WO2008059925A1 - Gas barrier film laminate - Google Patents
Gas barrier film laminate Download PDFInfo
- Publication number
- WO2008059925A1 WO2008059925A1 PCT/JP2007/072192 JP2007072192W WO2008059925A1 WO 2008059925 A1 WO2008059925 A1 WO 2008059925A1 JP 2007072192 W JP2007072192 W JP 2007072192W WO 2008059925 A1 WO2008059925 A1 WO 2008059925A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- gas barrier
- barrier film
- layer
- resin
- film laminate
- Prior art date
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
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- 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
- Y10T428/31—Surface property or characteristic of web, sheet or block
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- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31507—Of polycarbonate
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- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31511—Of epoxy ether
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- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
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- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31721—Of polyimide
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- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31786—Of polyester [e.g., alkyd, etc.]
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- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
Definitions
- the present invention relates to a film laminate excellent in gas barrier properties, appearance, and adhesion between layers.
- each of a transparent resin layer / an oxide thin film layer / a hygroscopic resin layer for the purpose of improving water vapor barrier properties.
- Two or more resin layers are laminated for the purpose of improving heat resistance and gas barrier properties, and an organic / inorganic hybrid layer obtained by a sol-gel method is used between layers.
- an organic / inorganic hybrid layer obtained by a sol-gel method is used between layers.
- Patent Document 3 discloses a film in which the influence of moisture is suppressed and foam whitening and bubble mixing are eliminated by paying attention to the adhesive composition.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2003-249349
- Patent Document 2 Japanese Patent Application Laid-Open No. 2004-136466
- Patent Document 3 Japanese Unexamined Patent Publication No. 2006-51751
- the present invention relates to a gas barrier film laminate that remarkably reduces the generation of bubbles and foreign substances between gas barrier film layers, and is excellent in gas noirality and interlayer adhesion. Means for solving the problem
- the present invention provides:
- a gas film laminate having at least two gas barrier film layers laminated via an adhesive layer, the gas barrier film layer, the base film, and at least one surface of the base film And at least one structural unit layer composed of an inorganic thin film layer, and a bubble having a diameter of 0.5 mm or more and a diameter of 0.5 mm or more present between the gas barrier film layers.
- a gas barrier film laminate excellent in gas barrier properties and interlayer adhesion can be obtained while significantly reducing the generation of bubbles and foreign substances between gas barrier film layers.
- the gas barrier film laminate of the present invention is a gas barrier film laminate having at least two gas barrier film layers laminated via an adhesive layer, the gas barrier film laminating force S, the substrate film, and the substrate A bubble having a diameter of 0.5 mm or more and a diameter of at least one structural unit layer comprising an anchor coat layer and an inorganic thin film layer sequentially formed on at least one surface of the film.
- the number of foreign materials of 0.5 mm or more is 3 or less in total per 100 cm 2 .
- the gas NORA film laminate of the present invention is obtained by laminating at least two gas barrier film layers with an adhesive layer interposed therebetween.
- the method for applying the adhesive layer either a method of applying an adhesive on the gas barrier film layer surface or a method of laminating an adhesive film between the gas barrier films can be used.
- thermosetting adhesive an energy ray curable adhesive, or the like can be used.
- thermosetting adhesive examples include polyester resins, urethane resins, acrylate resins, ether resins, phenol resins, furan resins, urea resins, melamine resins, and epoxy resins.
- energy ray curable adhesive examples include urethane resins and polyester resins. Of the above, at least one selected from urethane resins, epoxy resins, polyester resins, and acrylic resins is preferable. Further, from the viewpoint of reducing the generation of bubbles, an epoxy resin or an epoxy resin that is preferable to an acrylic resin is more preferable.
- the adhesive composition include, for example, a urethane (meth) acrylate component, an epoxy (meth) acrylate component, an alicyclic (meth) acrylate component, and as necessary. And a polymerization initiator.
- the adhesive is not limited to thermosetting resins.
- thermoplastic resin such as polyetheramide imide.
- the above adhesive resins can be used alone, but two or more types can be used in combination.
- the adhesive layer which moisture permeability of 40 ° C, 90% RH in the thickness 1 mu m in terms in terms of improving the gas barrier property of the inorganic thin film is less than 1000g / m 2 / 24hr is preferred. More preferably not more than 300g / m 2 / 24hr.
- the oxygen permeability of the adhesive layer is, in 25 ° C, 90% RH, preferably not more than 1000ml / m 2 / 24hr / MPa , more preferably 500ml / m 2 / 24hr / MPa or less, still more preferably not more than 100ml / m 2 / 24hr / MPa .
- the water vapor permeability of the gas barrier film layer is, 40 ° C, and at at 90% RH conditions 0. 2g / m 2 / 24hr or less, and the oxygen of the adhesive layer
- the transmittance is preferably in the above range.
- the adhesive layer has a large number of aromatic rings such as a meta-xylene diamine skeleton, a noraxylene diamine skeleton, and a bisphenol skeleton, so that the adhesive layer can have gas nooriety. It is preferable to use an adhesive. Furthermore, it is preferable to use an epoxy resin as an adhesive from the viewpoint of suppressing the generation of bubbles after the formation of the gas barrier film laminate.
- Examples of epoxy resins that have gas barrier properties and suppress the generation of bubbles! / are examples of epoxy resins having a glycidylamine moiety from which metaxylylenediamine is also derived, 1 , 3-bis (aminomethyl) cyclohexane-derived epoxy resin with glycidylamine moiety, diaminodiphenylmethane force-induced epoxy resin with glycidylamine moiety, para-aminophenol-derived glycidyl An epoxy resin having a amide moiety, an epoxy resin having a glycidyl ether moiety induced by bisphenol A force, an epoxy resin having a glycidyl ether moiety induced by bisphenol F force, and a glycidyl ether moiety derived from phenol nopolac.
- the above epoxy resin is preferably contained in an adhesive layer in an amount of 50% by mass or more. 100% by mass.
- the epoxy resin curing agent is preferably the following reaction product (A) and (B), reaction product (A) and (C), or (A ), (B) and (C). These may be used alone or in combination of two or more.
- (B) A polyfunctional compound having at least one acyl group that can form an amide group site by reaction with a polyamine to form an oligomer.
- metaxylylenediamine or paraxylylenediamine a modification reaction product with an epoxy resin or a monoglycidyl compound using these as a raw material, a modification reaction with an alkylene oxide having 2 to 4 carbon atoms.
- Products, addition reaction products with epichlorohydrin reaction with polyfunctional compounds having at least one acyl group that can form an amide group site by reaction with these polyamines.
- reaction products are examples of reaction products.
- an aqueous adhesive an anionic aqueous polyurethane emulsion mainly composed of a polyolefin polyol obtained by reacting a polyolefin polyol and a polyisocyanate as a main skeleton, and amines as other components. And a water-soluble high-boiling organic solvent can also be used.
- a water-based adhesive is effective for bonding a polyolefin resin material or a polyester resin material.
- the above water-based adhesive is effective for bonding a polyolefin resin material or a polyester resin material.
- Polyether polyurethane emulsion Polyether polyurethane emulsion, polyester polyurethane emulsion, Polycarbonate-based polyurethane emulsion, polyacrylate ester emulsion, ethylene, selected from aqueous plastic emulsions such as butyl acetate copolymer emulsion, styrene butadiene copolymer emulsion, polyacetate emulsion emulsion, etc.
- aqueous plastic emulsions such as butyl acetate copolymer emulsion, styrene butadiene copolymer emulsion, polyacetate emulsion emulsion, etc.
- aqueous plastic emulsions such as butyl acetate copolymer emulsion, styrene butadiene copolymer emulsion, polyacetate emulsion emulsion, etc.
- One kind or two or more kinds may
- the viscosity of the adhesive layer is adjusted not only by the resin composition of the adhesive composition, but also by adjusting the amount of residual solvent depending on the time each time the adhesive varnish is applied, or in the case of a thermosetting resin.
- the curing state can be controlled and adjusted.
- a gas barrier laminate with a good appearance can be obtained with a thickness of 01 m or less.
- it is prepared by adding inorganic particles such as crystalline silica, amorphous silica, aluminum hydroxide, alumina, aluminum nitride, boron nitride, and antimony trioxide, and organic particles such as silicone powder. It is possible.
- the inorganic particles and the organic particles may be used alone or in combination of two or more.
- silica particles are preferably used from the viewpoint of versatility and stability.
- the average particle diameter of inorganic particles or organic particles is preferably (m. ⁇ — ⁇ , ⁇ , more preferably (m. 01—20 ⁇ 111, more ⁇ is preferable (between 0.05 and 10).
- the content of inorganic particles and / or organic particles in the adhesive is 0.0; More preferably, it is 0.05 to 10% by mass.
- the adhesive may optionally contain additives such as a curing accelerator, a coupling agent, an inorganic ion adsorbent, a polymerization initiator, a tackifier, and a wetting agent.
- additives such as a curing accelerator, a coupling agent, an inorganic ion adsorbent, a polymerization initiator, a tackifier, and a wetting agent.
- the thickness of the adhesive layer made of an adhesive is preferably from 0.2 to 30 111, more preferably from 0.5 to 10 in terms of adhesive strength and workability.
- the thickness is preferably 1 to 100 ⁇ m from the viewpoint of additivity. More preferably, it is ⁇ 111. If a base film is used, its thickness is 3 ⁇ m from the viewpoint of barrier properties. m or more, preferably 5 to 100 m, preferably 6 to 160 m, more preferably about 10 to 100 111, with an adhesive layer formed on both sides of the base film. At this time, the thicknesses of the adhesive layers on both sides of the base film may be the same or different.
- the adhesive film should be stored when measured using a dynamic viscoelasticity measuring device that preferably has a low elastic modulus in order to reduce the thermal stress resulting from the difference in thermal expansion coefficient of the gas barrier film. It is preferable that the elastic modulus is 10 to 2000 MPa at 25 ° C and 3 to 50 MPa at 260 ° C! /.
- an epoxy resin for example, an epoxy resin, an acrylic resin, an epoxy group-containing acrylic copolymer, a phenol resin, an epoxy resin curing agent, and a semi-cured epoxy comprising an epoxy resin curing agent
- an epoxy resin for example, an acrylic resin, an epoxy group-containing acrylic copolymer, a phenol resin, an epoxy resin curing agent, and a semi-cured epoxy comprising an epoxy resin curing agent
- examples thereof include at least one selected from thermosetting resins.
- the surface roughness Rms of the adhesive layer or the adhesive film is preferably 0.05 to 40 m in order to improve the deaeration of bubbles generated between the films during curing. More preferably, it is preferably from 10 to 20 to 111, more preferably from 0.2 to 20 to 111.
- the value of the surface roughness Rms can be achieved by methods such as addition of inorganic particles or organic particles, mixing of two or more types of resins, mechanical unevenness processing, etc. Monkey.
- the gas barrier film laminate at least two, preferably at least three gas barrier film layers may be laminated.
- the inorganic thin film constituting the gas barrier film layer may be used.
- the adhesive layer is preferably provided on the protective layer surface and laminated, and the base material surface of the laminated gas noirfil layer is laminated together. More preferably.
- the gas barrier film laminate of the present invention does not contain any bubbles and / or foreign matters having a maximum diameter of 0.5 mm or more between gas barrier film layers, or contains 3 or less per 100 cm 2 .
- the diameter of bubbles or foreign objects can be measured with a method such as a microscope.
- a foreign material means resin powder, metal powder, etc. here, for example.
- the size of the bubble is obtained as a diameter.
- the number of such bubbles and foreign matters is determined by the gas barrier film lamination. 3 or less force per 100 cm 2 of body
- the number is preferably 2 or less, more preferably 1 or less, and even more preferably 0.1 or less.
- the number of bubbles and foreign matters is preferably 2 or less per 100 cm 2 of the gas barrier film laminate.
- between gas barrier film layers refers to the total number of bubbles and foreign substances existing in all the plurality of layers formed by the plurality of gas barrier film layers.
- the methods (a), (d) and (e) are as described above.
- the above (b) lamination in a vacuum atmosphere is preferably performed under a vacuum atmosphere of 200 Pa or less, more preferably 20 Pa or less, and even more preferably 10 Pa or less in order to suppress the generation of bubbles between gas barrier films. It is preferable to carry out by irradiating energy rays.
- the heating in the above methods (a) and (b) is preferably performed at a temperature of 30 to 250 ° C, more preferably 50 from the viewpoint of suppressing the generation of bubbles between the gas barrier film layers. ⁇ 200 ° C, more preferably 80 ⁇ ; 180 ° C.
- the heating is preferably performed under pressure from the viewpoint of adhesiveness.
- the applied pressure is preferably carried out at a surface pressure l ⁇ 50kgf / cm 2, more preferably surface pressure 5 ⁇ 25kgf / cm 2, further preferably a surface pressure of 1 0 ⁇ 20kgf / cm 2.
- the heating / pressurizing means is not particularly limited. For example, it is sealed! /, N!
- the above composition is placed in a mold and the metal plate of the mold is heated from the outside.
- Indirect heating for example, a heater is adhered to the outer surface of the metal plate and heated, or a flow path of a heat medium is provided on the metal plate. It is provided and heated by steam, heating oil, etc. in a jacket system.
- An example is a method in which the mold is pressurized at a predetermined pressure and then cooled to obtain a gas barrier film laminate.
- Examples of energy rays include active energy rays such as visible light, ultraviolet rays, electron beams, and radiation. Among these, ultraviolet rays, electrons, and the like from the viewpoint of efficiently suppressing the generation of bubbles between the gas-nore film layers. Lines are preferred.
- active energy rays such as visible light, ultraviolet rays, electron beams, and radiation.
- ultraviolet rays, electrons, and the like from the viewpoint of efficiently suppressing the generation of bubbles between the gas-nore film layers. Lines are preferred.
- various light emitting characteristics such as low-pressure mercury lamps, high-pressure mercury lamps, xenon lamps, etc. can be used without any particular restrictions, depending on film thickness, curing conditions, etc. Can be adjusted.
- the irradiation energy of ultraviolet rays preferably the 100 ⁇ 5000mj / cm 2 instrument particularly 1000 ⁇ 3000mj / cm 2 is preferred. If the irradiation energy is within the above range, the resin layer is sufficiently cured, and it is also
- a method of curing by irradiating an electron beam as an active energy ray is preferable because a photoinitiator is unnecessary.
- the absorbed dose of the electron beam is preferably in the range of! ⁇ 200kGy, because the curing of the resin layer is sufficiently advanced. Particularly preferred is 5 ⁇ ; in the range of! OOkGy, the curing proceeds sufficiently. Further, it is more preferable because it hardly damages the plastic film or the resin layer. If the absorbed dose is within the above range, the resin layer is sufficiently cured, and the gas nooriety that damages the plastic film and the resin layer is not impaired.
- a force that can be used as a force S A force that can damage the plastic film or resin layer of the electron beam Acceleration voltage is lkV to 200kV It is preferable to irradiate the electron beam. If the acceleration voltage of the electron beam is within the above range, the curing depth is sufficient, and the mechanical properties of the obtained gas-noria film laminate substrate are not deteriorated. In addition, since the resin layer is formed by irradiating an electron beam with a low acceleration voltage of 10 kV or less, particularly 50 kV or less, it is possible to suppress a decrease in mechanical strength of the base material for the gas barrier final laminate. preferable.
- the gas barrier film layer forming the gas barrier film laminate of the present invention comprises at least one layer of a base film and a structural unit layer formed on the base film.
- a shrinkage ratio of 150 ° C. is 0.0; a plastic film having a shrinkage ratio of 0.0 to 5% is preferable. preferable.
- the shrinkage rate can be measured by a dimensional change before and after heating with a hot air oven.
- the raw material for the base film can be used without any particular limitation as long as it is a resin that can be used for ordinary packaging materials.
- polyolefins such as homopolymers or copolymers of ethylene, propylene, butene, etc.
- amorphous polyolefins such as cyclic polyolefins
- polyesters such as polyethylene terephthalate, polyethylene 2, 6 naphthalate, nylon 6, nylon 66 , Nylon 12, copolymer nylon and other polyamides, polybutyl alcohol, ethylene acetate butyl copolymer partial hydrolyzate (EVOH), polyimide, polyether terimide, polysulfone, polyethersulfone, polyetheretherketone, polycarbonate , Polymetatalylate, polybutylbutyral, polyarylate, fluororesin, acrylate resin, biodegradable resin and the like.
- polyolefins such as homopolymers or copolymers of ethylene,
- polyester resin polycarbonate resin, polymethacrylic resin, polyetherimide resin, polyethersulfone, and cyclic olefinic resin are preferable from the viewpoint of film strength and cost.
- the base film is a known additive such as an antistatic agent, a light blocking agent, an ultraviolet absorber, a plasticizer, a lubricant, a filler, a colorant, a stabilizer, a lubricant, a crosslinking agent, an antiblocking agent, An antioxidant etc. can be contained.
- the plastic film as the substrate film is formed by using the above-mentioned raw materials, but when used as a substrate, it may be unstretched or stretched. Also good. Moreover, you may laminate
- a base film can be produced by a conventionally known method. For example, a raw material resin is melted by an extruder, extruded by an annular die or a T die, and rapidly cooled to be substantially amorphous. A non-oriented unstretched film can be produced.
- the unstretched film is subjected to known methods such as uniaxial stretching, tenter sequential biaxial stretching, tenter simultaneous biaxial stretching, and tubular simultaneous biaxial stretching in the direction of film flow (vertical axis) or the direction of film flow. And by stretching in the direction perpendicular to it (horizontal axis), it is possible to manufacture a film stretched in at least uniaxial direction.
- the thickness of the base film is usually 5 to 500 depending on its use from the viewpoint of mechanical strength, flexibility, transparency, etc. as the base material of the gas barrier film laminate of the present invention.
- m preferably in the range of 10 to 200 111, including a sheet having a large thickness.
- the structural unit layer constituting the gas barrier film layer is composed of an anchor coat layer and an inorganic thin film.
- the anchor coat layer constituting the structural unit layer at least one layer selected from resins such as thermosetting resins and thermoplastic resins, metals, metal oxides, and metal nitrides should be used.
- Power S can be.
- both a solvent-soluble resin and a water-based resin can be used.
- the resin containing, epoxy resin, oxazoline group-containing resin, modified styrene resin, modified silicon resin, alkyl titanate, etc. can be used alone or in combination of two or more.
- polyester-based resins from the viewpoint of gas barrier properties, polyester-based resins, urethane-based resins, acrylic resins, isocyanate group-containing resins, oxazoline group-containing resins, carpositimide-based resins, alcoholic hydroxyl group-containing resins and at least two of them. It is preferable to use at least one resin selected from the group consisting of copolymers of seed resins. Of these, polyester resins are preferred.
- the polyester resin used for the anchor coat layer can be obtained by reacting a polyvalent carboxylic acid component with a polyhydric alcohol component.
- a polyvalent carboxylic acid component examples include terephthalic acid, isophthalic acid, adipic acid, sebacic acid, azelaic acid, taltophthalic acid, diphenylcarboxylic acid, and dimethylphthalic acid.
- the molecular weight of the resin constituting the anchor coat layer is from the viewpoint of gas barrier properties and adhesion.
- the number average molecular weight is 3,000 to 30,000, preferably ⁇ 4,000 to 28,000, and more preferably ⁇ 5,000 to 25,000.
- silane coupling agent it is preferable to add a silane coupling agent to the anchor coat layer from the viewpoint of improving adhesion between the layers.
- silane coupling agents include / 3-(3, 4-epoxy
- Ring agent 7-Aminopropyltrimethoxysilane, N- ⁇ (aminoethyl) ⁇ —Aminopropylmethyl jetoxylan, ⁇ - ⁇ (aminoethyl) ⁇ —Aminopropyltrimethoxylane, ⁇ - ⁇ (aminoethyl)
- amino group-containing silane coupling agents such as ⁇ -aminopropyltriethoxylane, and mixtures thereof. From the viewpoint of adhesion between layers, preferable
- silane coupling agents may be used alone or in combination of two or more. From the viewpoint of adhesion, the silane coupling agent is preferably contained in an amount of 0.;! To 80% by mass, and more preferably 1 to 50% by mass with respect to the resin forming the anchor coat layer.
- polyisocyanate as a curing agent that preferably contains a curing agent in the anchor coat layer.
- aliphatic polyisocyanates such as hexamethylene diisocyanate and dicyclohexylmethane diisocyanate, xylene diisocyanate, tolylene diisocyanate, diphenylenemethane diisocyanate, polymethylene polyphene.
- aromatic polyisocyanates such as dirange isocyanate, tolidine diisocyanate, and naphthalene diisocyanate.
- polyisocyanates having two or more functions are preferred from the viewpoint of improving barrier properties.
- the anchor coat layer may contain various known additives as required.
- additives include polyhydric alcohols such as glycerin, ethylene glycol, polyethylene glycol, and polypropylene glycol, aqueous epoxy resins, lower alcohols such as methanol, ethanol, normal propanol, and isopropanol, and ethylene glycol monomono thio enoate.
- polyhydric alcohols such as glycerin, ethylene glycol, polyethylene glycol, and polypropylene glycol
- aqueous epoxy resins such as methanol, ethanol, normal propanol, and isopropanol
- lower alcohols such as methanol, ethanol, normal propanol, and isopropanol
- ethylene glycol monomono thio enoate such as ethylene glycol monomono thio enoate.
- Propylene Glycole Monomethinoatenore Propylene Glycoleo Lechinino Retein
- Etherenoles such as glyconolemonochinenoeteenore, esters such as propylene glycolenole monoacetate and ethylene glycol monoacetate, antioxidants, weathering stabilizers, ultraviolet absorbers, antistatic agents, pigments, dyes, antibacterials Examples include agents, lubricants, inorganic fillers, antiblocking agents, and adhesives.
- chromium, ano-remium, silicon, Eckenole, titanium, tin, iron, molybdenum, or an alloy of two or more of these is preferable.
- the metal oxide or metal nitride the above metal oxides and nitrides are preferable from the viewpoint of gas barrier properties and adhesion.
- the anchor coat layer from the above viewpoint, at least one selected from chromium, silicon oxide, aluminum oxide, titanium oxide, silicon nitride, aluminum nitride, and titanium nitride is used. More preferably, at least one of silicon oxide and silicon nitride is more preferable. It is also preferable to use a hydrocarbon-based substance such as diamond-like carbon as the anchor coat layer.
- the thickness of the anchor coat layer is 0.
- This anchor coat layer can be subjected to a crosslinking treatment by irradiation with energy rays in order to improve water resistance and durability.
- a method for forming the anchor coat layer a known coating method is appropriately adopted. For example, any method such as reverse roll coater, gravure coater, rod coater, air doctor coater, spray or brush coating method can be used. Moreover, you may immerse a base film and a vapor deposition film in a resin liquid.
- the solvent can be evaporated using a known drying method such as heat drying such as hot air drying or hot roll drying at a temperature of about 80 to 200 ° C. or infrared drying. Thereby, a laminated film having a uniform coating layer is obtained.
- heat drying such as hot air drying or hot roll drying at a temperature of about 80 to 200 ° C. or infrared drying.
- PVD physical vapor deposition
- ion plating ion plating
- sputtering a method of forming an anchor coat layer made of at least one selected from metals, metal oxides, and metal nitrides.
- the strength S that can be used for any method such as CVD (Chemical Vapor Deposition), coating method, etc.
- the vapor deposition method is preferable.
- any method similar to the method that can be used for forming the inorganic thin film described later can be used.
- the base film may be subjected to a surface treatment such as normal chemical treatment or electric discharge treatment before application of the anchor coating agent.
- an inorganic thin film is formed on the above-mentioned anchor coat layer.
- the inorganic substance constituting the inorganic thin film include silicon, aluminum, magnesium, zinc, tin, Nickel, titanium, hydrocarbon, etc., or oxides, carbides, nitrides, or mixtures thereof are preferable, but silicon oxide, silicon nitride, aluminum oxide, aluminum nitride, diamond-like carbon, etc. are preferable. It is a substance mainly composed of hydrocarbons. In particular, silicon oxide and aluminum oxide are preferable in that high gas barrier properties can be stably maintained.
- the above inorganic substances may be used alone or in combination of two or more.
- the vapor deposition method is preferable in that a uniform thin film having high gas noorality can be obtained, which can use any of the vapor deposition method and the coating method.
- This deposition method includes PVD (physical vapor deposition), CVD (chemical vapor deposition) and other methods such as vacuum deposition, ion plating, and sputtering!
- the thickness of the inorganic thin film is generally a force S that is 0.5 ;! to 500 nm, preferably 0.5 to 40 nm. If it is in the above-mentioned range, sufficient gas barrier properties can be obtained, and excellent transparency can be obtained without causing cracks and separation in the inorganic thin film.
- the gas barrier film layer includes those in which an inorganic thin film is formed between the base film and the structural unit layer.
- the inorganic thin film those similar to the inorganic thin film constituting the structural unit layer described above can be used.
- the gas noor film layer may have a protective layer as the uppermost layer.
- resin for forming the protective layer solvent-based and water-based resins can be used, and deviations can be used. Specifically, polyester resins, urethane resins, acrylic resins, and polybutyl alcohol resins can be used. , Ethylene 'unsaturated carboxylic acid copolymer, ethylene bur Lucol resin, bur modified resin, nitrocellulose resin, silicone resin, isocyanate resin, epoxy resin, oxazoline group-containing resin, modified styrene resin, modified silicone resin, alkyl titanate, etc. It can be used in combination.
- one or more inorganic particles selected from silica sol, alumina sol, particulate inorganic filler and layered inorganic filler are mixed with the one or more resins to improve barrier properties, abrasion resistance, and slipperiness.
- a layer made of an inorganic particle-containing resin formed by polymerizing the resin raw material in the presence of the inorganic particles are mixed with the one or more resins to improve barrier properties, abrasion resistance, and slipperiness.
- the resin for forming the protective layer is preferably the above aqueous resin from the viewpoint of improving the gas barrier property of the inorganic thin film.
- the aqueous resin is preferably a bull alcohol resin or an ethylene vinyl alcohol resin.
- a resin layer formed by applying an aqueous liquid containing polybutyl alcohol and an ethylenic unsaturated carboxylic acid copolymer can be used as the protective layer.
- the thickness of the protective layer is preferably from 0.05 to 10 m, more preferably from 0.1 to 3111, from the viewpoints of printability and processability.
- a known coating method is appropriately adopted.
- any method such as a reverse roll coater, a gravure coater, a rod coater, an air doctor coater, a spray or a coating method using a brush can be used.
- the vapor deposition film may be immersed in a protective layer resin solution. After application, moisture can be evaporated using a known drying method such as hot air drying at a temperature of about 80 to 200 ° C., heat drying such as hot roll drying, or infrared drying. As a result, a film having a uniform coating layer is obtained.
- the structural unit layer forming the gas nore film layer is preferably at least one layer from the viewpoint of barrier properties, preferably 1 to 10 layers, more preferably;! To 5 layers. It is.
- the structural unit layers may be the same or different.
- the number of constituent unit layers one constituent unit composed of an anchor coat layer and an inorganic thin film is defined as one constituent unit layer.
- the gas barrier film laminate of the present invention preferably has the above gas barrier from the viewpoint of force S, gas barrier properties, and productivity that have at least two gas barrier film layers comprising a base film and at least one structural unit layer.
- the film layer has 2 to 100 layers, more preferably 3 to 20 layers, still more preferably 3 to 10 layers.
- the plurality of gas barrier film layers are the same. It may be one or different.
- one gas barrier film layer comprising a base film and at least one structural unit layer is defined as one gas barrier film layer.
- various gas barrier film laminates in which additional constituent layers are further laminated as required can be used according to applications.
- a gas barrier film in which a plastic film is provided on the inorganic thin film or the protective layer is used for various applications.
- the thickness of the plastic film is usually selected in the range of 5 to 500 111, preferably 10 to 200 111, depending on the application, from the viewpoints of mechanical strength, flexibility and transparency as the base material of the laminate. Is done.
- the width and length of the film are not particularly limited, and can be selected according to the intended use.
- the resin that can be heat sealed include known resins such as polyethylene resin, polypropylene resin, ethylene acetate butyl copolymer, ionomer resin, acrylic resin, and biodegradable resin.
- a printing layer is formed on the coating surface of the inorganic thin film or the protective layer, and a heat seal layer is further laminated thereon. It is done.
- aqueous and solvent-based resin-containing printing inks can be used as the printing ink for forming the printing layer.
- the resin used for the printing ink include an acrylic resin, a urethane resin, a polyester resin, a chlorinated resin, a butyl acetate copolymer resin, or a mixture thereof.
- antistatic agents for printing inks, antistatic agents, light shielding agents, ultraviolet absorbers, plasticizers, lubricants, fillers, colorants, stabilizers, lubricants, antifoaming agents, crosslinking agents, anti-blocking agents, and antioxidants. You may add well-known additives, such as.
- the printing method for providing the printing layer is not particularly limited, and a known printing method such as an offset printing method, a gravure printing method, a screen printing method, or the like can be used.
- a known printing method such as an offset printing method, a gravure printing method, a screen printing method, or the like
- known drying methods such as hot air drying, hot roll drying and infrared drying can be used.
- the plastic film is the same as the thermoplastic polymer film as the base film used in the gas barrier film laminate of the present invention. Things can be used.
- paper, polyester resin, polyamide resin or biodegradable resin is preferred from the viewpoint of obtaining sufficient rigidity and strength of the laminate!
- the gas barrier properties, film quality and coating layer quality are improved.
- Heat treatment is preferably performed from the viewpoint of stabilization and fine dispersion of bubbles.
- the conditions for the heat treatment vary depending on the type and thickness of the elements constituting the gas barrier film layer, but are not particularly limited as long as the method can maintain the necessary temperature and time.
- a heating device can be incorporated in a part of the film production apparatus such as a coater or slitter, and heating can be performed during the production process.
- the temperature of the heat treatment is not particularly limited as long as the temperature is equal to or lower than the melting point of the base material, plastic film, etc. used, but the treatment time necessary for the effect of the heat treatment to be manifested can be set appropriately. It is preferable that the temperature is higher than ° C, and it is more preferable that the temperature is higher than 70 ° C.
- the upper limit of the heat treatment temperature is usually 200 ° C., preferably 160 ° C., from the viewpoint of preventing deterioration of gas barrier properties due to thermal decomposition of elements constituting the gas barrier film laminate.
- the treatment time depends on the heat treatment temperature, and the higher the treatment temperature, the shorter the force S is preferable.
- the treatment time is about 3 days to 6 months, if it is 80 ° C, the treatment time is about 3 hours to 10 days, and if it is 120 ° C, the treatment time is from 1 hour. In the case of about 1 day and 1 50 ° C, the processing time is about 3 to 60 minutes. be able to.
- the gas barrier film laminate of the present invention 40 ° C, water vapor transmission rate of at 90% RH conditions (moisture permeability) is possible in terms of the contents held or less 0. 02g / m 2 / 24hr more preferably preferably fixture or less 0. 01g / m 2 / 24hr, more preferably 0 ⁇ 005g / m 2 / 24hr or less It is below.
- the gas-nore film laminate preferably has a total light transmittance of 70% or more, more preferably 75% or more, and still more preferably 80 or more.
- the method for producing a gas barrier film laminate of the present invention includes (a) a step of forming a gas barrier film layer by sequentially forming at least one structural unit layer comprising an anchor coat layer and an inorganic thin film layer on a base material, And (b) a method for producing a gas barrier film laminate comprising a step of laminating at least two layers of the obtained gas barrier film layer via an adhesive layer made of an epoxy resin.
- the method for producing a gas barrier film laminate of the present invention comprises (a) a step of forming at least one structural unit layer comprising an anchor coat layer and an inorganic thin film layer on a substrate in order, and forming a gas barrier film layer; (B) A step of laminating at least two layers of the obtained gas barrier film layer through an adhesive layer, and (c) Heating in a vacuum atmosphere of lOOOPa or less after or simultaneously with laminating the gas noor film layer. Or a step of irradiating energy rays.
- Each of the gas barrier film layer, the anchor coat layer, the inorganic thin film layer, the gas barrier film laminate in which at least two gas barrier film layers are laminated, and the adhesive layer are as described above.
- it is also suitable for heating in a vacuum atmosphere and energy ray irradiation.
- Oxygen permeability 30000ml / m 2 / 24hr / MPa the biaxially oriented polypropylene (OPP) film having a thickness of 20 m to water vapor transmission rate is 8g / m 2 / 24hr, an adhesive is applied at a predetermined thickness
- the oxygen permeability of the adhesive layer was calculated by measuring the oxygen permeability at 25 ° C and 90% RH of the OPP film coated with adhesive using OX-TRAN2 / 21 manufactured by MOCON.
- the film laminate is cut into a strip with a width of 15 mm, and one end of the film is peeled off.
- T-peel is peeled off at a speed of 300 mm / min by a peel tester (manufactured by Shimadzu, product name EZ-TEST)
- the laminate strength (g / 15 mm) was measured.
- PET Polyethylene terephthalate resin
- P1146 Polypropylene film
- the surface of the gas barrier film layer was measured in a non-contact mode (dynamic force mode) of a scanning probe microscope (SPI3800 manufactured by Seiko Instruments Inc.). The scanning speed, the number of measurement points in one measurement area, and tilt correction were selected so that the surface condition can be clearly measured.
- the surface roughness (Rms) of the surface shape of the film was obtained by AREA analysis of “CROSSSECTION” analysis of the software attached to the scanning probe microscope SPI3800.
- PET (“Novapex” manufactured by Mitsubishi Chemical Corporation) is melt extruded to form a sheet, stretched in the longitudinal direction at a stretching temperature of 95 ° C and a stretching ratio of 3.3, and then stretched at 110 ° C and a stretching ratio of 3
- the shrinkage rate at thickness 12 111, 150 ° C is 1% to 2% in MD (flow) direction, TD (flow right angle) direction 0 ⁇
- a 5% biaxially stretched PET film was obtained.
- thermosetting adhesive layer having a thickness after drying of about 3 Hm and a surface roughness (Rms) of 0.20 ⁇ m was formed.
- Gas barrier film with adhesive layer formed is 12cm x 1 Cut out to 2cm, and overlap each adhesive layer of 5 gas barrier films with the PET surface of the base material, and unstretched 60m thick polypropylene film (Toyobo) cut into 12cmX12cm with the outermost adhesive layer ("Pyrene Film CT P1146" manufactured by Co., Ltd.) was stacked and vacuum-packed with lOPa by the method described above.
- the gas barrier film laminate sealed with a vacuum bag was heated in an oven at 120 ° C. for 30 minutes under atmospheric pressure to melt and bond the adhesive layer to obtain a gas barrier film laminate. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- PEN polyethylene naphthalate film
- Teijin Limited thickness 75 111.
- PEI polyetherimide film
- Superio UT manufactured by Mitsubishi Plastics, Inc., thickness 10 m
- a gas barrier film laminate was produced in the same manner as in Example 1 except that the number of laminated gas barrier film layers was nine. Said evaluation was performed about the obtained gas nolia film laminated body. The results are shown in Table 1.
- Example 6 The 10 nm-thick silicon nitride and silicon oxide layers deposited by applying predetermined power to monosilane, oxygen, ammonia, and hydrogen as source gases by plasma CVD under reduced pressure vacuum are used as the anchor coat layer of the gas barrier film layer.
- a gas barrier film laminate was prepared in the same manner as in Example 1 except that the composite film SiON layer (ratio of silicon nitride and silicon oxide was 8: 2) and the number of laminated gas barrier film layers was nine. Said evaluation was performed about the obtained gas noria film laminated body. The results are shown in Table 1. [0066] Example 6
- the gas barrier film was laminated in the same manner as in Example 1 except that the anchor coat layer of the gas barrier film layer was formed using a DC magnetron sputtering apparatus with chromium as a target and sputtered in an argon atmosphere of lPa to form 0.1 nm of chromium. Made the body. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- Example 1 except that the anchor coat layer of the gas barrier film layer was formed using a mixture of the following urethane resin, acrylic resin, and oxazoline resin as a solid component in a mass ratio of 4: 3: 3.
- a gas barrier film laminate was produced in the same manner. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- Example 1 except that the gas barrier film layer anchor coat layer was formed using a mixture of the following urethane resin, acrylic resin, and carpositimide resin as a solid component in a mass ratio of 4: 3: 3. In the same manner, a gas nolia film laminate was produced. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- Examples 7 and 8 the following resins were used as the urethane resin, acrylic resin, oxazoline resin, and carpositimide resin used for the anchor coat layer, respectively.
- a polyester polyol comprising 664 parts of terephthalic acid, 631 parts of isophthalic acid, 472 parts of 1,4 butanediol, and 447 parts of neopentyl alcohol was obtained.
- 321 parts of adipic acid and 268 parts of dimethylolpropionic acid were added to the obtained polyester polyol to obtain a polyester polyol A containing a pendant carboxyl group.
- 160 parts of hexamethylene diisocyanate was added to 1880 parts of the polyester polyol Anore A to obtain an aqueous polyurethane resin aqueous paint.
- ⁇ Acrylic resin> A mixture of 40 parts by weight of ethyl acrylate, 30 parts by weight of methyl methacrylate, 20 parts by weight of methacrylic acid, and 10 parts by weight of glycidyl metatalylate is solution polymerized in ethyl alcohol. Removed. The aqueous acrylic resin water-based paint was obtained by adjusting the pH to 7.5 with aqueous ammonia.
- a flask equipped with a stirrer, reflux condenser, nitrogen inlet tube, thermometer and dropping funnel is charged with 179 parts deionized water and 1 part polymerization initiator 2, 2'-azobis (2amidinopropane) dihydrochloride.
- the mixture was heated to 60 ° C while flowing nitrogen gas.
- a monomer mixture prepared beforehand by 2 parts of ethyl acrylate, 2 parts of methyl methacrylate and 16 parts of 2-isopropenyl-2-oxazoline was added dropwise from the dropping funnel over 1 hour. Thereafter, the reaction was carried out at 60 ° C for 10 hours under a nitrogen stream. After the reaction, the reaction mixture was cooled to obtain a 2-oxazoline group-containing resin aqueous solution having a solid content concentration of 10% by weight.
- Example 1 Similar to Example 1 except that the anchor coat layer used in Example 1 was formed on the inorganic thin film surface of the gas barrier film layer prepared in Example 1 and the inorganic thin film layer of Example 1 was formed in the next stage. Thus, a gas barrier film laminate was produced. The above evaluation was performed on the obtained gas nolia film laminate. The results are shown in Table 1.
- Example 1 as an adhesive layer, 50 parts by mass of urethane phthalate as a urethane (meth) acrylate component and bisphenol A glycidyl as an epoxy (meth) acrylate component Luether-type epoxy acrylate (weight average molecular weight 2000) 20 parts by mass, alicyclic (meth) terminated as a talylate component, 30 parts by mass of tricyclodecane diatalylate, as a polymerization initiator 2-hydroxy-1 ⁇ 4 [4 1 (2 Hydroxy 2 methyl-propionyl) benzyl] phenyl ⁇ 2-methyl-propane 1-on 2 parts by weight of a mixed solution was applied, and after drying, the thickness was about 3 m and the surface roughness (Rms) 0.
- Rms surface roughness
- a gas barrier film laminate was produced in the same manner as in Example 10 except that the number of laminated gas barrier film layers was nine. Said evaluation was performed about the obtained gas nolia film laminated body. The results are shown in Table 1.
- the anchor coat layer of the gas barrier film was deposited by applying a predetermined power and supplying monosilane, oxygen, ammonia, and hydrogen as source gases by plasma CVD under a reduced-pressure vacuum.
- a gas barrier film laminate was prepared in the same manner as in Example 10 except that the silicon composite film SiON layer (the ratio of silicon nitride and silicon oxide was 8: 2) and the number of laminated gas barrier film layers was nine. . Said evaluation was performed about the obtained gas noria film laminated body. The results are shown in Table 1.
- Example 1 as an adhesive layer, a bisphenol A type epoxy resin (weight average molecular weight: 400, epoxy equivalent 200, Epicoat 828 manufactured by Yuka Shell Epoxy Co., Ltd.) (Weight average molecular weight: 960, phenolic hydroxyl group equivalent: 120, Phenolite LF2882 manufactured by Dainippon Ink & Chemicals, Inc.) 2 5 parts by mass, phenoxy resin (weight average molecular weight as a high molecular weight component compatible with epoxy resin) : 50, 000, Phenototo YP-50, manufactured by Toto Kasei Co., Ltd.
- a bisphenol A type epoxy resin weight average molecular weight: 400, epoxy equivalent 200, Epicoat 828 manufactured by Yuka Shell Epoxy Co., Ltd.
- phenoxy resin weight average molecular weight as a high molecular weight component compatible with epoxy resin
- the obtained varnish was applied onto a release PET film having a thickness of 50 am and a surface roughness of RmsO. 10 ⁇ m with a knife coater and heated at 110 ° C for 15 minutes to remove the solvent.
- the resin is semi-cured to produce an adhesive film with a release PET film with an adhesive layer thickness of 10 m, and the release PET film is peeled off from the adhesive film with a release PET film.
- An adhesive film having S10 m and surface roughness (Rms) of 0.1 ⁇ m was prepared.
- the obtained adhesive film was used in the same manner except that the number of laminated gas barrier film layers was nine.
- a gas barrier film laminate sealed with a vacuum bag was heated in an oven at 120 ° C under atmospheric pressure. Was heated for 30 minutes to melt bond the adhesive layer to obtain a gas barrier film laminate. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- a gas barrier film laminate was produced in the same manner as in Example 13 except that the adhesive film prepared in Example 13 was pressed with an embossing roll and the surface roughness (Rms) on both sides was changed to 5 am.
- the above-described evaluation was performed on the obtained gas nolia film laminate. The results are shown in Table 1.
- the following epoxy adhesive was applied to the inorganic thin film surface of the gas barrier film layer prepared in Example 1, and the thickness after drying was about 3 am, and the surface roughness (Rms) was 0.25, im.
- An adhesive layer was formed and laminated on the PET surface of another gas barrier film under the atmosphere.
- the above-mentioned adhesive was applied in the same manner to the inorganic thin film surface of the obtained gas barrier film, and the outermost A gas barrier film laminate was obtained by laminating an adhesive layer of layers and an unstretched polypropylene film having a thickness of 60 ⁇ (“Pyrene Film CT P1146” manufactured by Toyobo Co., Ltd.). Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- a reaction vessel was charged with 1 mol of metaxylylenediamine. The temperature was raised to 60 ° C. under a nitrogen stream, and 0.93 mol of methyl acrylate was added dropwise over 1 hour. After completion of the dropwise addition, the mixture was stirred at 120 ° C for 1 hour, and further heated to 160 ° C in 3 hours while distilling off generated methanol. The mixture was cooled to 100 ° C., and a predetermined amount of methanol was added so that the solid content concentration became 70% by weight to obtain an epoxy resin curing agent a.
- Example 15 a gas barrier film laminate was obtained in the same manner as in Example 15 except that the gas barrier film layer was replaced with the gas barrier film layer used in Example 2. Said evaluation was performed about the obtained gas nolia film laminated body. The results are shown in Table 1.
- Example 16 an adhesive layer was similarly provided on the inorganic thin film surface of the other laminated gas barrier film layers, and a similar gas barrier film layer was further provided thereon to form three layers. Thus, a gas nolia film laminate was obtained. The obtained gas barrier film laminate was evaluated as described above. The results are shown in Table 1.
- Example 15 5 mass% of silica particles having an average particle diameter of 0.01 m (Snowtech MEK-ST, manufactured by Nissan Chemical Industries, Ltd.) was added to the epoxy adhesive layer based on the resin solid content.
- a gas barrier film laminate was obtained in the same manner as Example 15 except for the above. The above gas barrier film laminate was evaluated as described above. The results are shown in Table 1.
- Example 15 the same procedure as in Example 15 was conducted, except that polymer particles having an average particle size of 0.1 m (Staphyroid AC3364, manufactured by Ganz Kasei Co., Ltd.) were added to the epoxy adhesive in an amount of 10% by mass based on the resin solid content. Thus, a gas barrier film laminate was obtained. The gas barrier film laminate thus obtained was evaluated as described above. The results are shown in Table 1.
- a gas barrier film laminate was prepared in the same manner as in Example 1 except that the gas barrier film layer was laminated under atmospheric pressure without vacuum packaging. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- a gas barrier film laminate was prepared in the same manner as in Example 10 except that the gas barrier film was laminated under atmospheric pressure without vacuum packaging. Said evaluation was performed about the obtained gas barrier film laminated body. The results are shown in Table 1.
- Example 15 was the same as Example 15 except that the adhesive was changed to a urethane-based adhesive ("AD900" manufactured by Toyo Morton Co., Ltd. and "CAT-RT85” in a ratio of 10: 1.5). Thus, a gas barrier film laminate was produced. The obtained gas barrier film laminate was evaluated as described above. The results are shown in Table 1.
- AC is a composite film of S-silica and oxide silica SiON brows
- the gas barrier film laminate of the present invention is widely used for packaging of articles that require blocking of various gases such as water vapor and oxygen, for example, packaging for preventing deterioration of food, industrial products, pharmaceuticals, and the like.
- transparent conductive sheets used in liquid crystal display elements, solar cells, electromagnetic shields, touch panels, EL substrates, color filters, etc. can also be used suitably.
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Description
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US12/514,485 US8343623B2 (en) | 2006-11-16 | 2007-11-15 | Gas barrier film laminate |
JP2008544193A JP5020255B2 (ja) | 2006-11-16 | 2007-11-15 | ガスバリアフィルム積層体 |
EP07831922.5A EP2080613B1 (en) | 2006-11-16 | 2007-11-15 | Gas barrier film laminate |
US13/594,209 US8568868B2 (en) | 2006-11-16 | 2012-08-24 | Gas barrier film laminate |
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US13/594,209 Continuation US8568868B2 (en) | 2006-11-16 | 2012-08-24 | Gas barrier film laminate |
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EP (1) | EP2080613B1 (ja) |
JP (2) | JP5020255B2 (ja) |
KR (1) | KR101392004B1 (ja) |
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TW200831294A (en) | 2008-08-01 |
CN101535040A (zh) | 2009-09-16 |
TWI438100B (zh) | 2014-05-21 |
US8568868B2 (en) | 2013-10-29 |
EP2080613A1 (en) | 2009-07-22 |
US8343623B2 (en) | 2013-01-01 |
KR101392004B1 (ko) | 2014-05-07 |
EP2080613B1 (en) | 2016-03-16 |
JP5456806B2 (ja) | 2014-04-02 |
EP2080613A4 (en) | 2011-06-29 |
JP2012096551A (ja) | 2012-05-24 |
US20100015431A1 (en) | 2010-01-21 |
JP5020255B2 (ja) | 2012-09-05 |
US20120315462A1 (en) | 2012-12-13 |
JPWO2008059925A1 (ja) | 2010-03-04 |
KR20090085622A (ko) | 2009-08-07 |
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