WO2022172735A1 - 積層ポリエステルフィルム、およびポリエステルフィルムの製造方法 - Google Patents
積層ポリエステルフィルム、およびポリエステルフィルムの製造方法 Download PDFInfo
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- WO2022172735A1 WO2022172735A1 PCT/JP2022/002364 JP2022002364W WO2022172735A1 WO 2022172735 A1 WO2022172735 A1 WO 2022172735A1 JP 2022002364 W JP2022002364 W JP 2022002364W WO 2022172735 A1 WO2022172735 A1 WO 2022172735A1
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- polyester film
- laminated polyester
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- NJSUFZNXBBXAAC-UHFFFAOYSA-N ethanol;toluene Chemical compound CCO.CC1=CC=CC=C1 NJSUFZNXBBXAAC-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- OAMZXMDZZWGPMH-UHFFFAOYSA-N ethyl acetate;toluene Chemical compound CCOC(C)=O.CC1=CC=CC=C1 OAMZXMDZZWGPMH-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 108010067216 glycyl-glycyl-glycine Proteins 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 229940097364 magnesium acetate tetrahydrate Drugs 0.000 description 1
- XKPKPGCRSHFTKM-UHFFFAOYSA-L magnesium;diacetate;tetrahydrate Chemical compound O.O.O.O.[Mg+2].CC([O-])=O.CC([O-])=O XKPKPGCRSHFTKM-UHFFFAOYSA-L 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
- ABMFBCRYHDZLRD-UHFFFAOYSA-N naphthalene-1,4-dicarboxylic acid Chemical compound C1=CC=C2C(C(=O)O)=CC=C(C(O)=O)C2=C1 ABMFBCRYHDZLRD-UHFFFAOYSA-N 0.000 description 1
- DFFZOPXDTCDZDP-UHFFFAOYSA-N naphthalene-1,5-dicarboxylic acid Chemical compound C1=CC=C2C(C(=O)O)=CC=CC2=C1C(O)=O DFFZOPXDTCDZDP-UHFFFAOYSA-N 0.000 description 1
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920002114 octoxynol-9 Polymers 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 description 1
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001816 polyoxyethylene sorbitan tristearate Substances 0.000 description 1
- 235000010988 polyoxyethylene sorbitan tristearate Nutrition 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 159000000000 sodium salts Chemical group 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
- 235000011071 sorbitan monopalmitate Nutrition 0.000 description 1
- 229940031953 sorbitan monopalmitate Drugs 0.000 description 1
- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003866 tertiary ammonium salts Chemical group 0.000 description 1
- 239000012974 tin catalyst Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- GZXOHHPYODFEGO-UHFFFAOYSA-N triglycine sulfate Chemical compound NCC(O)=O.NCC(O)=O.NCC(O)=O.OS(O)(=O)=O GZXOHHPYODFEGO-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N urethane group Chemical group NC(=O)OCC JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229940042596 viscoat Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/30—Producing shaped prefabricated articles from the material by applying the material on to a core or other moulding surface to form a layer thereon
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/14—Layered products comprising a layer of synthetic resin next to a particulate layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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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
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/022—Mechanical properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2315/00—Other materials containing non-metallic inorganic compounds not provided for in groups B32B2311/00 - B32B2313/04
- B32B2315/02—Ceramics
-
- 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
- B32B2457/00—Electrical equipment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Definitions
- the present invention relates to a laminated polyester film that is excellent in removing layers provided on the laminated polyester film.
- a general method for producing an MLCC is to use a plastic film as a substrate, laminate a ceramic green sheet and an electrode on a release film having a release layer provided on the substrate, dry and solidify, and then The laminate is peeled off from the release film, a plurality of layers are laminated, and the laminate is fired. In this process, the release film is discarded as an unnecessary material during the process.
- the amount of release film that is discarded as unnecessary material is increasing, and the environmental burden is becoming an issue.
- the components of the release layer contained in the release film used in the manufacturing process of MLCC are generally different in composition from the components constituting the film from the viewpoint of releasability, so the release layer is attached. If the release film is remelted as it is, the components of the release layer are present as foreign matter, making reuse difficult.
- Patent Document 1 discloses a method of cleaning a release film having a release layer with a metal brush and reusing the film after removing the release layer. It is Further, Patent Document 2 discloses a method of providing a water-soluble resin layer between a release layer and a polyester film, removing the release layer by washing with water, and then reusing the layer. Furthermore, in Patent Document 3, a ceramic green sheet having good smoothness and peelability is obtained by specifying the process conditions for laminating the ceramic green sheet, and a water-soluble resin layer is provided between the release layer and the polyester film. A method is disclosed in which the release layer is removed by providing and washing with water, and then reused.
- JP 2012-171276 A Japanese Patent No. 4284936 Japanese Patent Application Laid-Open No. 2004-160773
- the laminated polyester film used as the base material of the release film is required to have "reusability", and the film itself is required to be processable in subsequent processes.
- an object of the present invention is to provide a laminated polyester film that is highly reusable and suitable for processing in subsequent processes.
- Condition 1 20 ⁇ X P ⁇ 45
- Condition 2 3.0 ⁇ XH ⁇ 10 ⁇ X P (mN/m): polar component of surface free energy of layer X ⁇ X H (mN/m): hydrogen bond component of surface free energy of layer X
- thickness xa (nm) of layer X The laminated polyester film according to [I], wherein the surface roughness RzjisB (nm) of the surface (B surface) opposite to the surface (A surface) having the layer X of the polyester film satisfies the following conditions.
- Condition 3 1.0 ⁇ RzjisB/xa ⁇ 20.0 xa (nm): thickness of layer X [III]
- Condition 4 20 ⁇ X P ⁇ 30
- Condition 5 6.0 ⁇ XH ⁇ 10 [IV]
- the laminated polyester film according to [II] or [III] which satisfies the following conditions.
- Condition 6 1.5 ⁇ RzjisB/xa ⁇ 10.0 [V]
- [XI] The laminated polyester film of [X], wherein the degree of crystallinity of the layer X is higher than 31% and not higher than 40%.
- [XII] The laminated polyester film according to any one of [I] to [XI], wherein the layer X contains a resin having a degree of polymerization of 200 or more.
- [XIII] The laminated polyester film according to any one of [I] to [XII], which has a layer Y, a layer X, and a polyester film satisfying the following conditions in this order.
- Condition 9 80 ⁇ HY(1) ⁇ 120
- Condition 10 1 ⁇
- Method for measuring solvent durability Testing machine: Gakushin type testing machine (Friction tester type II described in JIS L 0849 (2013)) Friction element: Cotton cloth (Kanba No.
- [XIX] The laminated polyester film according to any one of [XVI] to [XVIII], wherein the release layer is a ceramic green sheet containing barium titanate as a main component.
- MLCC laminated ceramic capacitor
- the polyester film has a layer (A layer) that constitutes the A surface that is one surface of the polyester film, a layer (B layer) that constitutes the B surface that is the other surface, and a layer that does not have a surface (C layer ), wherein the layer C contains a recycled polyester raw material, the laminated polyester film according to any one of [I] to [XXI].
- [XXIII] Using the laminated polyester film according to [XXII], which has at least a release layer, a layer Y, and a polyester film in this order, the step of peeling the release layer from the layer Y; A step of removing the layer Y from the film from which the release layer and the layer Y have been removed, a step of producing a recycled raw material from the film from which the release layer and the layer Y have been removed, and a step of forming a film using the recycled raw material.
- a method for producing a polyester film is Using the laminated polyester film according to [XXII], which has at least a release layer, a layer Y, and a polyester film in this order, the step of peeling the release layer from the layer Y; A step of removing the layer Y from the film from which the release layer and the layer Y have been removed, a step of producing a recycled raw material from the film from which the release layer and the layer Y have been removed, and a step of forming a film
- the present invention relates to a polyester film and a laminated polyester film having one or more layers.
- the polyester referred to in the present invention comprises a dicarboxylic acid component and a diol component.
- the term "constituent" refers to a minimum unit that can be obtained by hydrolyzing a polyester.
- Dicarboxylic acid constituents constituting such polyesters include terephthalic acid, isophthalic acid, phthalic acid, 1,4-naphthalenedicarboxylic acid, 1,5-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid, and 1,8-naphthalene.
- Dicarboxylic acids, aromatic dicarboxylic acids such as 4,4′-diphenyldicarboxylic acid and 4,4′-diphenyletherdicarboxylic acid, and ester derivatives thereof can be mentioned.
- Diol constituents constituting such polyesters include ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,2-butanediol, and 1,3-butanediol. and alicyclic diols such as cyclohexanedimethanol and spiroglycol, and diols in which a plurality of the above diols are linked.
- PET polyethylene terephthalate
- PEN polyethylene-2,6-naphthalenedicarboxylate
- isophthalic acid and naphthalenedicarboxylic acid are copolymerized with some of the dicarboxylic acid components of PET.
- polyester obtained by copolymerizing cyclohexanedimethanol, spiroglycol, and diethylene glycol as part of the diol component of PET is preferably used.
- a preferred embodiment of the laminated polyester film of the present invention is a polyester film and a laminated polyester film having a layer X that satisfies the following conditions 1 and 2, and is more preferable from the viewpoint of simpler configuration and higher productivity.
- One aspect is a laminated polyester film having a layer X that satisfies the following conditions 1 and 2 on at least one side of the polyester film.
- Condition 1 20 ⁇ X P ⁇ 45 Condition 2: 3.0 ⁇ XH ⁇ 10 ⁇ X P (mN/m): Polar component of surface free energy of layer X ⁇ X H (mN/m): Hydrogen bonding component of surface free energy of layer X
- the polar component of surface free energy ⁇ X P and the hydrogen bonding component ⁇ X H are ,
- the static contact angle at 25 ° C. with glycerol, ethylene glycol, formamide, and diiodomethane is determined on the layer X surface of the laminated polyester film, and the static contact angle with each liquid and the following non-patent document 1 are described.
- Non-Patent Document 1 J.P. Panzer: J.P. Colloid Interface Sci. , 44, 142 (1973). .
- Non-Patent Document 2 Yasuaki Kitazaki, Toshio Hata: Japan Adhesive Association Paper, 8, (3) 131 (1972).
- the solvent resistance referred to here means, for example, coating a release layer on the layer X with a coating agent containing a solvent, or further coating a ceramic green sheet thereon with a slurry containing a solvent.
- ⁇ X P is more preferably 20 mN/m or more and 30 mN/m or less, more preferably 22 mN/m or more and 28 mN/m or less
- ⁇ X H is 4.0 mN/m or more and 10 mN. /m or less, more preferably 6.0 mN/m or more and 10 mN/m or less, and particularly preferably 7 mN/m or more and 9 mN/m or less.
- the polar component ⁇ X P and the hydrogen bonding component ⁇ X H are within the above range, so side chain groups such as carboxylates, sulfonates, and tertiary ammonium salts are used. It is one of preferred embodiments to introduce an ionic polar group. Among them, sulfonates can be preferably used from the viewpoint of water solubility and solvent resistance. That is, it is more preferable that the layer X contains a resin having a sulfonate-modified polyvinyl alcohol skeleton.
- the amount of copolymerization is preferably 0.1 mol % or more and 10 mol % or less, more preferably 0.5 mol % or more and 10 mol % or less, still more preferably 0.5 mol % or more and 5.0 mol %, based on the entire resin having a polyvinyl alcohol skeleton. % or less, particularly preferably 1.0 mol % or more and 3.0 mol % or less.
- the degree of polymerization is preferably more than 200 and 1000 or less, more preferably 300 or more and 1000 or less, and still more preferably 400 or more and 600 or less.
- the degree of saponification is preferably 30 or more and 90 or less, more preferably 60 or more and 88 or less.
- the difference between the contact angle HX (1) 1 second after water contacts the layer X and the contact angle HX (20) 20 seconds after water contacts the layer X is preferably 5° or more and 60° or less.
- represents the amount of change in the contact angle of water before and after the lapse of a certain period of time. , a large value indicates that the amount of change in the contact angle of water before and after the lapse of a certain period of time is large.
- Further, by setting
- the layer X of the laminated polyester film of the present invention preferably contains a water-soluble substance.
- a water-soluble substance in the layer X it becomes easy to set
- the layer X contains a water-soluble substance, by washing the laminated polyester film containing the layer X with water, the layer X dissolves in water, removing the layer X and the layer laminated above the layer X, It becomes easy to take out a polyester film with high purity.
- the water-soluble substance is preferably contained in an amount of 60% by mass or more, more preferably 90% by mass or more, even more preferably 95% by mass or more, with respect to the entire layer X, and may consist only of a water-soluble substance. Especially preferred. From the viewpoint of taking out a polyester film with high purity, it is preferable that the layer X and the polyester film are in contact with each other.
- water-soluble substances examples include resins having a water-soluble polyester skeleton, resins having a polyester urethane skeleton, resins having a polyvinyl alcohol skeleton (hereinafter, polyvinyl alcohol may be referred to as PVA), and polyvinylpyrrolidone skeletons. Resins (hereinafter, polyvinylpyrrolidone may be referred to as PVP) and those containing starch as a main component can be exemplified.
- PVP polyvinylpyrrolidone
- the term “water-soluble” as used herein means that the amount of change in mass when immersed in water at 50° C. for 10 minutes is 15% or more, and an aqueous solution is formed. A specific method is as follows.
- water-soluble means that the resin is immersed in water at 50 ° C. for 10 minutes, removed from the water, and the water droplets adhering to the surface are sufficiently wiped off with a waste cloth.
- the amount of change ⁇ M is 15% or more, and an aqueous solution is obtained.
- ⁇ M
- the main component means that 60% by mass or more of the component is contained in 100% by mass of the layer.
- the layer X preferably contains a resin having a polyvinyl alcohol skeleton, and the layer X more preferably consists of only a resin having a polyvinyl alcohol skeleton.
- a resin having a PVA skeleton is preferable because it has few non-polar sites and many hydrophilic groups, so it has high water solubility and solvent resistance.
- the degree of polymerization is preferably more than 200 and 1000 or less, more preferably 300 or more and 1000 or less, and still more preferably 400 or more and 600 or less.
- the degree of polymerization is preferably more than 200 and 1000 or less, more preferably 300 or more and 1000 or less, and still more preferably 400 or more and 600 or less.
- the degree of polymerization is more than 200, the coatability can be improved when the layer X is provided by coating. You can prevent it from getting worse.
- the degree of polymerization refers to the average degree of polymerization determined by JIS K 6726 (1994).
- the required average degree of polymerization is more than 200 and 1000 or less. , more preferably 300 or more and 1000 or less, and even more preferably 400 or more and 600 or less.
- the layer X preferably contains 60% by mass or more of a resin having a polyvinyl alcohol skeleton with respect to the entire layer X, more preferably 90% by mass or more, and further preferably 95% by mass or more.
- it is particularly preferably composed only of a resin having a polyvinyl alcohol skeleton.
- the layer X preferably exhibits water solubility.
- the degree of saponification is preferably 30 or more and 90 or less, more preferably 60 or more and 88 or less.
- Polyvinyl alcohol has at least hydroxyl groups and acetic acid groups as side chains. Therefore, when the degree of saponification is high, crystallization tends to occur easily due to molecular chain packing. When the degree of saponification is 90 or less, the degree of crystallinity can be lowered and the washability with water is further improved. Further, when the degree of saponification is 30 or more, the amount of acetic acid groups can be kept below a certain level, so that the water washability is improved.
- can easily be set within a preferable range, and the solvent resistance can be improved.
- the resin having a polyvinyl alcohol skeleton used as the layer X it is also a preferred embodiment to use a copolymerized polyvinyl alcohol in which a functional group other than a hydroxyl group or an acetic acid group is copolymerized on the side chain.
- a hydrophilic and bulky functional group such as a sulfonate
- sulfonic acid can be preferably used from the viewpoint of water solubility and solvent resistance. That is, layer X preferably contains a resin having a sulfonate-modified polyvinyl alcohol skeleton.
- the copolymerization amount is preferably 0.1 mol % or more and 10 mol % or less, more preferably 0.5 mol % or more and 5.0 mol % or less, still more preferably 1.0 mol %, based on the entire resin having a polyvinyl alcohol skeleton. % or more and 3.0 mol % or less.
- the amount of copolymerization is within the above range, when the layer X is provided by coating, the coatability is improved, and it is possible to suppress uneven distribution on the film and an excessive increase in crystallinity.
- sodium sulfonate is preferable.
- the copolymerization component is a sodium salt as described above, sodium can be supplied by sodium hydroxide used as an alkali for saponification.
- the layer X does not contain an acrylic resin or polyester resin having a binder function, or a resin with a cross-linking action such as melamine or oxazoline that improves film-forming properties. Binders and cross-linking resins tend to interact with hydroxyl groups on the side chains of resins having a polyvinyl alcohol skeleton, making it difficult to make
- the crystallinity of layer X of the laminated polyester film of the present invention is preferably 14% or more and 40% or less, more preferably 15% or more and 40% or less, and even more preferably 31% or more and 40% or less.
- the degree of crystallinity generally represents the degree of crystallization of a substance, and the higher the degree of crystallinity, the more free-energy-stable crystal portions the substance contains. That is, the higher the degree of crystallinity, the more stable the substance itself.
- a crystallinity of 15% or more can improve solvent resistance. Further, when the degree of crystallinity is 40% or less, water washability can be further improved. Further,
- the degree of crystallinity of the layer X can be set within the above-described range by setting the copolymerization amount, the degree of polymerization, and the degree of saponification within the preferred ranges described above.
- the crystallinity of layer X shall be obtained by the method described in the examples.
- a preferred embodiment of the laminated polyester film of the present invention is a laminated polyester film having a polyester film and a layer X, wherein the thickness xa (nm) of the layer X and the surface having the layer X of the polyester film (surface A ) is a laminated polyester film having a surface roughness RzjisB (nm) on the opposite side (surface B) that satisfies the following conditions.
- a more preferable aspect is that the surface on the opposite side (B surface) is the surface (A surface) having the layer X of the polyester film. is the opposite side (B side).
- the layer X satisfies the above performance and an embodiment in which the layer X exhibits hydrophilicity can be cited as more preferred embodiments other than the above.
- that the layer X exhibits hydrophilicity means that the surface free energy value is 10 mN/m or more when measured by the method described in Examples. If the layer X is not exposed, the layer X is exposed by polishing until the thickness of the layer X is in the range of 30 to 70% of the original thickness of the layer X, and the surface free energy of the layer X is increased. shall be requested.
- the properties of the film may change significantly when stored in a moist and hot atmosphere. You may encounter problems when using .
- the occurrence of such a change in properties can be greatly suppressed. This will be explained in detail below.
- the layer X comes into contact with the surface of the polyester film on the opposite side (side B) to the side having the layer X (side A).
- RzjisB is the 10-point average roughness measured by the method described in Examples, and the larger the value, the greater the unevenness of the surface.
- the value of RzjisB/xa is small and less than 0.2, that is, when RzjisB is small, or the value of xa is large, or both, under conditions where surface pressure is applied in the roll shape, in a moist and hot atmosphere
- the layer X tends to adhere to the surface of the B side, and the layer X may be transferred to the surface of the B side.
- the shape of the layer X may change, the washability of the layer X may deteriorate, or when another layer is applied in contact with the layer X, the coatability and function of the layer may deteriorate. .
- the value of RzjisB/xa is more preferably 1.0 or more and 10.0 or less, still more preferably 1.5 or more and 10.0 or less, and particularly preferably 3.0 or more and 8.5 or less. .
- the thickness xa (nm) of the layer X and the surface roughness RzjisX (nm) of the layer X preferably satisfy Condition 7 below.
- RzjisX refers to surface roughness RzjisX of layer X, which is a 10-point average roughness measured by the method described in Examples.
- RzjisX represents the roughness of the surface of the layer X opposite to the surface in contact with the polyester film.
- the roughness of the layer X is affected by the roughness of the A side of the polyester film, but by setting RzjisX/xa to 3.0 or less, the layer X can cover the entire A side, The hydrophilicity of layer X can be improved. Moreover, when another layer is applied in contact with the layer X, the coatability and function of the layer can be fully exhibited.
- RzjisX/xa By setting RzjisX/xa to 0.01 or more, the handleability of the film can be improved. From the same viewpoint as above, RzjisX/xa is more preferably 0.5 or more and 1.5 or less.
- the thickness xa of the layer X is preferably 10 nm or more and 500 nm or less. Setting xa to 10 nm or more makes it easier to satisfy Conditions 3 and 7, thereby increasing productivity. In addition, by setting xa to 500 nm or less, it is possible to improve coatability when the layer X is provided by coating.
- a preferred embodiment of the laminated polyester film of the present invention is a laminated polyester film having a layer Y satisfying the following formula on at least one surface layer.
- a laminated polyester film having a layer Y, a layer X, and a polyester film satisfying the following formula in this order can be mentioned as a more preferable embodiment from the viewpoint of further improving water washability.
- a particularly preferred embodiment is a laminated polyester film having a layer Y that satisfies the following conditions on the surface opposite to the contact surface.
- the contact angle with water to satisfy 80 ⁇ HY (1), the releasability can be sufficiently improved, and the laminated polyester film having the layer Y can be suitably used as a release film. can.
- the laminated polyester film having the layer Y can be suitably used as a release film. can.
- HY(1) ⁇ 120 it becomes difficult to repel the coating agent for forming the release layer when the release layer is provided by coating, and coating defects such as pinholes occur in the release layer. can be prevented.
- HY(1) is more preferably 85° or more and 110° or less.
- HY(20) changes compared to HY(1), and by setting
- means that the layer Y is permeable to water.
- a large amount of water permeates the polyester film side of the substrate, making it easier to separate from other layers at the surface of the substrate. It becomes easy to remove Y from the laminated polyester film with water and to recycle it. From the same point of view, it is more preferable to satisfy 5 ⁇
- ⁇ 90 the physical properties of the layer Y are stabilized, and deterioration of the layer Y due to water vapor or the like can be suppressed.
- of the layer Y within the preferred range described above is not particularly limited. , a surface free energy polar component ⁇ X P of 20 mN/m or more and 30 mN/m or less and a surface free energy hydrogen bonding component ⁇ X H of 6.0 mN/m or more and 10 mN/m or less on at least one side of a polyester film.
- a laminated polyester film having a layer X of which is a preferred embodiment a method of forming a laminated polyester film having a layer Y on the opposite side of the layer X in contact with the polyester film can be mentioned.
- Examples of resins that can be used for layer Y of the laminated polyester film having a substrate/layer Y structure include silicone compounds having a dimethylsiloxane skeleton, compounds having long-chain alkyl groups, compounds having a polyolefin skeleton, perfluoroalkyl groups, and the like.
- One or more compounds selected from fluorine-containing compounds can be preferably used.
- compounds having a polyolefin skeleton can be preferably used.
- Compounds having a polyolefin as a main skeleton tend to have good compatibility with surfactants described later, so that
- Examples of compounds having a polyolefin skeleton include polyethylene, polypropylene, polybutadiene, hydrogenated polybutadiene, polyisoprene, hydrogenated polyisoprene, polyisobutylene, and ⁇ -olefins.
- the above copolymers can be mentioned.
- An ⁇ -olefin is an olefin having a double bond at one end of the molecular chain, and examples thereof include 1-octene.
- the layer Y preferably contains a surfactant.
- the amount of surfactant added to 100 parts by mass of the compound having a polyolefin skeleton is preferably 0.5 parts by mass or more and 4 parts by mass or less, more preferably 1 part by mass or more and 2 parts by mass or less.
- the amount of the surfactant is 0.5 parts by mass or more, the amount of the surfactant is sufficient to spread over the entire layer Y, making it easier for water to permeate the layer Y. If the added amount of the surfactant exceeds 4 parts by mass, the surfactant may gather on the surface of the layer Y and contaminate the release material.
- surfactants that can be used in the layer Y of the laminated polyester film having a structure of substrate/layer Y include various nonionic surfactants such as polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, poly Polyoxyethylene alkyl ethers such as oxyethylene stearyl ether and polyoxyethylene oleyl ether; Polyoxyethylene alkylphenyl ethers such as polyoxyethylene octylphenyl ether and polyoxyethylene nonylphenyl ether; Polyoxyethylene monolaurate and polyoxyethylene Polyoxyethylene fatty acid esters such as monostearate and polyoxyethylene monooleate; Sorbitan fatty acid esters such as sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate and sorbitan monooleate; Polyoxyethylene sorbitan monolaurate , polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbit
- polyoxyethylene sorbitan fatty acid ester polyoxyethylene glyceryl ether fatty acid ester; polyoxyethylene-polyoxypropylene block copolymer; These nonionic surfactants can be used singly or in combination of two or more.
- Examples of highly water-repellent resins that can be used for layer Y of a laminated polyester film having a substrate, layer X, and layer Y include a silicone compound having a dimethylsiloxane skeleton, a compound having a long-chain alkyl group, and a compound having fluorine. be done.
- a silicone (organopolysiloxane) having a dimethylsiloxane skeleton having high water permeability is preferable, and a resin having a curable silicone skeleton can be particularly preferably used.
- the resin having a curable silicone skeleton is an "addition reaction type" organohydrogenpolyloxane obtained by heating and curing an organohydrogenpolyloxane and an organopolysiloxane containing an alkenyl group in the presence of a platinum catalyst.
- the resin having an addition reaction type silicone skeleton preferably include polydimethylsiloxane and hydrogen siloxane containing vinyl groups at the terminals, such as KS-847, KS-847T manufactured by Shin-Etsu Chemical Co., Ltd., KS-841, KS-774, KS-3703T, X-62-2825, SD7333 manufactured by Dow Toray Co., Ltd., SRX357, SRX345, LTC310, LTC303E, LTC300B, LTC350G, LTC750A, LTC851, LTC759, LTC755, LTC755, LTC766 , etc. ("LTC" is a registered trademark).
- the resin having a condensation reaction type silicone skeleton and the catalyst are preferably those containing polydimethylsiloxane and hydrogensiloxane containing hydroxyl groups at the terminals and an organotin catalyst, such as SRX290 and SY manufactured by Dow Toray Industries, Inc. LOFF23 can be mentioned.
- resins and catalysts having a UV-curable silicone skeleton include those containing organopolysiloxane containing an acryloyl group or methacryloyl group and a photopolymerization initiator, polydimethylsiloxane containing an alkenyl group, and polydimethylsiloxane containing a mercapto group.
- Those containing dimethylsiloxane and a photopolymerization initiator are preferable, and FM-0711, FM-0721, FM-0725, FM-7711, FM-7721, FM-7725 manufactured by JNC Co., Ltd., BY24 manufactured by Dow Toray Industries, Inc. -510H and BY24-544.
- the resin having a cationically polymerizable silicone skeleton and the catalyst preferably include a siloxane containing an epoxy group and an onium salt initiator, such as TPR6501, UV9300 and XS56 manufactured by Momentive Performance Materials Japan LLC. -A2775 and the like.
- the layer Y of the laminated polyester film of the present invention has a surface solvent durability of 5% or more and 100% or less. More preferably, it is 10% or more and 100% or less.
- Solvent durability refers to the value obtained by performing a rubbing test using a solvent on the surface of the layer Y of the laminated polyester film, and dividing the peeling force of the layer Y surface by the peeling force of the layer Y surface after the rubbing test. . Details of the measurement method will be described later. Higher solvent durability means higher solvent resistance, and deterioration of smoothness and removability due to water in subsequent steps can be suppressed. The substantial upper limit of the solvent durability is 100%. If a highly removable resin is used to improve reusability, solvent durability tends to be low.
- the hydrogen bond component ⁇ YH of the surface free energy of the layer Y of the laminated polyester film of the present invention is preferably 1.5 mN/m or more and 10 mN/m or less, and 1.5 mN/m or more and 5.0 mN/m or less. is more preferable.
- the layer Y becomes more permeable to water. It can be easily removed by peeling off the layer formed on the substrate from the side closer to the substrate surface.
- the layer X when the layer X is also present, the layer X can be more actively removed by the water permeating the layer Y, and the layers X and Y can be easily removed from the laminated polyester film.
- a release layer is provided on the surface opposite to the surface in contact with the layer X or the base material of the layer Y, and the release layer is peeled off from the layer Y. It can be suitably used for the purpose. Furthermore, since the laminated polyester film of the present invention can remove the layer X and the layer Y with water, after peeling off the release object, the layer X and the layer Y are removed to obtain a polyester film with high purity. can be extracted. Furthermore, after removing the layer X and the layer Y from the laminated polyester film of the present invention, it is preferable to take out a polyester film with high purity and reuse it.
- the method of recycling include a method of providing the layer X and the layer Y again on the polyester film taken out and using it as a release film, and a method of remelting the polyester film and molding it again into a polyester film.
- the method of remelting and molding into a polyester film again is preferable because the reuse application is not limited, it can be used for various purposes, and can greatly contribute to the reduction of environmental load.
- the component containing the dimethylsiloxane bond is likely to become a foreign matter when mixed with the polyester film and remelted, and the polyester deteriorates. It is preferred to remove layer Y in order to re-melt and reuse the film of the present invention, as it may promote the process and may not be extrudable after melting.
- the release layer is an organic pressure-sensitive adhesive containing acrylic as a main component, or an inorganic material containing metal or metal oxide as a main component. sheet.
- barium titanate which is a metal oxide, is indispensable for manufacturing MLCCs, and the amount of release film used in the process for manufacturing barium titanate sheets is increasing.
- the barium titanate sheet of the present invention by using the laminated polyester film of the present invention having the layer X and the layer Y, after use in the process of producing the barium titanate sheet, the barium titanate sheet of the present invention
- the barium titanate sheet of the present invention By removing the layer X and the layer Y from the laminated polyester film, a polyester film with high purity can be obtained and reused, making it possible to greatly contribute to the reduction of the environmental load.
- the method for producing the laminated polyester film of the present invention is described below, but the present invention is not limited to the laminated polyester film obtained by this method.
- the polyester film of the laminated polyester film of the present invention uses a method (melt casting method) in which dried raw materials are heated and melted in an extruder as necessary, and extruded from a die onto a cooled cast drum to be processed into a sheet. be able to. It is preferable that the sheet is adhered and solidified by static electricity on a drum cooled to a surface temperature of 20° C. or more and 60° C. or less to produce an unstretched sheet.
- the temperature of the casting drum is more preferably 20°C or higher and 40°C or lower, and still more preferably 20°C or higher and 30°C or lower.
- the unstretched sheet is 3.6 times or more in the longitudinal direction (MD) of the film and 3.9 times or more in the width direction (TD) of the film at a temperature T1n (° C.) that satisfies the following formula (i). , preferably biaxially stretched at an area magnification of 14.0 times or more and 20.0 times or less.
- the draw ratio in the film width direction is preferably 4.0 times or more, more preferably 4.3 times or more and 5.0 times or less.
- Tg Glass transition temperature of polyester film (°C)
- a method for stretching the film in the longitudinal direction a method using a speed difference between rolls is preferably used. At this time, it is also a preferred embodiment to divide the film into a plurality of sections while fixing the film with nip rolls so that the film does not slip.
- the biaxially stretched film is heat-set for 1 second or more and 30 seconds or less at a temperature (Th0 (° C.)) that satisfies the following formula (ii), uniformly slowly cooled, and then cooled to room temperature. It is preferred to obtain a polyester film by. (ii) Tmf-35 (°C) ⁇ Th0 (°C) ⁇ Tmf (°C) Tmf: Melting point of film (°C)
- the polyester film of the laminated polyester film of the present invention in addition to the production method described above, it is preferable that particles are contained in the film so that conditions 3 and 7 are within the ranges described above.
- the particles to be contained spherical particles having a uniform particle size distribution, such as colloidal silica particles, crosslinked polystyrene particles, and calcium carbonate particles, are preferably used.
- the particle content is preferably 0.01% by mass or more and 3.0% by mass or less with respect to the mass of the polyester film.
- the particle size of the particles is preferably 50 nm or more and 5000 nm or less.
- the particle diameter of the particles is preferably 100 nm or more and 5000 nm or less, particularly preferably 300 nm or more and 2000 nm or less.
- the particle diameter of the particles is preferably 50 nm or more and 1000 nm or less, particularly preferably 50 nm or more and 400 nm or less.
- the sheet extruded on the cast drum preferably has a laminated structure of two or more layers, and the layer constituting the A side (A layer) , and an intermediate layer (C layer) between the layers (B layer) constituting the B surface.
- an intermediate layer (C layer) is provided between the A layer and the B layer, it is possible to use raw materials recycled by the method described below for the C layer, which is preferable.
- the present invention is not limited to films obtained by such methods.
- a method of dissolving the resin forming the layer X in water and coating it on the polyester film of the present invention can be preferably used.
- a coating method general coating methods such as gravure coating, Meyer bar coating, air knife coating, and doctor knife coating can be used.
- the surface layer of the polyester film after being uniaxially stretched in the longitudinal direction is coated with a resin that is the source of the layer X, and the polyester film is stretched in the width direction while the layer X is formed.
- An in-line coating method for forming a film can be preferably used.
- the thickness of the layer X is preferably 10 nm or more and 500 nm or less.
- the thickness is 10 nm or more, the layer X can exhibit sufficient water absorbency, and good removability can be achieved.
- by setting the thickness to 500 nm or less it is possible to suppress the occurrence of blocking and the deterioration of handling properties. From the same point of view, it is more preferably 50 nm or more and 200 nm or less.
- the layer Y may be provided simultaneously with the layer X, or may be provided separately. When they are provided at the same time, a method of applying two layers at the same time using a die or the like, or a method of applying a coating agent in which the components of the layer X and the components of the layer Y are mixed in advance can be used. In order to improve the lamination accuracy of the layers X and Y, it is preferable to provide the layers X and Y separately when the layers X and Y are provided.
- a general coating method such as gravure coating, Meyer bar coating, air knife coating, doctor knife coating, etc., using a coating liquid in which the components of layer Y are dissolved in the laminated polyester film containing layer X obtained by the above method. can be applied using
- the thickness of the layer Y is preferably 10 nm or more and 1000 nm or less. When the thickness is 10 nm or more, the function of the layer Y can be sufficiently exhibited, and when the thickness is 1000 nm or less, the moisture permeability of the layer Y can be sufficiently exhibited,
- the laminated polyester film containing the layer X and the layer Y of the present invention is unwound, and hot water is supplied to the surface of the unwound laminated polyester film. It is preferable to perform a step of peeling the surface laminated portion (layer X, layer Y) from the laminated polyester film and a step of winding the peeled polyester film.
- the temperature of hot water is preferably 50°C or higher and 120°C or lower. By setting the temperature to 50° C. or higher, a sufficient washability can be obtained.
- the temperature By setting the temperature to 120° C. or less, it is possible to suppress the occurrence of a case where the glass transition temperature of the polyester film is exceeded and the film cannot be transported.
- the time that the surface of the laminated polyester film is in contact with water is preferably 5 seconds or longer, more preferably 10 seconds or longer, and still more preferably 30 seconds or longer and 600 seconds or shorter.
- the step of applying hot water to the surface of the unwound laminated polyester film includes a method of covering the entire laminated polyester film in a water tank, and a method of pressurizing heated water and spraying it onto the laminated polyester film.
- the speed at which the laminated polyester film is conveyed is 5 m/min or more, preferably 10 m/min or more, more preferably 20 m/min or more and 100 m/min or less.
- the tension is preferably 5 N/m or more and 100 N/m or less, more preferably 20 N/m or more and 80 N/m or less, and still more preferably 30 N/m or more and 50 N/m or less.
- the tension is preferably 5 N/m or more and 100 N/m or less, more preferably 20 N/m or more and 80 N/m or less, and still more preferably 30 N/m or more and 50 N/m or less.
- the film roll from which layer X and layer Y have been removed by the above-described method is introduced into a crusher having a rotating blade driven by a motor and pulverized, it is introduced into an extruder and melted, extruded into a strand, It is preferable to adopt a method of obtaining recycled raw materials by cutting into pellets.
- the melting temperature is preferably 250° C. or higher and 300° C. or lower in order to keep the intrinsic viscosity of the recycled raw material in a preferable range.
- the screw which an extruder has may be single-screw or twin-screw.
- Films from which layer X and layer Y have been removed may contain particles themselves or may contain residues from the removal of layer X and layer Y.
- the extruder is preferably a twin screw.
- the recycled raw material thus obtained can be used as the raw material for the A layer, the B layer, and the C layer.
- the obtained recycled raw material preferably contains 0.0001% by mass or more and 0.3% by mass or less of components other than polyester. If the amount of components other than polyester exceeds 0.3% by mass, a large amount of foreign matter is generated when a film is formed using recycled raw materials depending on the manufacturing apparatus, making it difficult to obtain desired properties. is used in the layer A or layer B of the laminated film of the present invention, the surface properties of the layer A or layer B may not be satisfied. When trying to reduce the amount of impurities so that the polyester component is less than 0.0001% by mass, the damage to the substrate film in the step of removing layer X and layer Y increases, and it becomes difficult to obtain recycled polyester. There is
- the recycled raw material may be used in any of the A layer, the B layer, and the C layer, but it is particularly preferable to use it in the C layer. Since the recycled raw material may contain particles contained in the laminated film as a component other than the polyester, when the recycled raw material is used for the A layer or the B layer, the surface properties of the A layer or the B layer may be affected. On the other hand, when it is used for the C layer, which is an intermediate layer between the A layer and the B layer, since the C layer does not have a surface, the surface properties are not impaired even when a recycled raw material is used, which is preferable.
- the layer Y is provided and used as a release film for the process or other functional performance layer film. Furthermore, layer X and layer Y are washed with water and removed to obtain a polyester film of high purity. Therefore, the obtained polyester film can be reused as it is, or the film can be remelted into chips, used as a recycled raw material for film production, and reused as a film.
- the recycled raw material has an intrinsic viscosity (IV) of 0.5 or more and 0.7 or less, particularly preferably 0.55 or more and 0.65 or less, from the viewpoint of film-forming properties.
- each layer of the laminated film is obtained by the following method. A cross section of the film is cut out with a microtome in a direction parallel to the width direction of the film. The cross section is observed with a scanning electron microscope at a magnification of 5000 times to measure the thickness of each laminated layer.
- Amount of terminal carboxyl groups The amount of terminal carboxyl groups (the amount of COOH terminal groups) is determined by the method described in International Publication No. 2010/103945.
- a time-of-flight secondary ion mass spectroscopy (TOF-SIMS) spectrum and a Fourier transform infrared spectroscopy (FT-IR) spectrum of the layer X are measured to analyze the presence or absence of a polyvinyl alcohol skeleton or the like.
- TOF-SIMS measurement conditions A TOF-SIMS spectrum is measured for the layer X surface using the following equipment. Apparatus: TOF. manufactured by ION-TOF.
- Apparatus Spectrum 100 manufactured by PerkinElmer Light source: special ceramics Detector: DTGS Resolution: 4 cm -1 Accumulation times: 256 Measurement wavenumber range: 4,000 to 680 cm -1 Measurement mode: Attenuated total reflection (ATR) method Attachment: Single reflection type ATR crystal (material: diamond/ZnSe).
- Copolymerization amount of layer X (mol%) The amount of copolymerization (mol %) is determined from the peak area of the carbon signal of the introduced modifying group in the 13 C-NMR spectrum and DEPT135 spectrum using the following equipment.
- the static contact angle was measured after the sample had been allowed to stand for 12 hours in an environment of 25°C in advance. , the ⁇ /2 method is used to calculate the static contact angle. Measurements are performed five times at different locations, and the average value of the static contact angles is used to calculate the dispersion component, polar component, and hydrogen bond component of the surface free energy of the layer X.
- H. Water contact angle (°) It is measured by the following method using a contact angle meter DM501 manufactured by Kyowa Interface Science Co., Ltd. and attached analysis software FAMAS. In an atmosphere of 23° C. and 65% RH, a moving image of the water droplet shape is taken for 20 seconds, with the time that the water droplet comes into contact with the sample surface as 0 seconds.
- the sample surface in contact with the water droplet is layer X
- the average value of the contact angles obtained from the water droplet shape after 1 second and the water droplet shape after 20 seconds is calculated.
- HX(20) and HY(1) and HY(20) when the sample surface in contact with the water droplet is layer Y.
- the crystallinity of the layer X Calculate In the calculation of c and d above, if there are two or more maximum absorbance values in the corresponding wavenumber range, c and d are calculated using the larger absorbance value. If there are three or more minimum absorbance values between wavenumbers of 1100 cm ⁇ 1 and 1200 cm ⁇ 1 , two minimum absorbance values are used to determine the baseline.
- the layer X side surface of the laminated polyester film the layer X may be the outermost surface, or the layer Y may be the outermost surface.
- Apparatus 670-IR (FT-IR manufactured by Varian)
- Light source Grover detector: DLatgs (deuterated L-alanine doped triglycine sulfate) Resolution: 4 cm -1
- Measurement method Attenuated total reflection method
- Accessory device Single reflection type ATR measurement accessory device (The Seagull TM ) ATR crystal; germanium incident angle: 60° Polarized: None
- the surface roughness Sa (B) of is measured using a non-contact surface profile measurement system "VertScan” (registered trademark) R550H-M100 manufactured by Ryoka Systems Co., Ltd. under the following conditions, and based on the following formula, ⁇ Sa is calculated. For the surface roughness, an arithmetic mean value of five measurements is adopted.
- ⁇ Sa Sa (B) - Sa (A) (Measurement condition)
- ⁇ Measurement mode WAVE mode.
- Objective lens 50x.
- Measurement area 187 x 139 ⁇ m.
- the polyester film was pulverized, dried at 180 ° C. for 2 hours, put into an extruder, melt-extruded at 280 ° C., and cooled to 25 ° C. On a cast drum. The sheet obtained is molded into a sheet, and the obtained sheet is subjected to the above-mentioned B.C. Measure the intrinsic viscosity by the method of The smaller the difference ( ⁇ IV) between the intrinsic viscosity IV (R) and the intrinsic viscosity IV of the polyester film, the better.
- RzjisB, RzjisX (nm) The three-dimensional surface roughness of the sample was measured using the following equipment and conditions, and the ten-point average roughness Rzjis of the surface roughness was calculated using analysis software. Let RzjisX (nm).
- Apparatus "surf-corder ET-4000A" manufactured by Kosaka Laboratory Analysis software: i-Face model TDA31 Stylus tip radius: 0.2 ⁇ m Measurement field of view: X direction: 380 ⁇ m Pitch: 1 ⁇ m Y direction: 280 ⁇ m Pitch: 5 ⁇ m Needle pressure: 50 ⁇ N Measurement speed: 0.1mm/s Cut-off value: low-pass; 0.8 mm, high-pass; none Leveling: All-pass filter: Gaussian filter (2D) Magnification: 100,000 times.
- a predetermined amount of sample is dissolved in orthochlorophenol at 160° C. for 40 minutes and filtered through a glass filter (3G3). After filtration, the residue is washed with dichloromethane, dried with hot air at 130° C. for 10 hours, weighed, and the ratio of the mass of the residue to the sample before dissolution is calculated (% by mass).
- a laminated polyester film in which the layer X and the layer Y are laminated is obtained by applying by a gravure coating method. Furthermore, the laminated polyester film in which the layer X and the layer Y thus prepared are laminated is used as a release film, and the surface of the layer Y opposite to the surface in contact with the layer X is coated as a release material, which will be described later. Dielectric paste is applied by a die coating method so as to have a thickness of 1.0 ⁇ m after drying. After that, from the obtained laminate, the release film roll for the process is obtained by releasing the dielectric and peeling off the material to be released. The film roll is introduced into a water washing device with an unwinding and winding device and washed with water at 60° C. for 2 minutes under a tension of 100 N/m to remove layer X and layer Y. Regarding the polyester film after layer X and layer Y have been removed, the above M.I. The removability of layer X and layer Y is evaluated.
- PET-1 Terephthalic acid and ethylene glycol were polymerized by a conventional method using antimony trioxide and magnesium acetate tetrahydrate as catalysts to obtain melt-polymerized PET.
- the resulting melt-polymerized PET had a glass transition temperature of 81° C., a melting point of 255° C., an intrinsic viscosity of 0.65, and a terminal carboxyl group content of 20 eq. /t.
- PEN Dimethyl 2,6-naphthalenedicarboxylate and ethylene glycol were transesterified using manganese acetate as a catalyst. After completion of the transesterification reaction, PEN was obtained by a conventional method using antimony trioxide as a catalyst. Further, during the polymerization, the content of ⁇ crystal type alumina particles having a particle size of 0.1 ⁇ m was added so as to be 0.1%. The resulting PEN had a glass transition temperature of 124° C., a melting point of 265° C., an intrinsic viscosity of 0.62, and a terminal carboxyl group content of 25 eq. /t.
- coating agent B 100 parts by mass of a condensation reaction type silicone resin release agent (product name SRX290 manufactured by Dow Toray Industries, Inc.), 6 parts by mass of a curing agent (product name SRX242C manufactured by Dow Toray Industries, Inc.), and toluene. The solvent was adjusted to have a solid content of 1.5% by mass, and a coating agent B was obtained.
- UV curable silicone resin release agent manufactured by JNC Co., Ltd., trade name FM-7721
- 1,9-nonanediol diacrylate manufactured by Osaka Organic Chemical Industry Co., Ltd., trade name “Viscoat” (registered trademark) #260
- a photopolymerization initiator manufactured by IGM Resins under the trade name "OMNIRAD” (registered trademark) 184
- toluene as a solvent to obtain a solid content of 1.5% by mass.
- a coating material C was obtained by adjusting as follows.
- PVA having a degree of saponification of 88, an average degree of polymerization of 500, and a copolymerization amount of sodium sulfonate of 0.1 mol% was prepared with reference to Japanese Patent Application Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent D.
- coating agent E PVA having a degree of saponification of 88, an average degree of polymerization of 500, and a copolymerization amount of sodium sulfonate of 0.5 mol% was prepared with reference to Japanese Patent Application Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating material E.
- coating agent F PVA having a degree of saponification of 88, an average degree of polymerization of 500, and a copolymerization amount of sodium sulfonate of 1 mol% was prepared with reference to Japanese Patent Application Laid-Open No. 9-227627. The PVA was dissolved in water to a concentration of 4% by mass to obtain coating agent F.
- PVA having a degree of saponification of 88, an average degree of polymerization of 400, and a copolymerization amount of sodium sulfonate of 3 mol% was prepared with reference to Japanese Patent Application Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent G.
- Coating Agent H PVA having a degree of saponification of 88, an average degree of polymerization of 300, and a copolymerization amount of sodium sulfonate of 5 mol% was prepared with reference to JP-A-9-227627. The PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent H.
- Coating Agent I PVA having a degree of saponification of 88, an average degree of polymerization of 1000, and a copolymerization amount of sodium sulfonate of 1 mol% was prepared with reference to JP-A-9-227627. The PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent I.
- PVA having a degree of saponification of 88, an average degree of polymerization of 300, and a copolymerization amount of sodium sulfonate of 1 mol% was prepared with reference to Japanese Patent Application Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating material J.
- PVA having a degree of saponification of 88, an average degree of polymerization of 1000, and a copolymerization amount of sodium carboxylate of 1 mol% was prepared with reference to JP-A-2008-291120.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent L.
- Coating Agent M PVA having a degree of saponification of 88, an average degree of polymerization of 450, and a copolymerization amount of 1,2-ethanediol of 6 mol% was prepared with reference to JP-A-2004-285143. The PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent M.
- PVA having a degree of saponification of 98, an average degree of polymerization of 500, and a copolymerization amount of sodium sulfonate of 1 mol% was prepared with reference to Japanese Patent Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating material N.
- PVA having a degree of saponification of 88, an average degree of polymerization of 2500, and a copolymerization amount of sodium sulfonate of 1 mol% was prepared with reference to Japanese Patent Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent O.
- Adhesive Q After charging 97 parts by mass of butyl acrylate, 3 parts by mass of acrylic acid, 0.2 parts by mass of azobisisobutyronitrile as a polymerization initiator, and 233 parts by mass of ethyl acetate, nitrogen gas is flowed and the mixture is stirred. Nitrogen substitution was performed for about 1 hour. After that, the flask was heated to 60° C. and reacted for 7 hours to obtain an acrylic polymer having a weight average molecular weight (Mw) of 1,100,000.
- PVA having a degree of saponification of 88, an average degree of polymerization of 300, and a copolymerization amount of 1,2-ethanediol of 10 mol% was prepared with reference to Japanese Patent Application Laid-Open No. 9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating agent R.
- PVA having a degree of saponification of 88, an average degree of polymerization of 200, and a copolymerization amount of sodium sulfonate of 3 mol% was prepared with reference to JP-A-9-227627.
- the PVA was dissolved in water to a concentration of 4% by mass to obtain a coating material S.
- Example 1 80 parts by mass of PET-1 and 20 parts by mass of MB-A are mixed as raw materials for the A layer and the B layer, vacuum dried at 160 ° C. for 2 hours, put into an extruder, melted at 280 ° C., It was extruded through a die onto a casting drum having a surface temperature of 25°C to produce an unstretched sheet. Subsequently, the sheet was preheated with a heated roll group, stretched 3.8 times in the longitudinal direction (MD direction) at a temperature of 90 ° C., and cooled with a roll group at a temperature of 25 ° C. to obtain a uniaxially stretched film.
- MD direction longitudinal direction
- the coating material D was applied by a bar coating method so that the coating thickness after drying was 100 nm, and then the film was held at both ends with clips and heated to 100 ° C. in the tenter. It was stretched 4.3 times in the width direction (TD direction) perpendicular to the longitudinal direction in the heating zone of . Subsequently, heat setting was performed at a temperature of 230° C. for 10 seconds in a heat treatment zone in the tenter. Then, after uniformly slow cooling in the cooling zone, the film was taken up to obtain a laminated polyester film in which the layer X was laminated.
- coating agent A On the surface of layer X of the obtained laminated polyester film opposite to the surface in contact with the polyester film, coating agent A was applied as layer Y so that the thickness after drying was 100 nm by gravure coating, and the layer was laminated. A polyester film was obtained.
- Dielectric paste was applied to the obtained laminated polyester film as a release material by a die coating method so that the thickness after drying was 1.0 ⁇ m, and 15 seconds after the application, the temperature was 100° C. and the wind speed was 5 m. Drying was performed for 2 minutes in an oven at 1/sec. Thereafter, the dielectric (releasable material) was released from the obtained laminate, and a film roll was obtained by winding up the laminated polyester film from which the releasable material was peeled off. The film roll was introduced into a washing device with an unwinding and winding device, washed with water at 100°C for 2 minutes under a tension of 30 N/m, and the polyester film from which layer X and layer Y were removed was collected. .
- Example 2-7 As the layer X, the coating agent E in Example 2, the coating agent F in Example 3, the coating agent G in Example 4, the coating agent H in Example 5, the coating agent I in Example 6, and the coating agent in Example 7 A laminated polyester film was produced in the same manner as in Example 1 except that J was used, and the release material was laminated and then peeled off, and then the layers X and Y were removed, and the polyester film was reused.
- Example 8 A laminated polyester film was prepared in the same manner as in Example 3 except that the thickness of layer X was changed as shown in the table, and the release material was laminated and then peeled off, and then layer X and layer Y were removed. and reused the polyester film.
- Example 10 A laminated polyester film was produced in the same manner as in Example 3 except that the polyester raw material used was changed to PEN, and the release material was laminated and then peeled off, and then the layers X and Y were removed, and the polyester film reused.
- Example 11 and 12 A laminated polyester film was prepared in the same manner as in Example 3 except that the thickness of layer Y was changed as shown in the table, and the release material was laminated and then peeled off, and then layer X and layer Y were removed. and reused the polyester film. In addition, Q. In the evaluation of the removability of layers X and Y after wet heat treatment, evaluation was performed by changing the thickness of layer Y as shown in the table.
- Example 13 A laminated polyester film was prepared in the same manner as in Example 3 except that the coating agent B was used as the layer Y, and the release material was laminated and then peeled off, and then the layers X and Y were removed, and the polyester film reused. In addition, Q. In the evaluation of the removability of Layer X and Layer Y after wet heat treatment, Coating B instead of Coating A was used as Layer Y for evaluation.
- Example 14 A laminated polyester film was prepared in the same manner as in Example 3, except that coating material C was used as layer Y and UV irradiation was performed at an integrated light amount of 200 mJ / cm 2 in an atmosphere with an oxygen concentration of 0.1% by volume after drying. After the release material was laminated, it was peeled off, and then the layers X and Y were removed, and the polyester film was reused. In addition, Q. In the evaluation of the removability of layer X and layer Y after wet heat treatment, as layer Y, coating material C was used instead of coating material A, and after drying, the cumulative amount of light was 200 mJ / in an atmosphere with an oxygen concentration of 0.1% by volume. A layer Y was laminated with UV irradiation at cm 2 and evaluated.
- Example 15-17 A laminated polyester film was prepared in the same manner as in Example 1 except that the coating agent K was used as the layer X in Example 15, the coating agent L was used in Example 16, and the coating agent M was used in Example 17. After laminating the release material, it was peeled off, and then the layer X and the layer Y were removed, and the polyester film was reused.
- Example 19 30 parts by mass of PET-1 and 20 parts by mass of MB-B are mixed as raw materials for the sides A and B, vacuum-dried at 160°C for 2 hours, put into an extruder, and melted at 280°C. It was extruded through a die onto a casting drum having a surface temperature of 25°C to produce an unstretched sheet. Subsequently, the sheet was preheated with a heated roll group, stretched 3.8 times in the longitudinal direction (MD direction) at a temperature of 90 ° C., and cooled with a roll group at a temperature of 25 ° C. to obtain a uniaxially stretched film.
- MD direction longitudinal direction
- the coating material F was applied by a bar coating method so that the coating thickness after drying and stretching was 100 nm, and then the both ends of the film were held with clips.
- the film was stretched 4.3 times in the width direction (TD direction) perpendicular to the longitudinal direction in a heating zone at a temperature of 100°C.
- heat setting was performed at a temperature of 230° C. for 10 seconds in a heat treatment zone in the tenter.
- the film was wound into a roll to obtain a laminated polyester film in which the layer X was laminated.
- a layer Y having a thickness of 0.1 ⁇ m is applied to the upper surface of the layer X (the surface opposite to the surface where the layer X contacts the polyester film).
- a laminated polyester film in which layer X and layer Y were laminated was obtained.
- a dielectric The body paste was applied by a die coating method so that the thickness after drying was 1.0 ⁇ m.
- a release film roll for a process was obtained in which the dielectric was released and the material to be released was peeled off. The film roll was introduced into a water washing device with an unwinding and winding device and washed with water at 60° C. for 2 minutes under a tension of 100 N/m to remove layer X and layer Y.
- Example 20 A laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, and a release film were obtained in the same manner as in Example 19 except that the thickness of layer X was as shown in the table. Each characteristic is shown in the table.
- Example 21 95 parts by mass of PET-1 and 5 parts by mass of MB-D were mixed as the raw material for the A side and vacuum-dried at 160 ° C. for 2 hours, and 50 parts by mass of PET-1 and MB- 50 parts by mass of B are mixed, the raw materials vacuum dried at 160 ° C. for 2 hours are put into separate extruders, melted at 280 ° C., and passed through a confluence device to determine the thickness of the layer (A layer) constituting the A side. After lamination so that the thickness of the layer constituting the B side (B layer) was 5/95, it was extruded through a die onto a casting drum having a surface temperature of 25° C. to prepare an unstretched sheet.
- the sheet was preheated with a heated roll group, stretched 3.8 times in the longitudinal direction (MD direction) at a temperature of 90 ° C., and cooled with a roll group at a temperature of 25 ° C. to obtain a uniaxially stretched film.
- the coating material F was applied by a bar coating method so that the coating thickness after drying and stretching was 100 nm, and then the both ends of the film were held with clips.
- the film was stretched 4.3 times in the width direction (TD direction) perpendicular to the longitudinal direction in a heating zone at a temperature of 100°C.
- heat setting was performed at a temperature of 230° C. for 10 seconds in a heat treatment zone within the tenter. Then, after uniformly slow cooling in a cooling zone, the film was wound into a roll to obtain a laminated polyester film in which the layer X was laminated.
- a layer Y having a thickness of 0.1 ⁇ m is formed on the surface opposite to the surface in contact with the polyester film of the layer X of the laminated polyester film in which the layer X is laminated.
- Coating agent A was applied by a gravure coating method to obtain a laminated polyester film in which layer X and layer Y were laminated.
- Example 22 A laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, and a release film were obtained in the same manner as in Example 21, except that the thickness of layer X was changed as shown in the table. rice field. Each characteristic is shown in the table.
- the raw material for side A is a mixture of 95 parts by mass of PET-1 and 5 parts by mass of MB-D
- the raw material for side B is a mixture of 10 parts by mass of PET-1 and 90 parts by mass of MB-C.
- a laminated polyester film in which the layer X was laminated, a polyester film in which the layer X and the layer Y were laminated, and a release film were obtained in the same manner as in Example 22 except that the above was carried out. Each characteristic is shown in the table.
- Example 24 adhesive Q was used as the material to be released, and was applied by a die coating method so that the thickness after drying was 10 ⁇ m. After that, from the obtained laminate, the pressure-sensitive adhesive Q was released, and a release film roll for a process in which the material to be released was peeled off was obtained. The film roll was introduced into a water washing device with an unwinding and winding device and washed with water at 60° C. for 2 minutes under a tension of 100 N/m to remove layer X and layer Y.
- Example 25 95 parts by mass of PET-1 and 5 parts by mass of MB-D were mixed as the raw material for the A side and vacuum-dried at 160 ° C. for 2 hours, and 50 parts by mass of PET-1 and MB- 50 parts by mass of B are mixed and vacuum-dried at 160 ° C. for 2 hours, and the intermediate layer (C layer) between the layer (A layer) constituting the A side and the layer (B layer) constituting the B side.
- PET-1 was vacuum-dried at 160°C for 2 hours.
- the raw materials were put into separate extruders, melted at 280°C, and laminated in the order of A layer/C layer/B layer through a confluence device.
- each layer had a thickness of 5/90/5
- it was extruded through a die onto a casting drum having a surface temperature of 25° C. to prepare an unstretched sheet.
- the sheet was preheated with a heated roll group, stretched 3.8 times in the longitudinal direction (MD direction) at a temperature of 90 ° C., and cooled with a roll group at a temperature of 25 ° C. to obtain a uniaxially stretched film.
- the coating material F was applied by a bar coating method so that the coating thickness after drying and stretching was 100 nm, and then the film was held at both ends with clips at 100 ° C. in a tenter.
- the film was stretched 4.3 times in the width direction (TD direction) perpendicular to the longitudinal direction in a heating zone at a temperature of . Subsequently, heat setting was performed at a temperature of 230° C. for 10 seconds in a heat treatment zone in the tenter. Then, after uniformly slow cooling in a cooling zone, the film was wound into a roll to obtain a laminated polyester film in which the layer X was laminated.
- a layer Y having a thickness of 0.1 ⁇ m is formed on the surface opposite to the surface in contact with the polyester film of the layer X of the laminated polyester film in which the layer X is laminated.
- Coating agent A was applied by a gravure coating method to obtain a laminated polyester film in which layer X and layer Y were laminated.
- Example 26 A laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, and a release film were obtained in the same manner as in Example 21 except that coating agent M was used as layer X.
- the polyester film obtained in Example 21 from which the layer X and the layer Y were removed was cut, put into an extruder with a vent hole, and extruded at 280 ° C. while removing moisture while maintaining a pressure reduction of 1 kPa or less to pellet.
- Recycled raw material-1 was obtained by processing into a shape.
- the recycled raw material has a glass transition temperature of 81° C., a melting point of 255° C., an intrinsic viscosity of 0.58, and a terminal carboxyl group content of 28 eq. /t.
- the amount of components other than polyester contained in the recycled raw material was 0.47% by mass.
- Reference example 2 The polyester film obtained in Example 25 from which layer X and layer Y were removed was cut, put into an extruder with a vent hole, and extruded at 280 ° C. while removing moisture while maintaining a vacuum of 1 kPa or less to pellet.
- Recycled raw material-2 was obtained by processing into a shape.
- the recycled raw material has a glass transition temperature of 81° C., a melting point of 255° C., an intrinsic viscosity of 0.58, and a terminal carboxyl group content of 28 eq. /t.
- the amount of components other than polyester contained in the recycled raw material was 0.03% by mass.
- Example 27 95 parts by mass of PET-1 and 5 parts by mass of MB-D were mixed as the raw material for the A side and vacuum-dried at 160 ° C. for 2 hours, and 50 parts by mass of PET-1 and MB- 50 parts by mass of B are mixed and vacuum-dried at 160 ° C. for 2 hours, and the intermediate layer (C layer) between the layer (A layer) constituting the A side and the layer (B layer) constituting the B side.
- As a raw material 50 parts by mass of PET-1 and 50 parts by mass of the recycled raw material obtained in Reference Example 1 were mixed, and the raw material was vacuum-dried at 160 ° C. for 2 hours, and layer X was laminated in the same manner as in Example 25. Laminated polyester A film, a polyester film in which layer X and layer Y are laminated, and a release film were obtained.
- Example 28-30 A laminated polyester film was produced in the same manner as in Example 21, except that as layer X, coating agent K was used in Example 28, coating agent G was used in Example 29, and coating agent L was used in Example 30.
- Example 31 85 parts by mass of PET-1, 5 parts by mass of MB-D, and 10 parts by mass of the recycled raw material-1 obtained in Reference Example 1 were mixed as the raw material constituting the A side, and the raw material was vacuum-dried at 160 ° C. for 2 hours, B side. 50 parts by mass of PET-1 and 50 parts by mass of MB-B are mixed as a raw material constituting the , and the raw material is vacuum dried at 160 ° C. for 2 hours, and a layer constituting the A side (A layer) and a layer constituting the B side Layer X is laminated in the same manner as in Example 25, using a raw material obtained by vacuum-drying 100 parts by mass of PET-1 at 160 ° C. for 2 hours as a raw material for the intermediate layer (C layer) with (B layer). , a polyester film in which the layer X and the layer Y were laminated, and a release film were obtained.
- Example 32 85 parts by mass of PET-1, 5 parts by mass of MB-D, and 10 parts by mass of the recycled raw material-1 obtained in Reference Example 1 were mixed as the raw material constituting the A side, and the raw material was vacuum-dried at 160 ° C. for 2 hours, B side. 10 parts by mass of PET-1, 40 parts by mass of MB-B, and 10 parts by mass of the recycled raw material-1 obtained in Reference Example 1 were mixed as raw materials constituting the , and the raw material was vacuum-dried at 160 ° C. for 2 hours. 100 parts by mass of PET-1 was vacuum-dried at 160 ° C.
- a laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, and a release film were obtained in the same manner as in Example 25.
- Example 33 85 parts by mass of PET-1, 5 parts by mass of MB-D, and 10 parts by mass of the recycled raw material-1 obtained in Reference Example 1 were mixed as the raw material constituting the A side, and the raw material was vacuum-dried at 160 ° C. for 2 hours, B side. 10 parts by mass of PET-1, 40 parts by mass of MB-B, and 10 parts by mass of the recycled raw material-1 obtained in Reference Example 1 were mixed as raw materials constituting the , and the raw material was vacuum-dried at 160 ° C. for 2 hours.
- Example 34 85 parts by mass of PET-1, 5 parts by mass of MB-D, and 10 parts by mass of the recycled raw material-1 obtained in Reference Example 1 were mixed as the raw material constituting the A side, and the raw material was vacuum-dried at 160 ° C. for 2 hours, B side. 50 parts by mass of PET-1 and 50 parts by mass of MB-B are mixed as a raw material constituting the , and the raw material is vacuum dried at 160 ° C. for 2 hours, and a layer constituting the A side (A layer) and a layer constituting the B side Layer X is laminated in the same manner as in Example 25, using a raw material obtained by vacuum-drying 100 parts by mass of PET-1 at 160 ° C. for 2 hours as a raw material for the intermediate layer (C layer) with (B layer). , a polyester film in which the layer X and the layer Y were laminated, and a release film were obtained.
- Example 35 95 parts by mass of PET-1 and 5 parts by mass of MB-D were used as raw materials for forming the A and B surfaces, and in Example 36, PET was used as a raw material for forming the A and B surfaces.
- -1 30 parts by mass and MB-C 70 parts by mass were used in the same manner as in Example 19, a laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, a release film got
- Example 37 50 parts by mass of PET-1 and 50 parts by mass of MB-B were mixed as the raw material for the A side, and the raw material was vacuum dried at 160 ° C. for 2 hours, and 95 parts by mass of PET-1 and MB- A laminated polyester film in which layer X was laminated in the same manner as in Example 21, except that 5 parts by mass of D were mixed and vacuum dried at 160 ° C. for 2 hours, and a polyester film in which layer X and layer Y were laminated , to obtain a release film.
- Example 38 On one side (Side A) of a polyester film "Lumirror” (registered trademark) #50T60 manufactured by Toray Industries, Inc., coating agent F is applied by a gravure coating method so that the coating thickness after drying is 100 nm, and is formed into a roll shape. The film was taken up to obtain a laminated polyester film in which the layer X was laminated.
- a layer Y having a thickness of 0.1 ⁇ m is formed on the surface opposite to the surface in contact with the polyester film of the layer X of the laminated polyester film in which the layer X is laminated.
- Coating agent A was applied by a gravure coating method to obtain a laminated polyester film in which layer X and layer Y were laminated.
- the intrinsic viscosity after reuse was not measured.
- Example 39 A laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, and a release film were obtained in the same manner as in Example 21 except that coating agent R was used as a component of layer X.
- Example 40 80 parts by mass of PET-1 and 20 parts by mass of MB-A are mixed as raw materials for the A layer and the B layer, vacuum dried at 160 ° C. for 2 hours, put into an extruder, melted at 280 ° C., It was extruded through a die onto a casting drum having a surface temperature of 25°C to produce an unstretched sheet. Subsequently, the sheet was preheated with a heated roll group, stretched 3.5 times in the longitudinal direction (MD direction) at a temperature of 95 ° C., and cooled with a roll group at a temperature of 25 ° C. to obtain a uniaxially stretched film.
- MD direction longitudinal direction
- the coating agent S was applied by a bar coating method so that the coating thickness after drying was 100 nm, and then the film was held at both ends with clips and heated to 95 ° C. in the tenter. It was stretched 3.7 times in the width direction (TD direction) perpendicular to the longitudinal direction in the heating zone of . Subsequently, heat setting was performed at a temperature of 220° C. for 10 seconds in a heat treatment zone within the tenter. Then, after uniformly slow cooling in the cooling zone, the film was taken up to obtain a laminated polyester film in which the layer X was laminated.
- coating agent A On the surface of layer X of the obtained laminated polyester film opposite to the surface in contact with the polyester film, coating agent A was applied as layer Y so that the thickness after drying was 100 nm by gravure coating, and the layer was laminated. A polyester film was obtained.
- Dielectric paste was applied to the obtained laminated polyester film as a release material by a die coating method so that the thickness after drying was 1.0 ⁇ m, and 15 seconds after the application, the temperature was 100° C. and the wind speed was 5 m. Drying was performed for 2 minutes in an oven at 1/sec. Thereafter, the dielectric (releasable material) was released from the obtained laminate, and a film roll was obtained by winding up the laminated polyester film from which the releasable material was peeled off. The film roll was introduced into a washing device with an unwinding and winding device, washed with water at 100°C for 2 minutes under a tension of 30 N/m, and the polyester film from which layer X and layer Y were removed was collected. .
- Example 41 A laminated polyester film in which layer X was laminated, a polyester film in which layer X and layer Y were laminated, and a release film were obtained in the same manner as in Example 21, except that the transverse stretching temperature was as shown in the table.
- Example 42 95 parts by mass of PET-1 and 5 parts by mass of MB-D were mixed as the raw material for the A side and vacuum-dried at 160 ° C. for 2 hours, and 50 parts by mass of PET-1 and MB- 50 parts by mass of B are mixed, the raw materials vacuum dried at 160 ° C. for 2 hours are put into separate extruders, melted at 280 ° C., and passed through a confluence device to determine the thickness of the layer (A layer) constituting the A side. After lamination so that the thickness of the layer constituting the B side (B layer) was 5/95, it was extruded through a die onto a casting drum having a surface temperature of 25° C. to prepare an unstretched sheet.
- the sheet was preheated with a heated roll group, stretched 3.8 times in the longitudinal direction (MD direction) at a temperature of 90 ° C., and cooled with a roll group at a temperature of 25 ° C. to obtain a uniaxially stretched film.
- the obtained uniaxially stretched film was stretched 4.3 times in the width direction (TD direction) perpendicular to the longitudinal direction in a heating zone at a temperature of 100° C. in a tenter while holding both ends of the film with clips.
- heat setting was performed at a temperature of 230° C. for 10 seconds in a heat treatment zone in the tenter. Then, after uniformly slow cooling in a cooling zone, the film was wound into a roll to obtain a laminated polyester film in which the layer X was not laminated.
- a layer Y is coated on one side of the polyester film on which the layer X is not laminated by a gravure coating method using a coating agent D so that the thickness after drying is 0.1 ⁇ m as the layer Y, and the layer Y is laminated. got the film.
- a dielectric paste was applied as a release material by a die coating method so that the thickness after drying was 1.0 ⁇ m.
- a release film roll for a process was obtained in which the dielectric was released and the material to be released was peeled off.
- the film roll was introduced into a water washing device with an unwinding and winding device and washed with water at 60° C. for 2 minutes under a tension of 100 N/m to remove the layer Y.
- Q In addition, Q.
- Coating Agent D was used instead of Coating Agent A for Layer Y and evaluated.
- Comparative Example 1 in which the degree of saponification of PVA constituting the layer X is high, is inferior in removability of the layers X and Y because the polar component ⁇ X P and the hydrogen bonding component ⁇ X H of the surface free energy of the layer X are not within the preferable range. It was something. After that, the N.M. When the pulverized polyester film was melt-extruded according to the section, the layers X and Y remained unremoved and deteriorated in the extruder, making it impossible to form a sheet.
- Example 3 A laminated polyester film was produced in the same manner as in Example 42 except that the coating agent A was used as the layer Y, and a ceramic green sheet and an adhesive sheet were laminated as the release objects, respectively, and evaluated, and the ceramic green sheet was peeled off. After that, the layer Y was removed and the polyester film was reused.
- the layer Y Since the layer X was not included and the HY(1)-HY(20) (°) of the layer Y was not within a preferable range, the layer Y was inferior in removability. After that, the N.M. When the pulverized polyester film was melt-extruded according to the section, the layer Y could not be removed and remained, causing deterioration in the extruder and making it impossible to form a sheet.
- the laminated polyester film of the present invention has excellent solvent resistance during post-processing and excellent removability of layers other than the polyester film.
- a water-repellent material for the layer Y of the present invention it can be suitably used as a release film for the manufacturing process of a multilayer ceramic capacitor (MLCC) using a dielectric paste as a release material.
- MLCC multilayer ceramic capacitor
- the polyester film can be easily recovered from the release film after being used in the MLCC manufacturing process, the polyester film can be easily reused as a raw material for melt film formation.
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Abstract
Description
条件1:20≦γXP≦45
条件2:3.0≦γXH≦10
γXP(mN/m):層Xの表面自由エネルギーの極性成分
γXH(mN/m):層Xの表面自由エネルギーの水素結合成分
[II]前記層Xの厚みxa(nm)と、前記ポリエステルフィルムの層Xを有する面(A面)とは反対側の面(B面)側の表面の粗さRzjisB(nm)が以下の条件を満たす[I]に記載の積層ポリエステルフィルム。
条件3:1.0≦RzjisB/xa≦20.0
xa(nm):層Xの厚み
[III]前記層Xが以下の条件を満たす[I]または[II]に記載の積層ポリエステルフィルム。
条件4:20≦γXP≦30
条件5:6.0≦γXH≦10
[IV]以下の条件を満たす[II]または[III]に記載の積層ポリエステルフィルム。
条件6:1.5≦RzjisB/xa≦10.0
[V]前記層Xの厚みxa(nm)と、前記層Xの表面の粗さRzjisX(nm)が以下の条件を満たす[I]から[IV]のいずれかに記載の積層ポリエステルフィルム。
条件7:0.01≦RzjisX/xa≦3.0
[VI]前記層Xの厚みxaが10nm以上500nm以下である[I]から[V]のいずれかに記載の積層ポリエステルフィルム。
[VII]前記層Xの水の接触角HX(1)(°)とHX(20)(°)が以下の条件を満たす[I]から[VI]のいずれかに記載の積層ポリエステルフィルム。
条件8:5≦|HX(1)-HX(20)|≦60
HX(1)(°):層Xに水が接触してから1秒後の接触角
HX(20)(°):層Xに水が接触してから20秒後の接触角
[VIII]前記層Xがポリビニルアルコール骨格を有する樹脂を含む[I]から[VII]のいずれかに記載の積層ポリエステルフィルム。
[IX]前記層Xがスルホン酸塩変性ポリビニルアルコール骨格を有する樹脂を含む[VIII]に記載の積層ポリエステルフィルム。
[X]前記層Xの結晶化度が14%以上40%以下である[I]から[IX]のいずれかに記載の積層ポリエステルフィルム。
[XI]前記層Xの結晶化度が31%より大きく、40%以下である[X]に記載の積層ポリエステルフィルム。
[XII]前記層Xが重合度200より大きな樹脂を含む[I]から[XI]のいずれかに記載の積層ポリエステルフィルム。
[XIII]以下の条件を満たす層Y、層X、ポリエステルフィルムをこの順で有する[I]から[XII]のいずれかに記載の積層ポリエステルフィルム。
条件9:80≦HY(1)≦120
条件10:1≦|HY(1)-HY(20)|≦90
HY(1)(°):層Yに水が接触してから1秒後の接触角
HY(20)(°):層Yに水が接触してから20秒後の接触角
[XIV]前記層Yの表面の以下の方法で求められる溶剤耐久率が5%以上100%以下である[XIII]に記載の積層ポリエステルフィルム。
[溶剤耐久率の測定方法]
試験機:学振型試験機(JIS L 0849(2013)に記載の摩擦試験機II形)
摩擦子:綿布(金巾3号)にトルエン:エタノールの混合溶媒(質量比1:1)を含浸
荷重:1kg
回数:30往復
溶剤耐久率(%)=F(A)/F(B)×100
F(A):層Y表面の剥離力
F(B):溶剤含浸布擦過試験後の層Y表面の剥離力
[XV]前記層Yの表面自由エネルギーの水素結合成分γYHが1.5以上10以下である[XIII]または[XIV]に記載の積層ポリエステルフィルム。
[XVI]前記層Yの層Xと接する面とは反対面に被離型層を設け、層Yから被離型層を剥離する離型用途に用いられる[XIII]から[XV]のいずれかに記載の積層ポリエステルフィルム。
[XVII]層Yから被離型層を剥離した後、層Xと層Yが除去される用途に用いられる[XVI]に記載の積層ポリエステルフィルム。
[XVIII]層Xと層Yを除去した積層ポリエステルフィルムを再利用する用途に用いられる[XVII]に記載の積層ポリエステルフィルム。
[XIX]前記被離型層が、チタン酸バリウムを主成分とするセラミックグリーンシートである[XVI]から[XVIII]のいずれかに記載の積層ポリエステルフィルム。
[XX]少なくとも積層セラミックコンデンサ(MLCC)製造工程用の離型フィルムの一部として用いられる、[I]から[XIX]のいずれかに記載の積層ポリエステルフィルム。
[XXI]少なくとも一方の表層に以下の条件を満たす層Yを有する積層ポリエステルフィルム。
条件11:80≦HY(1)≦120
条件12:1≦|HY(1)-HY(20)|≦90
HY(1)(°):層Yに水が接触してから1秒後の接触角
HY(20)(°):層Yに水が接触してから20秒後の接触角
[XXII]前記ポリエステルフィルムが、前記ポリエステルフィルムの一方の表面であるA面を構成する層(A層)、もう一方の表面であるB面を構成する層(B層)と、表面を有しない層(C層)とを有する3層以上の積層構成を有しており、前記C層が再生ポリエステル原料を含む、[I]から[XXI]のいずれかに記載の積層ポリエステルフィルム。
[XXIII]少なくとも被離型層、層Y、ポリエステルフィルムをこの順で有する、[XXII]に記載の積層ポリエステルフィルムを用い、前記層Yから被離型層を剥離する工程と、被離型層を剥離したフィルムから層Yを除去する工程と、被離型層と層Yを除去したフィルムから再生原料を製造する工程を備え、さらにその再生原料を用いてフィルムを製膜する工程を備える、ポリエステルフィルムの製造方法。
[XXIV]ポリエステルフィルムの片面(A面)に、親水性樹脂を主たる構成成分とする層Xを積層したポリエステルフィルムであって、層Xの厚みxa(nm)と、前記ポリエステルフィルムの層Xを有する面(A面)とは反対側の面(B面)側の表面の粗さRzjisB(nm)が以下の条件を満たす積層ポリエステルフィルム。
条件13:0.2≦RzjisB/xa≦20.0
[XXV]ポリエステルフィルムと、層Xを有する積層ポリエステルフィルムであって、層Xはスルホン酸塩変性ポリビニルアルコール骨格を有する樹脂を含有し、前記スルホン酸塩変性ポリビニルアルコール骨格を有する樹脂の、スルホン酸塩による共重合量が0.1mol%以上10mol%以下であり、かつ層XをJIS K 6726(1994)に記載の方法で平均重合度を求めた場合、求められる平均重合度が200以上2400以下であり、かつ層XをJIS K 6726(1994)に記載の方法でけん化度を求めた場合、求められるけん化度が30以上97以下である、積層ポリエステルフィルム。
条件1:20≦γXP≦45
条件2:3.0≦γXH≦10
γXP(mN/m):層Xの表面自由エネルギーの極性成分
γXH(mN/m):層Xの表面自由エネルギーの水素結合成分
表面自由エネルギーの極性成分γXPおよび水素結合成分γXHは、積層ポリエステルフィルムの層X表面に対して、グリセロール、エチレングリコール、ホルムアミド、ジヨードメタンによる25℃での静的接触角を求め、各液体での静的接触角と、以下の非特許文献1に記載の、各液体の表面自由エネルギーの分散成分、極性成分、水素結合成分を、以下の非特許文献2に記載の「畑、北崎の拡張ホークスの式」に導入し、連立方程式を解くことにより求めた値を指す。測定方法の詳細は後述する。なお、層Xが露出されていない場合は、層Xの厚みがもとの層Xの厚みの30~70%の範囲になるまで研磨することで層Xを露出させて、層Xの表面自由エネルギーを求めるものとする。
非特許文献1:J.Panzer :J.Colloid Interface Sci.,44,142 (1973).。
非特許文献2:北崎寧昭、畑敏雄:日本接着協会紙,8,(3) 131(1972).
表面自由エネルギーの極性成分γXPおよび水素結合成分γXHを当該範囲とすることで、層X自体の内部相互作用や、層Xと積層ポリエステルフィルムとの相互作用が強くなり、耐溶剤性が向上するとともに、層Xは水を吸収しやすくすることができるため、水あるいは水溶液を用いて洗浄することで層Xを積層ポリエステルフィルムから容易に除去することができる。なお、ここでいう耐溶剤性とは、例えば、層Xの上に離型層を溶剤を含んだ塗剤によりコーティングしたり、さらにその上にセラミックグリーンシートを、溶剤を含んだスラリーで塗工した際においても、積層ポリエステルフィルムの平滑性や水洗性などが大きく悪化しないことをいう。同様の観点から、γXPは20mN/m以上30mN/m以下であることがより好ましく、22mN/m以上28mN/m以下であることがさらに好ましく、また、γXHは4.0mN/m以上10mN/m以下がより好ましく、6.0mN/m以上10mN/m以下であることがさらに好ましく、7mN/m以上9mN/m以下であるであることが特に好ましい。
ΔM=|(M2-M1)|/M1×100(%)
M1(g):50℃の水に10分間浸漬する前の樹脂質量
M2(g):50℃の水に10分間浸漬した後の樹脂質量。
条件:0.2≦RzjisB/xa≦20.0
なかでも、構成がよりシンプルで生産性が高くなる観点から、より好ましい一態様は、前記反対側の面(B面)側の表面が、前記ポリエステルフィルムの層Xを有する面(A面)とは反対側の面(B面)である態様である。また、水洗性を高める観点から層Xが上記した性能を満たす層Xである態様や、層Xが親水性を示す態様を、上記とは別のより好ましい態様として挙げることができる。なお、層Xが親水性を示すとは、実施例に記載の方法で測定した際に表面自由エネルギーの値が10mN/m以上であることをいう。層Xが露出されていない場合は、層Xの厚みがもとの層Xの厚みの30~70%の範囲になるまで研磨することで層Xを露出させて、層Xの表面自由エネルギーを求めるものとする。
条件7:0.01≦RzjisX/xa≦3.0
RzjisXは、層Xの表面の粗さRzjisXをいい、実施例に記載の方法で測定される10点平均粗さである。層Xとポリエステルフィルムによる2層構成の場合、RzjisXは層Xのポリエステルフィルムを接する面とは反対側の面の粗さを表す。層Xの粗さは、ポリエステルフィルムのA面の粗さの影響を受けるが、RzjisX/xaを3.0以下とすることで、層XがA面側を全体的に覆うことが可能となり、層Xの親水性を向上することができる。また、層Xに接して別の層を塗布する場合、該層の塗布性や機能を十分に発現することが可能となる。
80≦HY(1)≦120、1≦|HY(1)-HY(20)|≦90
HY(1)(°):層Yに水が接触してから1秒後の接触角
HY(20)(°):層Yに水が接触してから20秒後の接触角
水に対する接触角を制御しHY(1)を上述の範囲とした層Yを有することで、層Yの表面エネルギーを低下させることができる結果、層Yを有する積層ポリエステルフィルムを離型用フィルムとして用いることが可能となる。
ため好ましい。
(i)Tg(℃)≦T1n(℃)≦Tg+40(℃)
Tg:ポリエステルフィルムのガラス転移温度(℃)
フィルムの長手方向の延伸方法には、ロール間の速度差を用いる方法が好適に用いられる。この際、フィルムが滑らないようにニップロールでフィルムを固定しながら、複数区間にわけて延伸することも好ましい実施形態である。
(ii)Tmf-35(℃)≦Th0(℃)≦Tmf(℃)
Tmf:フィルムの融点(℃)
(ii)を満たす条件によって二軸延伸フィルムを得ることにより、フィルムに適度な配向を付与せしめ、離型用フィルムとして使用する場合のハンドリング性を向上させることができる。
A.各層の厚み
下記の方法にて、積層フィルム各層の厚みを求める。フィルム断面を、フィルム幅方向に平行な方向にミクロトームで切り出す。該断面を走査型電子顕微鏡で5000倍の倍率で観察し、積層各層の厚みを測定する。
オルトクロロフェノール100mlに本発明のポリエステルフィルムを溶解させ(溶液濃度C=1.2g/dl)、その溶液の25℃での粘度を、オストワルド粘度計を用いて測定する。また、同様に溶媒の粘度を測定する。得られた溶液粘度、溶媒粘度を用いて、下記(a)式により、[η](dl/g)を算出し、得られた値でもって固有粘度(IV)とする。
(a)ηsp/C=[η]+K[η]2・C
(ここで、ηsp=(溶液粘度(dl/g)/溶媒粘度(dl/g))―1、Kはハギンス定数(0.343とする)である。)。
末端カルボキシル基量(COOH末端基量)は国際公開第2010/103945号に記載の方法で求める。
層Xの飛行時間型二次イオン質量分析(TOF-SIMS)スペクトルおよびフーリエ変換赤外分光(FT-IR)スペクトルを測定し、ポリビニルアルコール骨格などの有無を分析する。
[TOF-SIMSの測定条件]
層X表面に対して、下記の装置を用い、TOF-SIMSスペクトルを測定する。
装置:ION-TOF社製TOF.SIMS5
1次イオン種:Bi3 ++
1次イオンの加速電圧:25kV
パルス幅:125ns
パンチング:なし(高空間分解能測定)
ラスターサイズ:40μm×40μm
スキャン数:64回
2次イオンの極性:正
帯電中和:あり
後段加速電圧:9.5kV。
[FT-IRの測定条件]
層X表面に対して、下記の装置を用い、FT-IRスペクトルを測定する。
装置:PerkinElmer社製Spectrum100
光源:特殊セラミックス
検出器:DTGS
分解能:4cm-1
積算回数:256回
測定波数範囲:4,000~680cm-1
測定モード:減衰全反射(ATR)法
付属装置:1回反射型ATRクリスタル(材質:ダイヤモンド/ZnSe)。
下記の装置を用い、13C-NMRスペクトル、DEPT135スペクトルにおいて、変性基導入の炭素シグナルのピーク面積から共重合量(mol%)を求める。
装置:ECZ-600R(株式会社JEOL RESONANCE社製)
測定方法:Single 13C pulse with inverse gated1H decoupling
測定周波数:150.9MHz
パルス幅:5.25μs
ロック溶媒:D2O
化学シフト基準:TSP(0ppm)
積算回数:10000回
測定温度:20℃
試料回転数:15Hz。
JIS K 6726(1994)ポリビニルアルコール試験方法に準じて、試料に含有される酢酸基量を水酸化ナトリウム水溶液による滴定法により定量し、算出する。
JIS K 6726(1994)ポリビニルアルコール試験方法に準じて、試料を水酸化ナトリウム水溶液にて完全にけん化した後、オストワルド粘度系を用いて25℃での粘度を測定し、極限粘度から平均重合度を算出する。
共和界面科学株式会社製の接触角計DM501および付属の解析ソフトFAMASを用いて以下の方法で測定する。層X表面に対して、標準液としてグリセロール、エチレングリコール、ホルムアミド、ジヨードメタンを用い、25℃での各液体の静的接触角を求め、各液体での静的接触角と、非特許文献1に記載の、各液体の表面自由エネルギーの分散成分、極性成分、水素結合成分を、非特許文献2に記載の「畑、北崎の拡張ホークスの式」に導入し、連立方程式を解くことにより、層Xの表面自由エネルギーの分散成分、極性成分、水素結合成分を求める。
標準液としてベンジルアルコール、エチレングリコール、ホルムアミド、ジヨードメタン用いる以外は、層Xの表面自由エネルギーと同様の方法で測定する。
共和界面科学株式会社製の接触角計DM501および付属の解析ソフトFAMASを用いて以下の方法で測定する。23℃、65%RHの雰囲気下、試料表面に水滴が接触した時間を0秒として、20秒間にわたって水滴形状の動画を撮影する。場所を変えて5回測定し、水滴が接する試料表面が層Xの場合、1秒後の水滴形状および20秒後の水滴形状から求められる接触角の平均値を算出し、それぞれHX(1)、HX(20)、水滴が接する試料表面が層Yの場合、同様にしてHY(1)、HY(20)として算出する。
以下の装置、条件により、FT-IRのATR法にて層X側の面の積層ポリエステルフィルムのスペクトルを測定した後、同様に測定した東レ株式会社製ポリエステルフィルム“ルミラー”(登録商標)#50T60のスペクトルを除算し、差スペクトルを得る。次いで、波数1400cm-1~1550cm-1の間の吸光度の最小値をベースラインとした場合の、波数1400cm-1~1450cm-1の間の吸光度の極大値の値をcとし、波数1100cm-1~1200cm-1の間の吸光度の2つの極小値を直線で結んだ線をベースラインとした場合の、波数1130cm-1~1150cm-1の間の吸光度の極大値の値をdとし、非特許文献(J. Polymer Science:Part A-1, Vol. 4, p679-698(1966))に記載の式「Per cent crystallinity = 92(d/c)-18」に基づき、層Xの結晶化度を算出する。なお、上記cおよびdの算出において、該当波数範囲に吸光度の極大値が2つ以上の場合は吸光度の大きな方の値を用いてcおよびdを算出する。また、波数1100cm-1~1200cm-1の間の吸光度の極小値が3つ以上の場合は、吸光度が小さい2つを用いてベースラインを決定する。また、積層ポリエステルフィルムの層X側の面は、層Xが最表面であっても、層Yが最表面であってもよい。
装置:670-IR(Varian製FT-IR)
光源:グローバー
検知器:DLatgs(重水素化L-アラニンドープ硫酸三グリシン)
分解能:4cm-1
積算回数:256回
測定方法:減衰全反射法
付属装置:1回反射型ATR測定付属装置(The SeagullTM)
ATR結晶;ゲルマニウム
入射角:60°
偏光:なし。
株式会社大栄科学精機製作所製の学振型試験機(JIS L 0849(2013)準拠)を用いて以下の方法で測定する。
[溶媒含浸布による擦過処理]
以下の試験機、摩擦子を用いて、フィルムの層Y表面を擦過処理する。
試験機:学振型試験機(JIS L 0849(2013)に記載の摩擦試験機II形)
摩擦子:綿布(金巾3号)にトルエン:エタノールの混合溶媒(質量比1:1)を含浸
荷重:1.0kg
回数:30往復
[剥離処理]
層Y表面の擦過処理を行った部分にポリエステル粘着テープ(日東電工株式会社製No.31B、幅19mm)を2.0kgのローラーで圧着させながら貼り合わせ、23℃、65%RHの雰囲気下で24時間静置した後、共和界面科学株式会社製の剥離試験機VPA-H200剥離試験機を用いて、剥離角度180°、剥離速度300mm/minにて試料表面とポリエステル粘着テープの間の剥離力を測定し、50mm幅に換算してF(B)を求める。擦過前の層Y表面の剥離力F(A)も同様の手法で測定し、以下の式に基づき、溶剤耐久率を測定する。
溶剤耐久率(%)=F(A)/F(B)×100
J.被離型物の剥離性
被離型物を積層した積層ポリエステルの被離型物の表面に、ポリエステル粘着テープ(日東電工株式会社製No.31B、幅19mm)を貼り付けて、共和界面科学株式会社製の剥離試験機VPA-H200を用いて、剥離角度180°、剥離速度300mm/minにて強度を測定し、50mm幅に換算する。
被離型物を積層した積層ポリエステルから、被離型物を剥離した後、JIS K 7136(2000)に基づき、日本電色株式会社製のヘイズメーターNDH-5000を用いて、ヘイズHz(B)を測定する。被離型物を積層前の積層ポリエステルのヘイズHz(A)についても同様の手法で測定し、以下の式に基づき、ΔHzを算出する。
ΔHz=Hz(B)-Hz(A)
L.表面粗さ変化を指標とした耐溶剤性
被離型物を積層する前の積層ポリエステルの表面粗さSa(A)および被離型物を積層した積層ポリエステルから、被離型物を剥離した後の表面粗さSa(B)を、株式会社菱化システム製の非接触表面形状計測システム“VertScan”(登録商標)R550H-M100を用いて、下記の条件で測定し、以下の式に基づき、ΔSaを算出する。表面粗さは、5回測定の算術平均値を採用する。
ΔSa=Sa(B)-Sa(A)
(測定条件)
・測定モード:WAVEモード。
・対物レンズ:50倍。
・0.5×Tubeレンズ。
・測定面積:187×139μm。
層X、層Yを除去して得られたポリエステルフィルムを用い、上記H.項に従って、1秒後に得られる水の接触角を測定し、以下の通り判定する。
B;80°以上90°未満、もしくは65°未満
C;90°以上95°未満。
層X、層Yを除去した後のポリエステルフィルムを粉砕し、180℃で2時間乾燥した後、押出機に投入し280℃で溶融押出した後、25℃に冷却したキャストドラム上でシート状に成形し、得られたシートを上述のB.の方法によって固有粘度を測定する。その固有粘度IV(R)と、ポリエステルフィルムの固有粘度IVの差(ΔIV)が小さいほど望ましい。
下記装置、条件にてサンプルの3次元表面粗さを測定し、解析ソフトを用いて表面粗さの十点平均粗さRzjisを算出し、場所を変えて10回測定しその平均値をもってRzjisB、RzjisX(nm)とする。
装置:小坂研究所製“surf-corder ET-4000A”
解析ソフト:i-Face model TDA31
触針先端半径:0.2μm
測定視野:X方向:380μm ピッチ:1μm
Y方向:280μm ピッチ:5μm
針圧:50μN
測定速度:0.1mm/s
カットオフ値:低域;0.8mm、高域;なし
レベリング:全域
フィルター:ガウシアンフィルタ(2D)
倍率:10万倍。
所定量の試料をオルトクロロフェノールで160℃、40分間で溶解し、ガラス濾過器(3G3)で濾過する。濾過後、残渣をジクロロメタンで洗浄し、130℃で10時間熱風乾燥したものを計量し、溶解前の試料に対する残渣質量の割合を(質量%)で計算する。
各実施例の方法により得られた層Xが積層された積層ポリエステルフィルムの残りを、ロール形状のまま防湿梱包材(長岡産業(株)製アルミチューブ)で包み、60℃相対湿度80%の雰囲気下で7日間静置する。その後、層Xが積層された積層ポリエステルフィルムを取り出し、層Xのポリエステルフィルムと接する面とは反対の面に、層Yとして厚みが0.1μmとなるように、後述する塗剤Aを用いてグラビアコート法にて塗布し、層Xと層Yが積層された積層ポリエステルフィルムを得る。さらに、このようにして作製した層Xと層Yが積層された積層ポリエステルフィルムを離型用フィルムとして用い、層Yの層Xと接する面とは反対の面に、被離型物として、後述する誘電体ペーストをダイコート法によって乾燥後の厚みが1.0μmとなるように塗布する。その後、得られた積層体から、誘電体を離型するとともに、被離型物を剥離した工程用の離型用フィルムロールを得る。該フィルムロールを、巻出しと巻き取り装置のある水洗装置に導入し、100N/mの張力下で、60℃の水で2分間洗浄し、層Xと層Yを除去する。層X、層Yを除去した後のポリエステルフィルムについて、上記M.層X、層Yの除去性の評価を行う。
A層、B層を構成する原料としてPET-1を80質量部、MB-Aを20質量部を混合し、160℃で2時間真空乾燥した後押出機に投入し、280℃で溶融させ、ダイを通して表面温度25℃のキャスティングドラム上に押し出し、未延伸シートを作製した。続いて該シートを加熱したロール群で予熱した後、90℃の温度で長手方向(MD方向)に3.8倍延伸を行った後、25℃の温度のロール群で冷却して一軸延伸フィルムを得た。得られた一軸延伸フィルムに、乾燥後の塗布厚みが100nmとなるようにバーコート法にて塗剤Dを塗布し、続いてフィルムのフィルム両端をクリップで把持しながらテンター内の100℃の温度の加熱ゾーンで長手方向に直角な幅方向(TD方向)に4.3倍延伸した。さらに引き続いて、テンター内の熱処理ゾーンで230℃の温度で10秒間の熱固定を施した。次いで、冷却ゾーンで均一に徐冷後、巻き取り、層Xが積層された積層ポリエステルフィルムを得た。
層Xとして、実施例2では塗剤E、実施例3では塗剤F、実施例4では塗剤G、実施例5では塗剤H、実施例6では塗剤I、実施例7では塗剤Jを用いた以外は、実施例1と同様に積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。
層Xの厚みを表に記載のとおりに変えた以外は、実施例3と同様にして積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。
使用するポリエステル原料をPENに変えた以外は、実施例3と同様にして積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。
層Yの厚みを表に記載のとおりに変えた以外は、実施例3と同様にして積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。なお、Q.湿熱処理後の層X、層Yの除去性の評価において、層Yの厚みを表に記載のとおりに変えて評価した。
層Yとして、塗剤Bを用いた以外は、実施例3と同様に積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。なお、Q.湿熱処理後の層X、層Yの除去性の評価において、層Yとして、塗剤Aの代わりに塗剤Bを用いて評価した。
層Yとして、塗剤Cを用いて、乾燥後に酸素濃度0.1体積%の雰囲気下で積算光量200mJ/cm2でUV照射した以外は、実施例3と同様に積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。なお、Q.湿熱処理後の層X、層Yの除去性の評価において、層Yとして、塗剤Aの代わりに塗剤Cを用いて、乾燥後に酸素濃度0.1体積%の雰囲気下で積算光量200mJ/cm2でUV照射して層Yを積層して評価した。
層Xとして、実施例15では塗剤Kを、実施例16では塗剤Lを、実施例17では塗剤Mを用いた以外は、実施例1と同様にして積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。
A面、B面を構成する原料としてPET-1を30質量部、MB-Bを20質量部を混合し、160℃で2時間真空乾燥した後押出機に投入し、280℃で溶融させ、ダイを通して表面温度25℃のキャスティングドラム上に押し出し、未延伸シートを作製した。続いて該シートを加熱したロール群で予熱した後、90℃の温度で長手方向(MD方向)に3.8倍延伸を行った後、25℃の温度のロール群で冷却して一軸延伸フィルムを得た。得られた一軸延伸フィルムのA面側に、乾燥・延伸後の塗布厚みが100nmとなるようにバーコート法にて塗剤Fを塗布し、続いてフィルムのフィルム両端をクリップで把持しながらテンター内の100℃の温度の加熱ゾーンで長手方向に直角な幅方向(TD方向)に4.3倍延伸した。さらに引き続いて、テンター内の熱処理ゾーンで230℃の温度で10秒間の熱固定を施した。次いで、冷却ゾーンで均一に徐冷後、ロール形状に巻き取り、層Xが積層された積層ポリエステルフィルムを得た。得られた層Xが積層された積層ポリエステルフィルムの一部を用い、層Xの上面(層Xがポリエステルフィルムと接する面とは反対の面)に、層Yとして厚みが0.1μmとなるように塗剤Aを用いてグラビアコート法にて塗布し、層Xと層Yが積層された積層ポリエステルフィルムを得た。さらに、このようにして作製した層Xと層Yが積層された積層ポリエステルフィルムを離型用フィルムとして用い、層Yの層Xと接する面とは反対の面に、被離型物として、誘電体ペーストをダイコート法によって乾燥後の厚みが1.0μmとなるように塗布した。その後、得られた積層体から、誘電体を離型するとともに、被離型物を剥離した工程用の離型用フィルムロールを得た。該フィルムロールを、巻出しと巻き取り装置のある水洗装置に導入し、100N/mの張力下で、60℃の水で2分間洗浄し、層Xと層Yを除去した。
層Xの厚みを表に記載の通りとした以外は、実施例19と同様に層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。各特性を表に示す。
A面を構成する原料としてPET-1 95質量部とMB-D 5質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料を、それぞれ別々の押出機に投入し、280℃で溶融させ、合流装置を通してA面を構成する層(A層)の厚みとB面を構成する層(B層)の厚みが5/95となるように積層させた後、ダイを通して表面温度25℃のキャスティングドラム上に押し出し、未延伸シートを作製した。続いて該シートを加熱したロール群で予熱した後、90℃の温度で長手方向(MD方向)に3.8倍延伸を行った後、25℃の温度のロール群で冷却して一軸延伸フィルムを得た。得られた一軸延伸フィルムのA面側に、乾燥・延伸後の塗布厚みが100nmとなるようにバーコート法にて塗剤Fを塗布し、続いてフィルムのフィルム両端をクリップで把持しながらテンター内の100℃の温度の加熱ゾーンで長手方向に直角な幅方向(TD方向)に4.3倍延伸した。さらに引き続いて、テンター内の熱処理ゾーンで230℃の温度で10秒間の熱固定を施した。次いで、冷却ゾーンで均一に徐冷後、ロール形状に巻き取り、層Xが積層された積層ポリエステルフィルムを得た。
層Xの厚みを表に記載の通りに変えた以外は、実施例21と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。各特性を表に示す。
A面を構成する原料としてPET-1 95質量部とMB-D 5質量部を混合した原料、B面を構成する原料としてPET-1 10質量部とMB-C 90質量部を混合した原料とした以外は実施例22と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。各特性を表に示す。
実施例21において、被離型物として粘着剤Qを用い、ダイコート法によって乾燥後の厚みが10μmとなるように塗布した。その後、得られた積層体から、粘着剤Qを離型するとともに、被離型物を剥離した工程用の離型用フィルムロールを得た。該フィルムロールを、巻出しと巻き取り装置のある水洗装置に導入し、100N/mの張力下で、60℃の水で2分間洗浄し、層Xと層Yを除去した。
A面を構成する原料としてPET-1 95質量部とMB-D 5質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料、さらにA面を構成する層(A層)とB面を構成する層(B層)との中間の層(C層)の原料としてPET-1を160℃で2時間真空乾燥した原料を、それぞれ別々の押出機に投入し、280℃で溶融させ、合流装置を通してA層/C層/B層の順番となるように積層し、各層の厚みが5/90/5となるように積層させた後、ダイを通して表面温度25℃のキャスティングドラム上に押し出し、未延伸シートを作製した。続いて該シートを加熱したロール群で予熱した後、90℃の温度で長手方向(MD方向)に3.8倍延伸を行った後、25℃の温度のロール群で冷却して一軸延伸フィルムを得た。得られた一軸延伸フィルムに、乾燥・延伸後の塗布厚みが100nmとなるようにバーコート法にて塗剤Fを塗布し、続いてフィルムのフィルム両端をクリップで把持しながらテンター内の100℃の温度の加熱ゾーンで長手方向に直角な幅方向(TD方向)に4.3倍延伸した。さらに引き続いて、テンター内の熱処理ゾーンで230℃の温度で10秒間の熱固定を施した。次いで、冷却ゾーンで均一に徐冷後、ロール形状に巻き取り、層Xが積層された積層ポリエステルフィルムを得た。
層Xとして、塗剤Mを用いた以外は、実施例21と同様に層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
実施例21で得られた層Xと層Yを除去したポリエステルフィルムを裁断し、ベント孔付き押出機に投入し、1kPa以下の減圧度に保持し水分を除去しながら280℃にて押出してペレット状に加工し再生原料-1を得た。再生原料のガラス転移温度は81℃、融点は255℃、固有粘度は0.58、末端カルボキシル基量は28eq./tであった。再生原料に含まれるポリエステル以外の成分は0.47質量%であった。
実施例25で得られた層Xと層Yを除去したポリエステルフィルムを裁断し、ベント孔付き押出機に投入し、1kPa以下の減圧度に保持し水分を除去しながら280℃にて押出してペレット状に加工し再生原料-2を得た。再生原料のガラス転移温度は81℃、融点は255℃、固有粘度は0.58、末端カルボキシル基量は28eq./tであった。再生原料に含まれるポリエステル以外の成分は0.03質量%であった。
A面を構成する原料としてPET-1 95質量部とMB-D 5質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料、さらにA面を構成する層(A層)とB面を構成する層(B層)との中間の層(C層)の原料としてPET-1 50質量部と参考例1で得た再生原料50質量部を混合し、160℃で2時間真空乾燥した原料を用い、実施例25と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
層Xとして、実施例28では塗剤K、実施例29では塗剤G、実施例30では塗剤Lを用いた以外は、実施例21と同様に積層ポリエステルフィルムを作製した。
A面を構成する原料としてPET-1 85質量部、MB-D 5質量部、参考例1で得た再生原料-1 10質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料、さらにA面を構成する層(A層)とB面を構成する層(B層)との中間の層(C層)の原料としてPET-1 100質量部を160℃で2時間真空乾燥した原料を用い、実施例25と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
A面を構成する原料としてPET-1 85質量部、MB-D 5質量部、参考例1で得た再生原料-1 10質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 10質量部、MB-B 40質量部、参考例1で得た再生原料-1 10質量部を混合し、160℃で2時間真空乾燥した原料、さらにA面を構成する層(A層)とB面を構成する層(B層)との中間の層(C層)の原料としてPET-1 100質量部を160℃で2時間真空乾燥した原料を用い、実施例25と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
A面を構成する原料としてPET-1 85質量部、MB-D 5質量部、参考例1で得た再生原料-1 10質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 10質量部、MB-B 40質量部、参考例1で得た再生原料-1 10質量部を混合し、160℃で2時間真空乾燥した原料、さらにA面を構成する層(A層)とB面を構成する層(B層)との中間の層(C層)の原料としてPET-1 50質量部と参考例1で得た再生原料-1 50質量部を160℃で2時間真空乾燥した原料を用い、実施例25と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
A面を構成する原料としてPET-1 85質量部、MB-D 5質量部、参考例1で得た再生原料-1 10質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料、さらにA面を構成する層(A層)とB面を構成する層(B層)との中間の層(C層)の原料としてPET-1 100質量部を160℃で2時間真空乾燥した原料を用い、実施例25と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
実施例35においては、A面、B面を構成する原料としてPET-1 95質量部とMB-D 5質量部を用いた点、実施例36においてはA面、B面を構成する原料としてPET-1 30質量部とMB-C 70質量部を用いた点以外は実施例19と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
A面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 95質量部とMB-D 5質量部を混合し、160℃で2時間真空乾燥した原料を用いた以外は、実施例21と同様にして層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
東レ(株)製ポリエステルフィルム“ルミラー”(登録商標)#50T60の片面(A面)に、乾燥後の塗布厚みが100nmとなるようにグラビアコート法にて塗剤Fを塗布し、ロール形状に巻き取り、層Xが積層された積層ポリエステルフィルムを得た。
層Xの構成成分として塗剤Rを用いた以外は、実施例21と同様に層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
A層、B層を構成する原料としてPET-1を80質量部、MB-Aを20質量部を混合し、160℃で2時間真空乾燥した後押出機に投入し、280℃で溶融させ、ダイを通して表面温度25℃のキャスティングドラム上に押し出し、未延伸シートを作製した。続いて該シートを加熱したロール群で予熱した後、95℃の温度で長手方向(MD方向)に3.5倍延伸を行った後、25℃の温度のロール群で冷却して一軸延伸フィルムを得た。得られた一軸延伸フィルムに、乾燥後の塗布厚みが100nmとなるようにバーコート法にて塗剤Sを塗布し、続いてフィルムのフィルム両端をクリップで把持しながらテンター内の95℃の温度の加熱ゾーンで長手方向に直角な幅方向(TD方向)に3.7倍延伸した。さらに引き続いて、テンター内の熱処理ゾーンで220℃の温度で10秒間の熱固定を施した。次いで、冷却ゾーンで均一に徐冷後、巻き取り、層Xが積層された積層ポリエステルフィルムを得た。
横延伸温度を表に記載の通りとした以外は、実施例21と同様に層Xを積層した積層ポリエステルフィルム、層Xと層Yが積層されたポリエステルフィルム、離型用フィルムを得た。
A面を構成する原料としてPET-1 95質量部とMB-D 5質量部を混合し、160℃で2時間真空乾燥した原料、B面を構成する原料としてPET-1 50質量部とMB-B 50質量部を混合し、160℃で2時間真空乾燥した原料を、それぞれ別々の押出機に投入し、280℃で溶融させ、合流装置を通してA面を構成する層(A層)の厚みとB面を構成する層(B層)の厚みが5/95となるように積層させた後、ダイを通して表面温度25℃のキャスティングドラム上に押し出し、未延伸シートを作製した。続いて該シートを加熱したロール群で予熱した後、90℃の温度で長手方向(MD方向)に3.8倍延伸を行った後、25℃の温度のロール群で冷却して一軸延伸フィルムを得た。得られた一軸延伸フィルムのフィルム両端をクリップで把持しながらテンター内の100℃の温度の加熱ゾーンで長手方向に直角な幅方向(TD方向)に4.3倍延伸した。さらに引き続いて、テンター内の熱処理ゾーンで230℃の温度で10秒間の熱固定を施した。次いで、冷却ゾーンで均一に徐冷後、ロール形状に巻き取り、層Xが積層されていない積層ポリエステルフィルムを得た。
A面、B面を構成する原料としてPET-1を用い、層Xとして、比較例1では塗剤Nを、比較例2では塗剤Oを用いた以外は、実施例1と同様にして積層ポリエステルフィルムを作製し、被離型物を積層した後に剥離し、その後に層X、層Yを除去し、ポリエステルフィルムを再利用した。
層Yとして、塗剤Aを用いた以外は、実施例42と同様に積層ポリエステルフィルムを作製し、被離型物としてセラミックグリーンシートと粘着シートをそれぞれ積層して評価し、セラミックグリーンシートを剥離した後に層Yを除去し、ポリエステルフィルムを再利用した。
Claims (25)
- ポリエステルフィルムと、以下の条件を満たす層Xを有する積層ポリエステルフィルム。
条件1:20≦γXP≦45
条件2:3.0≦γXH≦10
γXP(mN/m):層Xの表面自由エネルギーの極性成分
γXH(mN/m):層Xの表面自由エネルギーの水素結合成分 - 前記層Xの厚みxa(nm)と、前記ポリエステルフィルムの層Xを有する面(A面)とは反対側の面(B面)側の表面の粗さRzjisB(nm)が以下の条件を満たす請求項1に記載の積層ポリエステルフィルム。
条件3:1.0≦RzjisB/xa≦20.0
xa(nm):層Xの厚み - 前記層Xが以下の条件を満たす請求項1または2に記載の積層ポリエステルフィルム。
条件4:20≦γXP≦30
条件5:6.0≦γXH≦10 - 以下の条件を満たす請求項2または3に記載の積層ポリエステルフィルム。
条件6:1.5≦RzjisB/xa≦10.0 - 前記層Xの厚みxa(nm)と、前記層Xの表面の粗さRzjisX(nm)が以下の条件を満たす請求項1から4のいずれかに記載の積層ポリエステルフィルム。
条件7:0.01≦RzjisX/xa≦3.0 - 前記層Xの厚みxaが10nm以上500nm以下である請求項1から5のいずれかに記載の積層ポリエステルフィルム。
- 前記層Xの水の接触角HX(1)(°)とHX(20)(°)が以下の条件を満たす請求項1から6のいずれかに記載の積層ポリエステルフィルム。
条件8:5≦|HX(1)-HX(20)|≦60
HX(1)(°):層Xに水が接触してから1秒後の接触角
HX(20)(°):層Xに水が接触してから20秒後の接触角 - 前記層Xがポリビニルアルコール骨格を有する樹脂を含む請求項1から7のいずれかに記載の積層ポリエステルフィルム。
- 前記層Xがスルホン酸塩変性ポリビニルアルコール骨格を有する樹脂を含む請求項8に記載の積層ポリエステルフィルム。
- 前記層Xの結晶化度が14%以上40%以下である請求項1から9のいずれかに記載の積層ポリエステルフィルム。
- 前記層Xの結晶化度が31%より大きく、40%以下である請求項10に記載の積層ポリエステルフィルム。
- 前記層Xが重合度200より大きな樹脂を含む請求項1から11のいずれかに記載の積層ポリエステルフィルム。
- 以下の条件を満たす層Y、層X、ポリエステルフィルムをこの順で有する請求項1から12のいずれかに記載の積層ポリエステルフィルム。
条件9:80≦HY(1)≦120
条件10:1≦|HY(1)-HY(20)|≦90
HY(1)(°):層Yに水が接触してから1秒後の接触角
HY(20)(°):層Yに水が接触してから20秒後の接触角 - 前記層Yの表面の以下の方法で求められる溶剤耐久率が5%以上100%以下である請求項13に記載の積層ポリエステルフィルム。
[溶剤耐久率の測定方法]
試験機:学振型試験機(JIS L 0849(2013)に記載の摩擦試験機II形)
摩擦子:綿布(金巾3号)にトルエン:エタノールの混合溶媒(質量比1:1)を含浸
荷重:1kg
回数:30往復
溶剤耐久率(%)=F(A)/F(B)×100
F(A):層Y表面の剥離力
F(B):溶剤含浸布擦過試験後の層Y表面の剥離力 - 前記層Yの表面自由エネルギーの水素結合成分γYHが1.5以上10以下である請求項13または14に記載の積層ポリエステルフィルム。
- 前記層Yの層Xと接する面とは反対面に被離型層を設け、層Yから被離型層を剥離する離型用途に用いられる請求項13から15のいずれかに記載の積層ポリエステルフィルム。
- 層Yから被離型層を剥離した後、層Xと層Yが除去される用途に用いられる請求項16に記載の積層ポリエステルフィルム。
- 層Xと層Yを除去した積層ポリエステルフィルムを再利用する用途に用いられる請求項17に記載の積層ポリエステルフィルム。
- 前記被離型層が、チタン酸バリウムを主成分とするセラミックグリーンシートである請求項16から18のいずれかに記載の積層ポリエステルフィルム。
- 少なくとも積層セラミックコンデンサ(MLCC)製造工程用の離型フィルムの一部として用いられる、請求項1から19のいずれかに記載の積層ポリエステルフィルム。
- 少なくとも一方の表層に以下の条件を満たす層Yを有する積層ポリエステルフィルム。
条件11:80≦HY(1)≦120
条件12:1≦|HY(1)-HY(20)|≦90
HY(1)(°):層Yに水が接触してから1秒後の接触角
HY(20)(°):層Yに水が接触してから20秒後の接触角
- 前記ポリエステルフィルムが、前記ポリエステルフィルムの一方の表面であるA面を構成する層(A層)、もう一方の表面であるB面を構成する層(B層)と、表面を有しない層(C層)とを有する3層以上の積層構成を有しており、前記C層が再生ポリエステル原料を含む、請求項1から21のいずれかに記載の積層ポリエステルフィルム。
- 少なくとも被離型層、層Y、ポリエステルフィルムをこの順で有する、請求項22に記載の積層ポリエステルフィルムを用い、前記層Yから被離型層を剥離する工程と、被離型層を剥離したフィルムから層Yを除去する工程と、被離型層と層Yを除去したフィルムから再生原料を製造する工程を備え、さらにその再生原料を用いてフィルムを製膜する工程を備える、ポリエステルフィルムの製造方法。
- ポリエステルフィルムの片面(A面)に、親水性樹脂を主たる構成成分とする層Xを積層したポリエステルフィルムであって、層Xの厚みxa(nm)と、前記ポリエステルフィルムの層Xを有する面(A面)とは反対側の面(B面)側の表面の粗さRzjisB(nm)が以下の条件を満たす積層ポリエステルフィルム。
条件13:0.2≦RzjisB/xa≦20.0 - ポリエステルフィルムと、層Xを有する積層ポリエステルフィルムであって、層Xはスルホン酸塩変性ポリビニルアルコール骨格を有する樹脂を含有し、前記スルホン酸塩変性ポリビニルアルコール骨格を有する樹脂の、スルホン酸塩による共重合量が0.1mol%以上10mol%以下であり、かつ層XをJIS K 6726(1994)に記載の方法で平均重合度を求めた場合、求められる平均重合度が200以上2400以下であり、かつ層XをJIS K 6726(1994)に記載の方法でけん化度を求めた場合、求められるけん化度が30以上97以下である、積層ポリエステルフィルム。
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KR1020237019456A KR20230144521A (ko) | 2021-02-10 | 2022-01-24 | 적층 폴리에스테르 필름, 및 폴리에스테르 필름의 제조 방법 |
CN202280008354.3A CN116745117A (zh) | 2021-02-10 | 2022-01-24 | 层叠聚酯膜及聚酯膜的制造方法 |
US18/275,533 US20240101772A1 (en) | 2021-02-10 | 2022-01-24 | Laminated polyester film, and method for producing polyester film |
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JP2021-019556 | 2021-02-10 | ||
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JP2021-192791 | 2021-11-29 | ||
JP2021192792A JP2022122824A (ja) | 2021-02-10 | 2021-11-29 | 積層ポリエステルフィルム、およびポリエステルフィルムの製造方法 |
JP2021-192792 | 2021-11-29 | ||
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US (1) | US20240101772A1 (ja) |
KR (1) | KR20230144521A (ja) |
TW (1) | TW202231491A (ja) |
WO (1) | WO2022172735A1 (ja) |
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JP2014141557A (ja) * | 2013-01-23 | 2014-08-07 | Mitsubishi Plastics Inc | 離型フィルム |
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JP2018058270A (ja) * | 2016-10-05 | 2018-04-12 | 三菱ケミカル株式会社 | 積層ポリエステルフィルム |
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JP2004160773A (ja) | 2002-11-12 | 2004-06-10 | Toray Ind Inc | セラミックグリーンシートの製造方法 |
JP2012171276A (ja) | 2011-02-23 | 2012-09-10 | Teijin Dupont Films Japan Ltd | 熱可塑性樹脂フィルムの製造装置及び製造方法 |
-
2022
- 2022-01-24 US US18/275,533 patent/US20240101772A1/en active Pending
- 2022-01-24 KR KR1020237019456A patent/KR20230144521A/ko unknown
- 2022-01-24 WO PCT/JP2022/002364 patent/WO2022172735A1/ja active Application Filing
- 2022-01-27 TW TW111103593A patent/TW202231491A/zh unknown
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JPH09226231A (ja) * | 1995-10-12 | 1997-09-02 | Kao Corp | 記録用シート |
JP2001071420A (ja) * | 1999-06-30 | 2001-03-21 | Mitsubishi Polyester Film Copp | 離型フィルム |
JP2001150620A (ja) * | 1999-11-25 | 2001-06-05 | Teijin Ltd | インク受像層易接着ポリエステルフイルム |
JP2008142960A (ja) * | 2006-12-07 | 2008-06-26 | Mitsubishi Polyester Film Copp | 離型フィルム |
JP2012069769A (ja) * | 2010-09-24 | 2012-04-05 | Fujifilm Corp | 太陽電池用バックシート用ポリマーシート及び太陽電池モジュール |
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JP2014141557A (ja) * | 2013-01-23 | 2014-08-07 | Mitsubishi Plastics Inc | 離型フィルム |
JP2017025172A (ja) * | 2015-07-18 | 2017-02-02 | 三菱樹脂株式会社 | 積層ポリエステルフィルム |
JP2018058270A (ja) * | 2016-10-05 | 2018-04-12 | 三菱ケミカル株式会社 | 積層ポリエステルフィルム |
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KR20230144521A (ko) | 2023-10-16 |
US20240101772A1 (en) | 2024-03-28 |
TW202231491A (zh) | 2022-08-16 |
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