene terephthalate film, a polyethylene naphthalate film, a polybutylene terephthalate film, a polyurethane film, and an ethylene-vinyl acetate copolymer film.
- PET polyethylene terephthalate
- PET polyethylene terephthalate
- Use of a film, a polybutylene terephthalate film or the like is a preferred embodiment.
- a method for preparing the separator with a haze of 90% or more and a total light transmittance of 50% or less is not particularly limited, and a known method can be used.
- a cavity is provided in a base material constituting the separator.
- a coloring material, roughening the surface of the substrate, or the like include the method described in JP-A-9-12759.
- the thickness of the substrate is usually about 5 to 200 ⁇ m, preferably about 10 to 100 ⁇ m. It is preferable for it to be in the above-mentioned range since it is excellent in the workability for bonding to the pressure-sensitive adhesive layer and the peelability and workability of the separator with respect to the pressure-sensitive adhesive layer.
- the surface of the substrate can be subjected to various surface treatments such as corona discharge treatment or various surface treatments such as embossing as necessary.
- various surface treatments such as corona discharge treatment or various surface treatments such as embossing as necessary.
- fillers inorganic fillers, organic fillers, etc.
- anti-aging agents such as antioxidants, UV absorbers, antistatic agents, lubricants, plasticizers, colorants (pigments, dyes, etc.), etc.
- additives may be blended.
- Examples of commercially available base materials include Diafoil W100, Diafoil W400 (above, manufactured by Mitsubishi Plastics), Lumirror # 50-EA3S (manufactured by Toray Industries, Inc.), CQ952 (manufactured by KOLON), and the like.
- the release layer has adhesiveness to the substrate and has releasability with respect to the pressure-sensitive adhesive layer, and can be formed from a release agent composition.
- a release agent composition for example, long-chain alkyl type compounds, such as silicone compounds, such as a dimethylsiloxane and a diphenylsiloxane, a silicone resin, a fluororesin, an ashioresin, etc. can be used.
- the release agent composition may contain other known additives such as antistatic agents, powders such as colorants, pigments, surfactants, plasticizers, and tackifiers. , Low molecular weight polymers, surface lubricants, leveling agents, antioxidants, corrosion inhibitors, light stabilizers, UV absorbers, polymerization inhibitors, silane coupling agents, inorganic or organic fillers, metal powders, particulates, etc. Can be added as appropriate according to the intended use.
- the separator is formed on the base material using the release agent composition.
- the method for forming the release layer on the substrate is not particularly limited.
- the release agent composition solution is applied to the substrate, and the polymerization solvent is dried and removed to remove the release layer on the substrate. It is produced by forming. Thereafter, curing may be performed for the purpose of adjusting the component transfer of the release layer.
- the release agent composition when the release agent composition is applied onto the substrate to produce a release layer, the release agent composition contains at least one polymerization solvent other than the polymerization solvent so that it can be uniformly applied onto the substrate. A new solvent may be added.
- a known method used for manufacturing the release layer is used. Specific examples include roll coating, gravure coating, reverse coating, roll brushing, spray coating, air knife coating, extrusion coating using a die coater, and the like.
- the thickness of the release layer is typically 1 to 200 nm, preferably 5 to 100 nm, more preferably 10 to 50 nm. When the thickness of the release layer is too small, it is difficult to peel the separator, and therefore, the work of attaching the optical surface protective film may be difficult. On the other hand, if it is too thick, it may affect the contamination of the pressure-sensitive adhesive layer of the optical surface protective film.
- the optical surface protective film with a separator of the present invention has a form in which the pressure-sensitive adhesive layer of the optical surface protective film and the release layer of the separator are bonded together.
- a known method is used for the bonding.
- a laminator manufactured by MC Kay Co., Ltd., MRK-600
- MRK-600 may be used to bond the optical surface protective film and the separator.
- the optical surface protection film which peeled the said separator from the surface of the adhesive layer of the said optical surface protection film with a separator can be stuck on an optical member, and an optical member can be protected. Since the separator is excellent in cushioning properties, dents are hardly generated, and the optical surface protective film is excellent in appearance quality (appearance), so that it can be used for surface protection during processing, transportation, shipping, etc. (surface In order to protect the surface of the optical member (polarizing plate, etc.), it is useful.
- haze was measured using a haze meter (manufactured by Murakami Color Research Laboratory, model HM-150) according to the method defined in JIS K7136 “Plastics—How to determine haze of transparent material”.
- the total light transmittance is measured using a haze meter (manufactured by Murakami Color Research Laboratory, Model HM-150) in accordance with the method specified in JIS K7361 “Plastics-Test method for total light transmittance of transparent materials”. It was.
- Tg glass transition temperature
- Tgn glass transition temperature of the homopolymer of each monomer.
- Formula: 1 / (Tg + 273) ⁇ [Wn / (Tgn + 273)] (Wherein Tg (° C.) is the glass transition temperature of the copolymer, Wn ( ⁇ ) is the weight fraction of each monomer, Tgn (° C.) is the glass transition temperature of the homopolymer of each monomer, and n is the type of each monomer.
- the glass plate of 100 mm ⁇ 110 mm was placed on the other suction plate (hereinafter referred to as suction plate 2).
- the suction plate 1 was rotated and overlapped with the suction plate 2, and the position of the suction plate 2 was adjusted by a CCD camera attached with a precision sheet bonding machine so that the hole of the optical surface protective film with a separator and the glass did not overlap.
- the suction plate 1 is temporarily lifted from the suction plate 2, the separator is peeled off, the suction plate 1 is moved again onto the suction plate 2, and the optical surface protection film is rolled at a pressure of 8 kgf / cm 2.
- the glass surface was bonded at a roll speed of 5 mm / sec. Whether or not automatic bonding is possible (evaluation) is: ⁇ when the surface protective film for optics is automatically and accurately aligned and bonded, and when the position of the optical surface protective film cannot be automatically and accurately aligned Was marked with x.
- the (meth) acrylic polymer (A) solution (35% by weight) is diluted with ethyl acetate to 29% by weight, and 500 parts by weight (100 parts by weight of solid content) of this solution is used as a crosslinking agent with a trifunctional isocyanate compound.
- Isocyanurate of certain hexamethylene diisocyanate (Coronate HX: C / HX, manufactured by Nippon Polyurethane Co., Ltd.) 4 parts by weight (solid content 4 parts by weight), dibutyltin dilaurate as a crosslinking catalyst (“Sn” in Table 2, 1% by weight) Ethyl acetate solution) 1.5 parts by weight (solid content 0.015 parts by weight) was added, and the mixture was stirred at about 25 ° C. for about 1 minute to prepare an acrylic pressure-sensitive adhesive (1) solution.
- the (meth) acrylic polymer (A) solution (35% by weight) is diluted to 29% by weight with ethyl acetate, and an isocyanate crosslinking agent (as a crosslinking agent) is added to 500 parts by weight (100 parts by weight of solid content) of this solution.
- Isocyanurate of hexamethylene diisocyanate (trade name “Coronate HX”: C / HX, manufactured by Nippon Polyurethane) 5 parts by weight (solid content 5 parts by weight), dibutyltin dilaurate (1% by weight ethyl acetate solution) as a crosslinking catalyst 3 Parts by weight (solid content: 0.03 parts by weight), polyoxyalkylene chain-containing compound (Aqualon HS-10, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) not containing the organopolysiloxane additive, 0.3 parts by weight (solid content 0 .3 parts) was added and mixed and stirred to prepare an acrylic pressure-sensitive adhesive (2) solution.
- the (meth) acrylic polymer (B) solution (30% by weight) is diluted with ethyl acetate to 29% by weight, and 500 parts by weight (100 parts by weight of solid content) of this solution is used as a crosslinking agent.
- silicone adhesive “X-40-3229” (solid content 60% by weight, manufactured by Shin-Etsu Chemical Co., Ltd.) is 100 parts by weight in solid content, and as a platinum catalyst, “CAT-PL-50T” (Shin-Etsu Chemical Co., Ltd.). (Product) 0.5 parts by weight and 100 parts by weight of toluene as a solvent were blended to obtain a silicone-based pressure-sensitive adhesive (5) solution.
- This release agent composition was applied to a PET film (manufactured by Mitsubishi Plastics, Diafoil W100) as a substrate having a thickness of 50 ⁇ m, and dried at 130 ° C. for 1 minute to produce separator III.
- the thickness of the release layer after drying was 20 nm.
- 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 on a polyethylene terephthalate (PET) film (thickness: 38 ⁇ m) as a base film using a Mayer bar, and the solvent was removed by drying at 130 ° C. for 1 minute. An antistatic layer (thickness: 0.2 ⁇ m) was formed to produce an antistatic treatment film.
- PET polyethylene terephthalate
- Examples 2 and 3 As shown in Table 2, in place of the acrylic pressure-sensitive adhesive (1) solution used in Example 1, an acrylic pressure-sensitive adhesive (2) solution or an acrylic pressure-sensitive adhesive (3) solution was used except that it was used. In the same manner as in Example 1, an optical surface protective film with a separator was produced.
- Examples 4 and 5 As shown in Table 3 and Table 4, instead of the acrylic adhesive (1) solution used in Example 1, a urethane adhesive (4) solution or a silicone adhesive (5) solution was used. Except for this, an optical surface protective film with a separator was prepared in the same manner as in Example 1 and the heating conditions and the thickness of the resulting pressure-sensitive adhesive layer were adjusted.
- Example 6 to 10 Comparative Examples 1 and 2> As shown in Table 6, an optical surface protective film with a separator was prepared in the same manner as in Example 1, except that separators II to VIII were used instead of separator I used in Example 1.
- Tables 1 to 6 show the above-described blending contents, various measurements, and evaluation results for the optical surface protective films with a separator according to Examples and Comparative Examples.
- surface shows an active ingredient.
- the separator-provided optical surface protective film with a separator is used at the time of production or transportation of an optical member used as a component of a liquid crystal display panel, a plasma display panel (PDP), an organic electroluminescence (EL) display, or the like. It is suitable as a surface protective film for protecting the optical member. In particular, it is useful as an optical surface protective film applied to optical members such as polarizing plates (polarizing films) for liquid crystal display panels, wave plates, retardation plates, optical compensation films, brightness enhancement films, light diffusion sheets, and reflective sheets. It is.
- polarizing plates polarizing films
- Optical surface protective film 3 Optical surface protective film with separator 10: Optical member 11: Base material 12: Release layer 21: Adhesive layer 22: Base material film
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Abstract
Description
ここに開示されるセパレータ付き光学用表面保護フィルム(以下、単に「表面保護フィルム」という場合がある。)は、一般に、粘着テープ、粘着ラベル、粘着フィルム等と称される形態の粘着剤層表面がセパレータにより保護されるものであり、特に光学部品(例えば、偏光板、波長板等の液晶ディスプレイパネル構成要素として用いられる光学部品)の加工、検査、搬送時に光学部品の表面を保護する表面保護フィルムとして好適である。前記表面保護フィルムにおける粘着剤層は、典型的には連続的に形成されるが、かかる形態に限定されるものではなく、例えば点状、ストライプ状等の規則的あるいはランダムなパターンに形成された粘着剤層であってもよい。また、ここに開示される表面保護フィルムは、ロール状であってもよく、枚葉状であってもよい。
本発明のセパレータ付き光学用表面保護フィルムは、基材フィルムを有することを特徴とする。ここに開示される技術において、基材フィルムを構成する樹脂材料は、特に制限なく使用することができるが、例えば、透明性、機械的強度、熱安定性、水分遮蔽性、等方性、可撓性、寸法安定性等の特性に優れたものを使用することが好ましい。特に、基材フィルムが可撓性を有することにより、ロールコーターなどによって粘着剤組成物を塗布することができ、ロール状に巻き取ることができ、有用である。
本発明で用いられる粘着剤層は、粘着性を有する粘着性ポリマーを含有する粘着剤組成物から形成されるものであれば、特に制限なく使用できる。前記粘着剤組成物としては、例えば、アクリル系粘着剤、ウレタン系粘着剤、合成ゴム系粘着剤、天然ゴム系粘着剤、シリコーン系粘着剤、ポリエステル系粘着剤等を使用することができ、中でも、アクリル系粘着剤、ウレタン系粘着剤、及び、シリコーン系粘着剤からなる群より選択される少なくとも1種を使用(含有)するものが好ましく、特に好ましくは、前記粘着性ポリマーである(メタ)アクリル系ポリマーを使用するアクリル系粘着剤を使用することである。
本発明で用いる粘着剤組成物は、オキシアルキレン基含有化合物を含有することも可能である。オキシアルキレン基含有化合物を含有することにより、更に軽剥離性を発現させることが可能である。オキシアルキレン基含有化合物としては、オキシアルキレン鎖を有するオルガノポリシロキサンやオルガノポリシロキサンを含まないオキシアルキレン基含有化合物が挙げられる。
本発明の表面保護フィルムは、前記粘着剤組成物が、架橋剤を含有することが好ましい。また、本発明においては、前記粘着剤組成物を用いて、粘着剤層とすることができる。例えば、前記粘着剤組成物が、前記(メタ)アクリル系ポリマーを含有するアクリル系粘着剤の場合、前記(メタ)アクリル系ポリマーの構成単位、構成比率、架橋剤の選択および添加比率等を適宜調節して架橋することにより、より耐熱性に優れた粘着剤層(表面保護フィルム)を得ることができる。
前記粘着剤組成物には、さらに、上述したいずれかの架橋反応をより効果的に進行させるための架橋触媒を含有させることができる。かかる架橋触媒として、例えば、ジラウリン酸ジブチルスズ、ジラウリン酸ジオクチルスズなどのスズ系触媒、トリス(アセチルアセトナト)鉄、トリス(ヘキサン-2,4-ジオナト)鉄、トリス(ヘプタン-2,4-ジオナト)鉄、トリス(ヘプタン-3,5-ジオナト)鉄、トリス(5-メチルヘキサン-2,4-ジオナト)鉄、トリス(オクタン-2,4-ジオナト)鉄、トリス(6-メチルヘプタン-2,4-ジオナト)鉄、トリス(2,6-ジメチルヘプタン-3,5-ジオナト)鉄、トリス(ノナン-2,4-ジオナト)鉄、トリス(ノナン-4,6-ジオナト)鉄、トリス(2,2,6,6-テトラメチルヘプタン-3,5-ジオナト)鉄、トリス(トリデカン-6,8-ジオナト)鉄、トリス(1-フェニルブタン-1,3-ジオナト)鉄、トリス(ヘキサフルオロアセチルアセトナト)鉄、トリス(アセト酢酸エチル)鉄、トリス(アセト酢酸-n-プロピル)鉄、トリス(アセト酢酸イソプロピル)鉄、トリス(アセト酢酸-n-ブチル)鉄、トリス(アセト酢酸-sec-ブチル)鉄、トリス(アセト酢酸-tert-ブチル)鉄、トリス(プロピオニル酢酸メチル)鉄、トリス(プロピオニル酢酸エチル)鉄、トリス(プロピオニル酢酸-n-プロピル)鉄、トリス(プロピオニル酢酸イソプロピル)鉄、トリス(プロピオニル酢酸-n-ブチル)鉄、トリス(プロピオニル酢酸-sec-ブチル)鉄、トリス(プロピオニル酢酸-tert-ブチル)鉄、トリス(アセト酢酸ベンジル)鉄、トリス(マロン酸ジメチル)鉄、トリス(マロン酸ジエチル)鉄、トリメトキシ鉄、トリエトキシ鉄、トリイソプロポキシ鉄、塩化第二鉄などの鉄系触媒を用いることができる。これら架橋触媒は、1種でもよく、2種以上を併用してもよい。
本発明のセパレータ付き光学用表面保護フィルム(表面保護フィルム)は、前記粘着剤層を基材フィルムの少なくとも片面に形成してなるものであるが、その際、粘着剤組成物の架橋は、粘着剤組成物の塗布後に行うのが一般的であるが、架橋後の粘着剤組成物からなる粘着剤層を基材フィルムなどに転写することも可能である。
本発明の表面保護フィルムは、基材フィルムの少なくとも片面に粘着剤層を有し、前記基材フィルムの粘着剤層と接触する面と反対面に、セパレータを有するものであって、前記セパレータが、離型層と基材を有し、前記セパレータのヘイズが、90%以上、全光線透過率が、50%以下であることを特徴とする。前記セパレータは、粘着剤層の粘着面を保護する目的で、粘着剤層表面にセパレータを貼り合わせるものであり、特にセパレータが特定のヘイズや全光線透過率のような光学特性を有することで、セパレータ付き光学用表面保護フィルムを光学部材上に、正確に位置調整し、位置調整後、セパレータを剥離した光学用表面保護フィルムを光学部材表面に貼付(積層)することができ、好ましい態様となる。
前記基材としては、紙やプラスチックフィルムが好適に用いられる。そのフィルムとしては、前記粘着剤層を保護し得るフィルムであれば特に限定されず、たとえば、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、ポリ塩化ビニルフィルム、塩化ビニル共重合体フィルム、ポリエチレンテレフタレートフィルム、ポリエチレンナ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などが挙げられ、特に、ポリエステル系フィルムであるポリエチレンテレフタレート(PET)フィルム、ポリエチレンナ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などの使用が好ましい態様である。
前記離型層は、前記基材に密着性を有し、かつ前記粘着剤層に対して剥離性を有し、離型剤組成物から形成することができる。前記離型剤組成物としては、特に制限されないが、例えば、ジメチルシロキサンやジフェニルシロキサン等のシリコーン化合物、シリコーン樹脂、フッ素樹脂、アシオレジン等の長鎖アルキル系化合物などを用いることができる。
前記セパレータは、前記基材上に、前記離型剤組成物を用いて形成してなるものである。
本発明のセパレータ付き光学用表面保護フィルムは、光学用表面保護フィルムの粘着剤層と、セパレータの離型層とを貼り合わせてなる形態である。貼り合わせは、公知の方法が用いられるが、例えば、ラミネータ―(エム・シー・ケイ(株)社製、MRK-600)を用い、光学用表面保護フィルムとセパレータを貼り合せる方式が挙げられる。
本発明において、前記セパレータ付き光学用表面保護フィルムの粘着剤層の表面から前記セパレータを剥離した光学用表面保護フィルムを光学部材に貼付し、光学部材を保護することができる。前記セパレータは、クッション性に優れるため、打痕が発生しにくく、また、前記光学用表面保護フィルムは、外観品位(外観性)に優れるため、加工、搬送、出荷時等の表面保護用途(表面保護フィルム)に使用できるため、前記光学部材(偏光板など)の表面を保護するために、有用なものとなる。
ヘイズ(ヘーズ)の測定は、JIS K7136「プラスチック-透明材料のヘーズの求め方」に規定の方法に準じ、ヘーズメーター(村上色彩技術研究所製、HM-150型)を用いて行った。
全光線透過率の測定は、JIS K7361「プラスチック-透明材料の全光線透過率の試験方法」に規定の方法に準じ、ヘーズメーター(村上色彩技術研究所製、HM-150型)を用いて行った。
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:1/(Tg+273)=Σ[Wn/(Tgn+273)]
(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。)
文献値:
2-エチルヘキシルアクリレート(2EHA):-70℃
ブチルアクリレート(BA):-55℃
2-ヒドロキシエチルアクリレート(HEA):-15℃
アクリル酸(AA):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。
使用する(メタ)アクリル系ポリマーの重量平均分子量(Mw)は、東ソー株式会社製GPC装置(HLC-8220GPC)を用いて測定を行った。測定条件は下記の通りである。
サンプル濃度:0.2重量%(THF溶液)
サンプル注入量:10μl
溶離液:THF
流速:0.6ml/min
測定温度:40℃
カラム:
サンプルカラム;TSKguardcolumn SuperHZ-H(1本)+TSKgel SuperHZM-H(2本)
リファレンスカラム;TSKgel SuperH-RC(1本)
検出器:示差屈折計(RI)
なお、重量平均分子量はポリスチレン換算値にて求めた。また、数平均分子量(Mn)を測定する際も、重量平均分子量(Mw)と同様に測定した。
セパレータ付き光学用表面保護フィルムのセパレータを切断しないように、表面保護フィルムのみを100mm×110mmにカットした。続いて、カットした表面保護フィルム四隅のそれぞれの角に接するように、セパレータに直径5mmの穴を空けた。
精密枚葉貼合機(クライムプロダクツ(株)社製、SE650naa)の一方の吸着板(以下、吸着板1と表記)に、上記方法により、穴を空けたセパレータ付き光学用表面保護フィルムをセパレータ側が上になるように設置し、もう一方の吸着板(以下、吸着板2と表記)に、100mm×110mmのガラスを設置した。吸着板1を回転させ吸着板2に重ね、精密枚葉貼合機付帯のCCDカメラにより、セパレータ付き光学用表面保護フィルムの穴とガラスが重ならないように、吸着板2の位置を調整した。位置調整後(図2参照)、吸着板2から吸着板1を一旦浮かし、セパレータを剥離し、再び吸着板1を吸着板2上に移動させ、光学用表面保護フィルムをロール圧力8kgf/cm2、ロール速度5mm/秒にてガラス表面に貼り合せた。
自動貼り合せの可否(評価)は、光学用表面保護フィルムを自動で正確に位置調整し、貼り合せることができた場合を○、光学用表面保護フィルムを自動で正確に位置調整できなかった場合を×とした。
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた四つロフラスコに、2-エチルヘキシルアクリレート(2EHA)100重量部、2-ヒドロキシエチルアクリレート(HEA)4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(AIBN)0.2重量部、酢酸エチル205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63℃付近に保って約4時間重合反応を行い、(メタ)アクリル系ポリマー(A)溶液(約35重量%)を調製した。前記(メタ)アクリル系ポリマー(A)の重量平均分子量(Mw)は65万であり、ガラス転移温度(Tg)は-68℃であった。
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた四つ口フラスコに、ブチルアクリレート(BA)95重量部、アクリル酸(AA)5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0.1重量部、酢酸エチル234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、(メタ)アクリル系ポリマー(B)溶液(30重量%)を調製した。前記(メタ)アクリル系ポリマー(B)の重量平均分子量(Mw)は、110万であり、ガラス転移温度(Tg)は、-47℃であった。
上記(メタ)アクリル系ポリマー(A)溶液(35重量%)を酢酸エチルで29重量%に希釈し、この溶液500重量部(固形分100重量部)に、架橋剤として、3官能イソシアネート化合物である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(コロネートHX:C/HX、日本ポリウレタン社製)4重量部(固形分4重量部)、架橋触媒としてジラウリン酸ジブチルスズ(表2中の「Sn」、1重量%酢酸エチル溶液)1.5重量部(固形分0.015重量部)を加えて、25℃付近に保って約1分間混合攪拌を行い、アクリル系粘着剤(1)溶液を調製した。
上記(メタ)アクリル系ポリマー(A)溶液(35重量%)を酢酸エチルで29重量%に希釈し、この溶液500重量部(固形分100重量部)に、架橋剤として、イソシアネート系架橋剤(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(商品名「コロネートHX」:C/HX、日本ポリウレタン社製)5重量部(固形分5重量部)、架橋触媒としてジラウリン酸ジブチルスズ(1重量%酢酸エチル溶液)3重量部(固形分0.03重量部)、添加剤であるオルガノポリシロキサンを含まないポリオキシアルキレン鎖含有化合物(アクアロンHS-10、第一工業製薬社製)0.3重量部(固形分0.3量部)を加えて、混合攪拌を行い、アクリル系粘着剤(2)溶液を調製した。
上記(メタ)アクリル系ポリマー(B)溶液(30重量%)を酢酸エチルで29重量%に希釈し、この溶液500重量部(固形分100重量部)に、架橋剤として、エポキシ系架橋剤(1,3-ビス(N,N-ジグリシジルアミノメチル)シクロヘキサン、エポキシ当量:110、官能基数:4、商品名「TETRAD-C」:T/C、三菱ガス化学社製)6重量部(固形分6重量部)を加えて、混合攪拌を行い、アクリル系粘着剤(3)溶液を調製した。
ポリオールとして、ヒドロキシル基を3個有するポリオールであるプレミノールS3011(旭硝子社製、Mn=10000)85重量部、ヒドロキシル基を3個有するポリオールであるサンニックスGP3000(三洋化成社製、Mn=3000)13重量部、ヒドロキシル基を3個有するポリオールであるサンニックスGP1000(三洋化成社製、Mn=1000)2重量部、架橋剤として、3官能イソシアネート化合物である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(コロネートHX:C/HX、日本ポリウレタン社製)18重量部、触媒として、鉄(III)アセチルアセトナート (トリス(アセチルアセトナト)鉄、表3中の「Fe」、東京化成工業社製)0.04重量部、濡れ性向上剤として、ミルスチン酸イソプロピル(エキセパールIPM、花王社製)30重量部、酸化防止剤としてIrganox1010(BASF社製)0.5重量部、希釈溶剤として酢酸エチル210重量部を配合し、ウレタン系粘着剤(4)溶液を得た。
シリコーン系粘着剤として、「X-40-3229](固形分60重量%、信越化学工業社製)を固形分で100重量部、白金触媒として、「CAT-PL-50T」(信越化学工業社製)0.5重量部、溶剤としてトルエン100重量部を配合して、シリコーン系粘着剤(5)溶液を得た。
表5に示すように、基材(PETフィルム)に離型層が設けられた離型層付き基材をセパレータとした市販品を使用した。
シリコーン離型剤(信越化学工業製、KS-847H)を100重量部、シリコーン硬化触媒(信越化学工業製、CAT-PL-50T)を3.3重量部入れ、トルエン(出光石油化学製)、ヘキサン(丸善石油化学製、ノルマルヘキサン)、メチルエチルケトン(出光興産製、MEK)が1:2:1の重量比でなる溶剤で0.3重量%に希釈し、離型剤組成物を得た。この離型剤組成物を厚み50μmの基材であるPETフィルム(三菱樹脂製、ダイアホイルW100)に塗布し、130℃で1分間乾燥させ、セパレータIIIを作製した。離型層の乾燥後の厚みは20nmであった。
表5に示すように、セパレータIIIで用いたPETフィルムの代わりに、表5に記載の商品名のPETフィルムを使用したこと以外は、セパレータIIIの作製と同様の方法で作製した。
〔帯電防止処理フィルムの作製〕
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。
得られた帯電防止剤溶液を、基材フィルムであるポリエチレンテレフタレート(PET)フィルム(厚さ:38μm)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、帯電防止処理フィルムを作製した。
上記アクリル系粘着剤(1)溶液を、上記の帯電防止処理フィルムの帯電防止処理面とは反対の面に塗布し、130℃で2分間加熱して、厚さ15μm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セパレータであるポリエチレンテレフタレートフィルム(東洋紡社製、商品名:クリスパー K7211-38μm、ヘイズ:99.3%、全光線透過率:13.6%、厚さ50μm)のシリコーン処理面を、貼り合わせ、セパレータ付光学用表面保護フィルムを作製した。
表2に示すように、実施例1で用いたアクリル系粘着剤(1)溶液の代わりに、アクリル系粘着剤(2)溶液又はアクリル系粘着剤(3)溶液を使用したこと以外は、実施例1と同様の方法で、セパレータ付光学用表面保護フィルムを作製した。
表3及び表4に示すように、実施例1で用いたアクリル系粘着剤(1)溶液の代わりに、ウレタン系粘着剤(4)溶液、又は、シリコーン系粘着剤(5)溶液を使用したこと以外は、実施例1と同様の方法で、加熱条件等や得られる粘着剤層の厚みを調整したセパレータ付光学用表面保護フィルムを作製した。
表6に示すように、実施例1で用いたセパレータIの代わりに、セパレータII~VIIIを使用したこと以外は、実施例1と同様の方法で、セパレータ付光学用表面保護フィルムを作製した。
2 :光学用表面保護フィルム
3 :セパレータ付き光学用表面保護フィルム
10:光学部材
11:基材
12:離型層
21:粘着剤層
22:基材フィルム
Claims (3)
- 基材フィルムの少なくとも片面に粘着剤層を有する光学用表面保護フィルム、及び、前記基材フィルムの粘着剤層と接触する面と反対面に、セパレータを有するセパレータ付き光学用表面保護フィルムであって、
前記セパレータが、離型層と基材を有し、
前記セパレータのヘイズが、90%以上、全光線透過率が、50%以下であることを特徴とするセパレータ付き光学用表面保護フィルム。 - 前記基材フィルムが、ポリエステルフィルムであることを特徴とする請求項1に記載のセパレータ付き光学用表面保護フィルム。
- 前記粘着剤層が、アクリル系粘着剤、ウレタン系粘着剤、及び、シリコーン系粘着剤から選択される少なくとも1種を含有する粘着剤組成物から形成されることを特徴とする請求項1又は2に記載のセパレータ付き光学用表面保護フィルム。
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