WO2022181246A1 - 共重合体、成形体、射出成形体および被覆電線 - Google Patents
共重合体、成形体、射出成形体および被覆電線 Download PDFInfo
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- WO2022181246A1 WO2022181246A1 PCT/JP2022/003665 JP2022003665W WO2022181246A1 WO 2022181246 A1 WO2022181246 A1 WO 2022181246A1 JP 2022003665 W JP2022003665 W JP 2022003665W WO 2022181246 A1 WO2022181246 A1 WO 2022181246A1
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- UJZCJVSSNLSCSR-UHFFFAOYSA-N (15,16,16,17,17,18,18,19,19,20,20-undecachloro-2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,13,13,14,14,15,22,22,22-triacontafluorodocosanoyl) 15,16,16,17,17,18,18,19,19,20,20-undecachloro-2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,13,13,14,14 Chemical compound FC(F)(F)CC(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(F)(Cl)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(=O)OOC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)CC(F)(F)F UJZCJVSSNLSCSR-UHFFFAOYSA-N 0.000 description 1
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- 238000002679 ablation Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- NSGQRLUGQNBHLD-UHFFFAOYSA-N butan-2-yl butan-2-yloxycarbonyloxy carbonate Chemical compound CCC(C)OC(=O)OOC(=O)OC(C)CC NSGQRLUGQNBHLD-UHFFFAOYSA-N 0.000 description 1
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- AAEHPKIXIIACPQ-UHFFFAOYSA-L calcium;terephthalate Chemical compound [Ca+2].[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 AAEHPKIXIIACPQ-UHFFFAOYSA-L 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical compound OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 description 1
- 125000006297 carbonyl amino group Chemical group [H]N([*:2])C([*:1])=O 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000002666 chemical blowing agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000007705 chemical test Methods 0.000 description 1
- KYKAJFCTULSVSH-UHFFFAOYSA-N chloro(fluoro)methane Chemical compound F[C]Cl KYKAJFCTULSVSH-UHFFFAOYSA-N 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000012438 extruded product Nutrition 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000003254 gasoline additive Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000005828 hydrofluoroalkanes Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- PEYVWSJAZONVQK-UHFFFAOYSA-N hydroperoxy(oxo)borane Chemical compound OOB=O PEYVWSJAZONVQK-UHFFFAOYSA-N 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 229920006120 non-fluorinated polymer Polymers 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 150000004978 peroxycarbonates Chemical class 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000009372 pisciculture Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001175 rotational moulding Methods 0.000 description 1
- 239000005336 safety glass Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—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 a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
- C08F214/262—Tetrafluoroethene with fluorinated vinyl ethers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/0001—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor characterised by the choice of material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
- C08F8/22—Halogenation by reaction with free halogens
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/443—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds
- H01B3/445—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds from vinylfluorides or other fluoroethylenic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
- B29K2027/18—PTFE, i.e. polytetrafluorethene, e.g. ePTFE, i.e. expanded polytetrafluorethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2071/00—Use of polyethers, e.g. PEEK, i.e. polyether-etherketone or PEK, i.e. polyetherketone or derivatives thereof, as moulding material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0018—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular optical properties, e.g. fluorescent or phosphorescent
- B29K2995/0026—Transparent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2800/00—Copolymer characterised by the proportions of the comonomers expressed
- C08F2800/20—Copolymer characterised by the proportions of the comonomers expressed as weight or mass percentages
Definitions
- the present disclosure relates to copolymers, molded articles, injection molded articles and coated wires.
- tetrafluoroethylene and the following general formula (I)- Rf-O-CF CF 2 (I) (Wherein, Rf represents a perfluoroalkyl group having 1 to 5 carbon atoms.)
- an extrusion molding method can be used to form a thin coating layer on a small-diameter core wire at a high speed, and an injection molding method can be used to obtain an injection-molded article having excellent surface smoothness with high productivity.
- a copolymer capable of obtaining a molded article excellent in wear resistance at 150° C., low carbon dioxide permeability, low chemical permeability, creep resistance, thermal rigidity, and heat deformation resistance after immersion in a chemical solution.
- the present disclosure contains tetrafluoroethylene units and perfluoro(propyl vinyl ether) units, and the content of perfluoro(propyl vinyl ether) units is 4.6 to 5.2 with respect to the total monomer units. % by mass, a melt flow rate at 372° C. of 22.0 to 28.0 g/10 min, and a functional group number of 50 or less per 10 6 main chain carbon atoms. be.
- an injection molded article containing the above copolymer is provided.
- a coated wire that includes a coating layer containing the above copolymer.
- a molded article containing the above copolymer wherein the molded article is a microtube, a container, a piping member, or a wire coating.
- a thin coating layer on a small-diameter core wire at a high speed by an extrusion molding method, and to obtain an injection-molded article having excellent surface smoothness with high productivity by an injection molding method.
- a copolymer capable of obtaining a molded article having excellent abrasion resistance at 150°C, low carbon dioxide permeability, low chemical permeability, creep resistance, thermal rigidity, and heat deformation resistance after immersion in a chemical solution. can do.
- the copolymer of the present disclosure contains tetrafluoroethylene (TFE) units and perfluoro(propyl vinyl ether) (PPVE) units.
- Microtubes (microcentrifuge tubes) that can accommodate small amounts of samples are used for storing and centrifuging small amounts of samples in biological or chemical tests. Microtubes made of fluororesin are used when heat resistance and chemical resistance are particularly required.
- a microtube is usually cylindrical or conical, with one end open and the other end closed. A lid is attached to one open end.
- centrifugation is performed for a long time at a high temperature of 95° C. or higher using such a microtube, the microtube may be deformed.
- the microtube may be worn or cracked.
- materials with excellent moldability.
- it since there are cases where chemicals are stored in microtubes, in order to prevent deterioration of the chemicals, it has excellent low chemical permeability so that it is difficult for chemicals such as electrolytes to escape to the outside. It is preferable to use a material having excellent low carbon dioxide permeability so that carbon dioxide does not easily penetrate inside.
- the moldability of the copolymer can be significantly improved, and at the same time such It was found that the 150° C. abrasion resistance, low carbon dioxide permeability, low chemical permeability, creep resistance, hot rigidity, and heat deformation resistance after immersion in a chemical solution of a molded product formed from the copolymer can be improved. served. Therefore, by using the copolymer of the present disclosure, it is possible to obtain a microtube that is resistant to deterioration of the sample and resistant to deformation or cracking even when centrifugation is performed at high temperature while containing a highly reactive chemical. .
- the copolymer of the present disclosure can form a thin coating layer on a small-diameter core wire at a high speed by an extrusion molding method.
- the copolymer of the present disclosure can be used not only as a material for valves, but also for a wide range of applications such as wire coating.
- the copolymer of the present disclosure is a melt-processable fluororesin.
- Melt processability means that the polymer can be melt processed using conventional processing equipment such as extruders and injection molding machines.
- the content of PPVE units in the copolymer is 4.6-5.2% by mass with respect to the total monomer units.
- the content of PPVE units in the copolymer is preferably 4.7% by mass or more, more preferably 4.8% by mass or more, still more preferably 4.9% by mass or more, and particularly preferably 5% by mass. 0% by mass or more, preferably 5.1% by mass or less, and more preferably 5.0% by mass or less. If the PPVE unit content of the copolymer is too high, a molded article having excellent low carbon dioxide permeability, creep resistance and high rigidity under heat cannot be obtained. If the PPVE unit content of the copolymer is too low, it is not possible to obtain a molded article that is excellent in wear resistance at 150° C. and heat deformation resistance after being immersed in a chemical solution.
- the content of TFE units in the copolymer is preferably 94.8 to 95.4% by mass, more preferably 94.9% by mass or more, and still more preferably 95% by mass, based on the total monomer units. 0% by mass or more, more preferably 95.3% by mass or less, still more preferably 95.2% by mass or less, particularly preferably 95.1% by mass or less, and most preferably 95.0% by mass. % by mass or less. If the TFE unit content of the copolymer is too low, it may not be possible to obtain a molded article having excellent low carbon dioxide permeability, creep resistance and high rigidity under heat. If the TFE unit content of the copolymer is too high, it may not be possible to obtain a molded article that is excellent in wear resistance at 150° C. and heat deformation resistance after being immersed in a chemical solution.
- the content of each monomer unit in the copolymer is measured by 19 F-NMR method.
- the copolymer can also contain monomeric units derived from monomers copolymerizable with TFE and PPVE.
- the content of monomer units copolymerizable with TFE and PPVE is preferably 0 to 1.5% by mass, more preferably 0.5% by mass, based on the total monomer units of the copolymer. 05 to 0.6% by mass, more preferably 0.1 to 0.3% by mass.
- the copolymer is preferably at least one selected from the group consisting of copolymers consisting only of TFE units and PPVE units, and TFE/HFP/PPVE copolymers, and copolymers consisting only of TFE units and PPVE units. Polymers are more preferred.
- the melt flow rate (MFR) of the copolymer is 22.0-28.0 g/10 minutes.
- the MFR of the copolymer is preferably 23.0 g/10 minutes or more, more preferably 23.1 g/10 minutes or more, and preferably 27.0 g/10 minutes or less. If the MFR of the copolymer is too high, it is not possible to obtain a molded article having excellent heat deformation resistance after being immersed in a chemical solution. If the MFR of the copolymer is too low, it becomes difficult to obtain an injection molded article having excellent surface smoothness when the copolymer is injected by injection molding, or the diameter of the copolymer is reduced by extrusion molding. When extruded onto small cords, the coating breaks and defects occur in the coating layer. On the other hand, if the MFR of the copolymer is too low, it is not possible to obtain a molded article having excellent low carbon dioxide permeability and low chemical liquid permeability.
- MFR is the mass of polymer that flows out per 10 minutes from a nozzle with an inner diameter of 2.1 mm and a length of 8 mm under a load of 5 kg at 372 ° C using a melt indexer according to ASTM D1238 (g / 10 minutes ) is the value obtained as
- the MFR can be adjusted by adjusting the type and amount of the polymerization initiator and the type and amount of the chain transfer agent used when polymerizing the monomers.
- the number of functional groups per 10 6 carbon atoms in the main chain of the copolymer is 50 or less.
- the number of functional groups per 10 6 carbon atoms in the main chain of the copolymer is preferably 40 or less, more preferably 30 or less, still more preferably 20 or less, and even more preferably 15 or less. , particularly preferably 10 or less, and most preferably less than 6.
- Infrared spectroscopic analysis can be used to identify the types of functional groups and measure the number of functional groups.
- the number of functional groups is measured by the following method.
- the above copolymer is cold-pressed to form a film having a thickness of 0.25 to 0.30 mm.
- the film is analyzed by Fourier Transform Infrared Spectroscopy to obtain the infrared absorption spectrum of the copolymer and the difference spectrum from the fully fluorinated base spectrum with no functional groups present. From the absorption peak of the specific functional group appearing in this difference spectrum, the number N of functional groups per 1 ⁇ 10 6 carbon atoms in the copolymer is calculated according to the following formula (A).
- N I ⁇ K/t (A) I: Absorbance K: Correction coefficient t: Film thickness (mm)
- Table 1 shows absorption frequencies, molar extinction coefficients and correction factors for some functional groups. Also, the molar extinction coefficient was determined from the FT-IR measurement data of the low-molecular-weight model compound.
- the absorption frequencies of —CH 2 CF 2 H, —CH 2 COF, —CH 2 COOH, —CH 2 COOCH 3 and —CH 2 CONH 2 are shown in the table, respectively, —CF 2 H, —COF and —COOH free.
- the absorption frequency of -COOH bonded, -COOCH 3 and -CONH 2 is several tens of Kaiser (cm -1 ) lower than that of -CONH 2 .
- the number of functional groups of —COF is determined from the number of functional groups obtained from the absorption peak at an absorption frequency of 1883 cm ⁇ 1 due to —CF 2 COF and from the absorption peak at an absorption frequency of 1840 cm ⁇ 1 due to —CH 2 COF. It is the sum of the number of functional groups.
- the functional group is a functional group present at the main chain end or side chain end of the copolymer, and a functional group present in the main chain or side chain.
- the functional group is introduced into the copolymer, for example, by a chain transfer agent or a polymerization initiator used in producing the copolymer.
- a chain transfer agent or a polymerization initiator used in producing the copolymer.
- —CH 2 OH is introduced at the main chain end of the copolymer.
- the functional group is introduced into the side chain end of the copolymer.
- the copolymer of the present disclosure is preferably fluorinated. It is also preferred that the copolymers of the present disclosure have —CF 3 end groups.
- the melting point of the copolymer is preferably 295 to 315°C, more preferably 300°C or higher, still more preferably 302°C or higher, preferably 308°C or lower, and more preferably 304°C or lower. .
- the melting point is within the above range, it is possible to obtain a copolymer that gives a molded article that is particularly excellent in mechanical properties at high temperatures and sealability at high temperatures.
- the melting point can be measured using a differential scanning calorimeter [DSC].
- the carbon dioxide permeability coefficient of the copolymer is preferably 1500 cm 3 ⁇ mm/(m 2 ⁇ 24h ⁇ atm) or less.
- the copolymers of the present disclosure exhibit excellent carbon dioxide reduction because the PPVE unit content, melt flow rate (MFR), and functional group number of the copolymer containing TFE units and PPVE units are appropriately adjusted. It has transparency. Therefore, by using the copolymer of the present disclosure, it is possible to form microtubes, piping members, and containers that can suppress the permeation of carbon dioxide from the outside. During storage or long-term residence in a pipe, the alkali in the aqueous solution reacts with carbon dioxide that permeates from the outside, and the problem of lowering the purity of the aqueous alkali solution is less likely to occur.
- the carbon dioxide permeability coefficient can be measured under the conditions of a test temperature of 70°C and a test humidity of 0% RH.
- a specific measurement of the carbon dioxide permeability coefficient can be performed by the method described in Examples.
- the electrolyte permeability of the copolymer is preferably 7.0 g ⁇ cm/m 2 or less, more preferably 6.5 g ⁇ cm/m 2 or less.
- the copolymers of the present disclosure are excellent electrolyte-lowering because the PPVE unit content, melt flow rate (MFR), and functional group number of the copolymers containing TFE units and PPVE units are appropriately adjusted. It has transparency. That is, by using the copolymer of the present disclosure, it is possible to obtain a molded article that is less permeable to chemicals such as electrolytic solutions.
- the electrolyte permeability can be measured under conditions of a temperature of 60°C and 30 days. Specific measurement of electrolyte permeability can be performed by the method described in Examples.
- the copolymer of the present disclosure can be produced by polymerization methods such as suspension polymerization, solution polymerization, emulsion polymerization, and bulk polymerization. Emulsion polymerization or suspension polymerization is preferred as the polymerization method. In these polymerizations, the conditions such as temperature and pressure, the polymerization initiator and other additives can be appropriately set according to the composition and amount of the copolymer.
- an oil-soluble radical polymerization initiator or a water-soluble radical polymerization initiator can be used as the polymerization initiator.
- the oil-soluble radical polymerization initiator may be a known oil-soluble peroxide, for example Dialkyl peroxycarbonates such as di-normal propyl peroxydicarbonate, diisopropyl peroxydicarbonate, disec-butyl peroxydicarbonate, di-2-ethoxyethyl peroxydicarbonate; Peroxyesters such as t-butyl peroxyisobutyrate and t-butyl peroxypivalate; Dialkyl peroxides such as di-t-butyl peroxide; Di[fluoro (or fluorochloro) acyl] peroxides; etc. are typical examples.
- Dialkyl peroxycarbonates such as di-normal propyl peroxydicarbonate, diisopropyl peroxydicarbonate, disec-butyl peroxydicarbonate, di-2-ethoxyethyl peroxydicarbonate
- Peroxyesters such as t-butyl peroxy
- Di[fluoro(or fluorochloro)acyl] peroxides include diacyl represented by [(RfCOO)-] 2 (Rf is a perfluoroalkyl group, ⁇ -hydroperfluoroalkyl group or fluorochloroalkyl group) peroxides.
- Di[fluoro(or fluorochloro)acyl] peroxides include, for example, di( ⁇ -hydro-dodecafluorohexanoyl) peroxide, di( ⁇ -hydro-tetradecafluoroheptanoyl) peroxide, di( ⁇ -hydro-hexadecafluorononanoyl)peroxide, di(perfluoropropionyl)peroxide, di(perfluorobutyryl)peroxide, di(perfluoropareryl)peroxide, di(perfluorohexanoyl)peroxide , di(perfluoroheptanoyl) peroxide, di(perfluorooctanoyl) peroxide, di(perfluorononanoyl) peroxide, di( ⁇ -chloro-hexafluorobutyryl) peroxide, di( ⁇ -chloro -decafluorohexanoyl
- the water-soluble radical polymerization initiator may be a known water-soluble peroxide, for example, persulfuric acid, perboric acid, perchloric acid, superphosphoric acid, ammonium salts such as percarbonic acid, potassium salts, sodium salts, disuccinic acid.
- Acid peroxides organic peroxides such as diglutaric acid peroxide, t-butyl permalate, t-butyl hydroperoxide and the like.
- a reducing agent such as sulfites may be used in combination with the peroxide, and the amount used may be 0.1 to 20 times the peroxide.
- a surfactant In polymerization, a surfactant, a chain transfer agent, and a solvent can be used, and conventionally known ones can be used.
- surfactant known surfactants can be used, such as nonionic surfactants, anionic surfactants and cationic surfactants.
- fluorine-containing anionic surfactants are preferable, and may contain etheric oxygen (that is, oxygen atoms may be inserted between carbon atoms), linear or branched surfactants having 4 to 20 carbon atoms
- a fluorine-containing anionic surfactant is more preferred.
- the amount of surfactant added (to polymerization water) is preferably 50 to 5000 ppm.
- chain transfer agents examples include hydrocarbons such as ethane, isopentane, n-hexane and cyclohexane; aromatics such as toluene and xylene; ketones such as acetone; ethyl acetate and butyl acetate; , alcohols such as ethanol; mercaptans such as methyl mercaptan; halogenated hydrocarbons such as carbon tetrachloride, chloroform, methylene chloride and methyl chloride.
- the amount of the chain transfer agent to be added may vary depending on the chain transfer constant of the compound used, but it is usually used in the range of 0.01 to 20% by mass relative to the polymerization solvent.
- solvents examples include water and mixed solvents of water and alcohol.
- a fluorinated solvent may be used in addition to water.
- Hydrochlorofluoroalkanes such as CH 3 CClF 2 , CH 3 CCl 2 F, CF 3 CF 2 CCl 2 H, CF 2 ClCF 2 CFHCl; CF 2 ClCFClCF 2 CF 3 , CF 3 CFClCFClCF 3 , etc.
- hydrofluoroalkanes such as CF3CFHCFHCF2CF2CF3 , CF2HCF2CF2CF2H , CF3CF2CF2CF2CF2CF2H ; CH _ _ _ _ _ _ 3OC2F5 , CH3OC3F5CF3CF2CH2OCHF2 , CF3CHFCF2OCH3 , CHF2CF2OCH2F , ( CF3 ) 2CHCF2OCH3 , CF3CF2 _ _ _ _ _ _ _ _ _ _ _ Hydrofluoroethers such as CH2OCH2CHF2 , CF3CHFCF2OCH2CF3 ; perfluorocyclobutane , CF3CF2CF2CF3 , CF3CF2CF2CF2CF3 , CF3CF2 _ _ _ _ Examples include perfluoroalkanes such as CF 2 CF 2
- the polymerization temperature is not particularly limited, and may be 0 to 100°C.
- the polymerization pressure is appropriately determined according to other polymerization conditions such as the type and amount of the solvent used, vapor pressure, polymerization temperature, etc., and may generally be from 0 to 9.8 MPaG.
- the copolymer When an aqueous dispersion containing a copolymer is obtained by a polymerization reaction, the copolymer can be recovered by coagulating, washing, and drying the copolymer contained in the aqueous dispersion. Moreover, when the copolymer is obtained as a slurry by the polymerization reaction, the copolymer can be recovered by removing the slurry from the reaction vessel, washing it, and drying it. The copolymer can be recovered in the form of powder by drying.
- the copolymer obtained by polymerization may be molded into pellets.
- a molding method for molding into pellets is not particularly limited, and conventionally known methods can be used. For example, a method of melt extruding a copolymer using a single-screw extruder, twin-screw extruder, or tandem extruder, cutting it into a predetermined length, and molding it into pellets can be used.
- the extrusion temperature for melt extrusion must be changed according to the melt viscosity of the copolymer and the production method, and is preferably from the melting point of the copolymer +20°C to the melting point of the copolymer +140°C.
- the method for cutting the copolymer is not particularly limited, and conventionally known methods such as a strand cut method, a hot cut method, an underwater cut method, and a sheet cut method can be employed.
- the obtained pellets may be heated to remove volatile matter in the pellets (deaeration treatment).
- the obtained pellets may be treated by contacting them with warm water of 30-200°C, steam of 100-200°C, or hot air of 40-200°C.
- a copolymer obtained by polymerization may be fluorinated.
- the fluorination treatment can be carried out by contacting the non-fluorinated copolymer with a fluorine-containing compound.
- the fluorine-containing compound is not particularly limited, but includes fluorine radical sources that generate fluorine radicals under fluorination treatment conditions.
- fluorine radical source include F 2 gas, CoF 3 , AgF 2 , UF 6 , OF 2 , N 2 F 2 , CF 3 OF, halogen fluoride (eg IF 5 , ClF 3 ), and the like.
- the fluorine radical source such as F 2 gas may have a concentration of 100%, but from the viewpoint of safety, it is preferable to mix it with an inert gas and dilute it to 5 to 50% by mass before use. It is more preferable to dilute to 30% by mass before use.
- the inert gas include nitrogen gas, helium gas, argon gas, etc. Nitrogen gas is preferable from an economical point of view.
- the conditions for the fluorination treatment are not particularly limited, and the copolymer in a molten state may be brought into contact with the fluorine-containing compound. Preferably, it can be carried out at a temperature of 100 to 220°C.
- the fluorination treatment is generally carried out for 1 to 30 hours, preferably 5 to 25 hours.
- the fluorination treatment is preferably carried out by contacting the unfluorinated copolymer with fluorine gas (F2 gas).
- a composition may be obtained by mixing the copolymer of the present disclosure with other components as necessary.
- Other components include fillers, plasticizers, processing aids, release agents, pigments, flame retardants, lubricants, light stabilizers, weather stabilizers, conductive agents, antistatic agents, ultraviolet absorbers, antioxidants, Foaming agents, fragrances, oils, softening agents, dehydrofluorination agents and the like can be mentioned.
- fillers include silica, kaolin, clay, organic clay, talc, mica, alumina, calcium carbonate, calcium terephthalate, titanium oxide, calcium phosphate, calcium fluoride, lithium fluoride, crosslinked polystyrene, potassium titanate, Examples include carbon, boron nitride, carbon nanotubes, glass fibers, and the like.
- the conductive agent include carbon black and the like.
- plasticizers include dioctylphthalic acid and pentaerythritol.
- processing aids include carnauba wax, sulfone compounds, low-molecular-weight polyethylene, fluorine-based aids, and the like.
- dehydrofluorination agents include organic oniums and amidines.
- Polymers other than the copolymers described above may be used as the other components.
- examples of other polymers include fluororesins, fluororubbers, and non-fluorinated polymers other than the copolymers described above.
- Examples of the method for producing the above composition include a method of dry mixing the copolymer and other components, a method of mixing the copolymer and other components in advance in a mixer, and then using a kneader, a melt extruder, or the like.
- the method of melt-kneading, etc. can be mentioned.
- the copolymer of the present disclosure or the composition described above can be used as a processing aid, molding material, etc., but is preferably used as a molding material.
- Aqueous dispersions, solutions, suspensions, and copolymer/solvent systems of the copolymers of the present disclosure are also available and can be applied as coatings, encapsulated, impregnated, and used to cast films. can However, since the copolymer of the present disclosure has the properties described above, it is preferably used as the molding material.
- a molded article may be obtained by molding the copolymer of the present disclosure or the above composition.
- the method for molding the above copolymer or composition is not particularly limited, and examples thereof include injection molding, extrusion molding, compression molding, blow molding, transfer molding, roto molding, roto lining molding, and the like. .
- extrusion molding, compression molding, injection molding, or transfer molding is preferable, and injection molding, extrusion, or transfer molding is more preferable because it can produce molded articles with high productivity.
- the injection molding method is preferably an extrusion molded article, a compression molded article, an injection molded article or a transfer molded article. is more preferred, and an injection molded article is even more preferred.
- Molded articles containing the copolymer of the present disclosure include, for example, nuts, bolts, joints, films, bottles, gaskets, wire coatings, tubes, hoses, pipes, valves, sheets, seals, packings, tanks, rollers, and containers. , cocks, connectors, filter housings, filter cages, flow meters, pumps, wafer carriers, wafer boxes, and the like.
- the copolymer of the present disclosure, the composition described above, or the molded article described above can be used, for example, in the following applications.
- Films for food packaging, lining materials for fluid transfer lines used in food manufacturing processes, packings, sealing materials, and fluid transfer members for food manufacturing equipment such as sheets
- Drug stoppers for drugs, packaging films, lining materials for fluid transfer lines used in the process of manufacturing drugs, packings, sealing materials, and chemical liquid transfer members such as sheets
- Inner lining members for chemical tanks and piping in chemical plants and semiconductor factories O (square) rings, tubes, packings, valve core materials, hoses, sealing materials, etc. used in automobile fuel systems and peripheral devices; fuel transfer members such as hoses, sealing materials, etc.
- Coating and ink components such as coating rolls, hoses, tubes, and ink containers for coating equipment; Tubes for food and drink or tubes such as food and drink hoses, hoses, belts, packings, food and drink transfer members such as joints, food packaging materials, glass cooking equipment; Parts for transporting waste liquid such as tubes and hoses for transporting waste liquid; Parts for transporting high-temperature liquids, such as tubes and hoses for transporting high-temperature liquids; Steam piping members such as steam piping tubes and hoses; Anti-corrosion tape for piping such as tape to be wrapped around piping on ship decks; Various coating materials such as wire coating materials, optical fiber coating materials, transparent surface coating materials and back coating materials provided on the light incident side surface of photovoltaic elements of solar cells; Sliding members such as diaphragms of diaphragm pumps and various packings; Agricultural films, weather-resistant covers for various roofing materials and side walls; Interior materials used in the construction field, coating materials for glasses such
- fuel transfer members used in the fuel system of automobiles include fuel hoses, filler hoses, and evaporation hoses.
- the above-mentioned fuel transfer member can also be used as a fuel transfer member for sour gasoline-resistant fuel, alcohol-resistant fuel, and fuel containing gasoline additives such as methyl tert-butyl ether and amine-resistant fuel.
- the above drug stoppers and packaging films for drugs have excellent chemical resistance against acids and the like.
- an anticorrosive tape to be wound around chemical plant pipes can also be mentioned.
- Examples of the above molded bodies also include automobile radiator tanks, chemical liquid tanks, bellows, spacers, rollers, gasoline tanks, containers for transporting waste liquids, containers for transporting high-temperature liquids, fisheries and fish farming tanks, and the like.
- Examples of the molded article include automobile bumpers, door trims, instrument panels, food processing equipment, cooking equipment, water- and oil-repellent glass, lighting-related equipment, display panels and housings for OA equipment, illuminated signboards, displays, and liquid crystals.
- Members used for displays, mobile phones, printed circuit boards, electrical and electronic parts, miscellaneous goods, trash cans, bathtubs, unit baths, ventilation fans, lighting frames and the like are also included.
- Molded articles containing the copolymer of the present disclosure are excellent in abrasion resistance at 150° C., low carbon dioxide permeability, low chemical liquid permeability, creep resistance, hot rigidity, and heat deformation resistance after immersion in a chemical liquid. It can be suitably used for nuts, bolts, joints, packings, valves, cocks, connectors, filter housings, filter cages, flowmeters, pumps, and the like. For example, it can be suitably used as a piping member (particularly a joint) used for transporting a chemical solution, or as a flowmeter housing having a flow path for a chemical solution in a flowmeter. The piping member and the flowmeter housing of the present disclosure are excellent in 150° C.
- the piping member and the flowmeter housing of the present disclosure can be suitably used for measuring the flow rate of high-temperature chemical solutions, and are less likely to be damaged even when chemicals are distributed.
- Molded articles containing the copolymer of the present disclosure are excellent in abrasion resistance at 150° C., low carbon dioxide permeability, low chemical liquid permeability, creep resistance, hot rigidity, and heat deformation resistance after immersion in a chemical liquid. It can be suitably used as a member to be compressed such as a gasket or packing.
- the size and shape of the member to be compressed of the present disclosure may be appropriately set according to the application, and are not particularly limited.
- the shape of the compressible member of the present disclosure may be annular, for example.
- the member to be compressed of the present disclosure may have a shape such as a circle, an oval, or a rectangle with rounded corners in a plan view, and may have a through hole in the center thereof.
- the member to be compressed of the present disclosure is preferably used as a member for configuring a non-aqueous electrolyte battery.
- the member to be compressed of the present disclosure is particularly suitable as a member used in contact with the non-aqueous electrolyte in the non-aqueous electrolyte battery because of its excellent low electrolyte permeability. That is, the member to be compressed of the present disclosure may have a liquid contact surface with the non-aqueous electrolyte in the non-aqueous electrolyte battery.
- the non-aqueous electrolyte battery is not particularly limited as long as it is a battery with a non-aqueous electrolyte, and examples thereof include lithium ion secondary batteries and lithium ion capacitors. Further, examples of members constituting the non-aqueous electrolyte battery include a sealing member and an insulating member.
- the non-aqueous electrolyte is not particularly limited, but includes propylene carbonate, ethylene carbonate, butylene carbonate, ⁇ -butyl lactone, 1,2-dimethoxyethane, 1,2-diethoxyethane, dimethyl carbonate, and diethyl carbonate. , ethyl methyl carbonate and the like can be used.
- the nonaqueous electrolyte battery may further include an electrolyte.
- the electrolyte is not particularly limited, but LiClO 4 , LiAsF 6 , LiPF 6 , LiBF 4 , LiCl, LiBr, CH 3 SO 3 Li, CF 3 SO 3 Li, cesium carbonate, or the like can be used.
- the member to be compressed of the present disclosure can be suitably used as, for example, a sealing member such as a sealing gasket and sealing packing, and an insulating member such as an insulating gasket and insulating packing.
- a sealing member is a member used to prevent leakage of liquid or gas or intrusion of liquid or gas from the outside.
- An insulating member is a member used to insulate electricity.
- Compressed members of the present disclosure may be members used for both sealing and insulating purposes.
- the member to be compressed of the present disclosure is excellent in creep resistance and thermal deformation resistance after being immersed in a chemical solution, so it can be suitably used in a high-temperature environment.
- the member to be compressed of the present disclosure is preferably used in an environment where the maximum temperature is 40°C or higher.
- the member to be compressed of the present disclosure is preferably used in an environment with a maximum temperature of 95°C or higher. Examples of cases where the compressed member of the present disclosure can reach such a high temperature include, for example, when the compressed member is attached to the battery in a compressed state and then another battery member is attached to the battery by welding, or when non-aqueous electrolysis For example, the liquid battery generates heat.
- the member to be compressed of the present disclosure is excellent in creep resistance and heat deformation resistance after being immersed in a chemical solution, so it can be suitably used as a sealing member for non-aqueous electrolyte batteries or an insulating member for non-aqueous electrolyte batteries.
- a sealing member for non-aqueous electrolyte batteries or an insulating member for non-aqueous electrolyte batteries For example, when charging a battery such as a non-aqueous electrolyte secondary battery, the temperature of the battery may temporarily rise to 40° C. or higher, particularly temporarily to 95° C. or higher.
- the member to be compressed of the present disclosure can be used in a battery such as a non-aqueous electrolyte secondary battery by being deformed at a high compression deformation rate at high temperature, or even when it comes into contact with a non-aqueous electrolyte at high temperature.
- the member to be compressed of the present disclosure when used as a sealing member, it has excellent sealing properties, and the sealing properties are maintained for a long period of time even at high temperatures.
- the member to be compressed of the present disclosure contains the copolymer, it has excellent insulating properties. Therefore, when the compressible member of the present disclosure is used as an insulating member, it adheres tightly to two or more conductive members to prevent short circuits over time.
- the copolymer of the present disclosure can be obtained at a high take-up speed without causing breakage of the coating even if the diameter of the cord is small. Since a thin coating layer can be formed on a small core wire and a coating layer having excellent electrical properties can be formed, it can be suitably used as a material for forming a wire coating. Therefore, a coated electric wire provided with a coating layer containing the copolymer of the present disclosure has almost no spark-generating defects even when the diameter of the core wire is small and the coating layer is thin. , and has excellent electrical properties.
- a covered electric wire includes a core wire and a coating layer provided around the core wire and containing the copolymer of the present disclosure.
- the coating layer can be an extruded product obtained by melt extruding the copolymer of the present disclosure on the core wire.
- the coated electric wire is suitable for LAN cables (Ethernet Cable), high frequency transmission cables, flat cables, heat resistant cables, etc., and particularly suitable for transmission cables such as LAN cables (Eathnet Cable) and high frequency transmission cables.
- the core wire for example, a metal conductor material such as copper or aluminum can be used.
- the core wire preferably has a diameter of 0.02 to 3 mm.
- the diameter of the cord is more preferably 0.04 mm or more, still more preferably 0.05 mm or more, and particularly preferably 0.1 mm or more.
- the diameter of the cord is more preferably 2 mm or less.
- core wires include AWG (American Wire Gauge)-46 (solid copper wire with a diameter of 40 micrometers), AWG-26 (solid copper wire with a diameter of 404 micrometers), AWG-24 (diameter 510 micrometer solid copper wire), AWG-22 (635 micrometer diameter solid copper wire), etc. may be used.
- AWG American Wire Gauge
- AWG-46 solid copper wire with a diameter of 40 micrometers
- AWG-26 solid copper wire with a diameter of 404 micrometers
- AWG-24 diameter 510 micrometer solid copper wire
- AWG-22 (635 micrometer diameter solid copper wire), etc.
- the thickness of the coating layer is preferably 0.1 to 3.0 mm. It is also preferable that the thickness of the coating layer is 2.0 mm or less.
- a coating layer having a thickness of 0.5 mm or less, 0.4 mm or less, 0.3 mm or less, or 0.2 mm or less can be formed without problems.
- a coaxial cable is an example of a high-frequency transmission cable.
- a coaxial cable generally has a structure in which an inner conductor, an insulating coating layer, an outer conductor layer and a protective coating layer are laminated in order from the core to the outer periphery.
- a molded article containing the copolymer of the present disclosure can be suitably used as an insulating coating layer containing the copolymer.
- the thickness of each layer in the above structure is not particularly limited, but usually the inner conductor has a diameter of about 0.1 to 3 mm, the insulating coating layer has a thickness of about 0.3 to 3 mm, and the outer conductor layer has a thickness of about 0.5-10 mm, the protective coating layer is about 0.5-2 mm thick.
- the coating layer may contain air bubbles, and it is preferable that the air bubbles are uniformly distributed in the coating layer.
- the average bubble diameter of the bubbles is not limited, for example, it is preferably 60 ⁇ m or less, more preferably 45 ⁇ m or less, even more preferably 35 ⁇ m or less, and even more preferably 30 ⁇ m or less. It is preferably 25 ⁇ m or less, particularly preferably 23 ⁇ m or less, and most preferably 23 ⁇ m or less. Also, the average bubble diameter is preferably 0.1 ⁇ m or more, more preferably 1 ⁇ m or more. The average bubble diameter can be obtained by taking an electron microscope image of the cross section of the electric wire, calculating the diameter of each bubble by image processing, and averaging the diameters.
- the coating layer may have an expansion rate of 20% or more. It is more preferably 30% or more, still more preferably 33% or more, and even more preferably 35% or more.
- the upper limit is not particularly limited, it is, for example, 80%.
- the upper limit of the expansion rate may be 60%.
- the foaming rate is a value obtained by ((specific gravity of wire coating material ⁇ specific gravity of coating layer)/specific gravity of wire coating material) ⁇ 100. The foaming rate can be appropriately adjusted depending on the application, for example, by adjusting the amount of gas inserted into the extruder, which will be described later, or by selecting the type of gas to be dissolved.
- the covered electric wire may have another layer between the core wire and the covering layer, and may have another layer (outer layer) around the covering layer.
- the electric wire of the present disclosure has a two-layer structure (skin-foam) in which a non-foaming layer is inserted between the core wire and the covering layer, or a two-layer structure in which the outer layer is covered with a non-foaming layer. (foam-skin), or a three-layer structure (skin-foam-skin) in which the outer layer of skin-foam is covered with a non-foamed layer.
- the non-foamed layer is not particularly limited, and includes TFE/HFP copolymers, TFE/PAVE copolymers, TFE/ethylene copolymers, vinylidene fluoride polymers, polyolefin resins such as polyethylene [PE], polychlorinated It may be a resin layer made of a resin such as vinyl [PVC].
- a coated electric wire can be produced, for example, by heating a copolymer using an extruder and extruding the molten copolymer onto a core wire to form a coating layer.
- the coating layer containing air bubbles can be formed by heating the copolymer and introducing a gas into the copolymer while the copolymer is in a molten state.
- a gas such as chlorodifluoromethane, nitrogen, carbon dioxide, or a mixture of the above gases can be used.
- the gas may be introduced into the heated copolymer as a pressurized gas or may be generated by incorporating a chemical blowing agent into the copolymer. The gas dissolves in the molten copolymer.
- copolymer of the present disclosure can be suitably used as a material for high-frequency signal transmission products.
- the product for high-frequency signal transmission is not particularly limited as long as it is a product used for high-frequency signal transmission. Molded bodies such as high-frequency vacuum tube bases and antenna covers, (3) coated electric wires such as coaxial cables and LAN cables, and the like.
- the above products for high-frequency signal transmission can be suitably used in equipment that uses microwaves, particularly microwaves of 3 to 30 GHz, such as satellite communication equipment and mobile phone base stations.
- the copolymer of the present disclosure can be suitably used as an insulator because of its low dielectric loss tangent.
- a printed wiring board is preferable in terms of obtaining good electrical characteristics.
- the printed wiring board include, but are not particularly limited to, printed wiring boards for electronic circuits such as mobile phones, various computers, and communication devices.
- an antenna cover is preferable in terms of low dielectric loss.
- a sheet with excellent surface smoothness can be obtained with high productivity by molding the copolymer of the present disclosure by an injection molding method.
- the molded article containing the copolymer of the present disclosure is excellent in wear resistance at 150° C., low carbon dioxide permeability, low chemical permeability, creep resistance, hot rigidity, and heat deformation resistance after immersion in a chemical solution. there is Therefore, a molded article containing the copolymer of the present disclosure can be suitably used as a film or sheet.
- the film of the present disclosure is useful as a release film.
- the release film can be produced by molding the copolymer of the present disclosure by melt extrusion molding, calendar molding, press molding, casting molding, or the like. From the viewpoint of obtaining a uniform thin film, the release film can be produced by melt extrusion molding.
- the film of the present disclosure can be applied to the surface of rolls used in OA equipment.
- the copolymer of the present disclosure is molded into a required shape by extrusion molding, compression molding, press molding, etc., and molded into a sheet, film, or tube, and surface materials such as OA equipment rolls or OA equipment belts. can be used for In particular, thin-walled tubes and films can be produced by melt extrusion.
- the molded article containing the copolymer of the present disclosure is excellent in wear resistance at 150° C., low carbon dioxide permeability, low chemical permeability, creep resistance, hot rigidity, and heat deformation resistance after immersion in a chemical solution. Therefore, it can be suitably used as a bottle or a tube.
- a bottle or tube of the present disclosure allows for easy viewing of the contents and is less prone to damage during use.
- the valve containing the copolymer of the present disclosure can be manufactured with high productivity, is less likely to be damaged even when repeatedly opened and closed at high frequency, and has excellent low carbon dioxide permeability and low chemical liquid permeability.
- the valve of the present disclosure may be a valve comprising a housing containing the above copolymer.
- melt flow rate (MFR) Melt flow rate (MFR)
- G-01 melt indexer
- N I ⁇ K/t (A)
- K Correction coefficient
- t Film thickness (mm)
- Table 2 shows the absorption frequencies, molar extinction coefficients, and correction factors for the functional groups in the present disclosure. The molar extinction coefficient was determined from the FT-IR measurement data of the low-molecular-weight model compound.
- melting point Using a differential scanning calorimeter (trade name: X-DSC7000, manufactured by Hitachi High-Tech Science Co., Ltd.), the temperature was first raised from 200 ° C. to 350 ° C. at a heating rate of 10 ° C./min, followed by a cooling rate. Cool from 350°C to 200°C at 10°C/min, then heat again from 200°C to 350°C at a heating rate of 10°C/min for the second time, and peak the melting curve during the second heating process. The melting point was obtained from
- Comparative example 1 51.8 L of pure water was put into an autoclave with a volume of 174 L, and after sufficient nitrogen substitution, 40.9 kg of perfluorocyclobutane and 2.75 kg of perfluoro(propyl vinyl ether) (PPVE) were charged, and the temperature in the system was The temperature was kept at 35° C. and the stirring speed was 200 rpm. Then, after pressurizing tetrafluoroethylene (TFE) to 0.64 MPa, 0.103 kg of a 50% methanol solution of di-n-propylperoxydicarbonate was added to initiate polymerization.
- TFE tetrafluoroethylene
- the resulting powder was melt-extruded at 360°C with a screw extruder (trade name: PCM46, manufactured by Ikegai Co., Ltd.) to obtain TFE/PPVE copolymer pellets.
- a screw extruder (trade name: PCM46, manufactured by Ikegai Co., Ltd.) to obtain TFE/PPVE copolymer pellets.
- the PPVE content was measured by the method described above.
- the obtained pellets were placed in a vacuum vibration reactor VVD-30 (manufactured by Okawara Seisakusho Co., Ltd.) and heated to 210°C. After evacuation, F2 gas diluted to 20 % by volume with N2 gas was introduced to atmospheric pressure. After 0.5 hours from the introduction of the F2 gas, the chamber was once evacuated, and the F2 gas was introduced again. Further, after 0.5 hours, the chamber was evacuated again and F 2 gas was introduced again. Thereafter, the F 2 gas introduction and evacuation operations were continued once an hour, and the reaction was carried out at a temperature of 210° C. for 10 hours. After completion of the reaction, the interior of the reactor was sufficiently replaced with N2 gas to complete the fluorination reaction. Using the fluorinated pellets, various physical properties were measured by the methods described above.
- Comparative example 2 51.8 L of pure water was put into an autoclave with a volume of 174 L, and after sufficient nitrogen substitution, 40.9 kg of perfluorocyclobutane, 2.05 k of perfluoro(propyl vinyl ether) (PPVE), and 2.12 kg of methanol were charged, The temperature in the system was kept at 35° C. and the stirring speed was kept at 200 rpm. Then, after pressurizing tetrafluoroethylene (TFE) to 0.64 MPa, 0.103 kg of a 50% methanol solution of di-n-propylperoxydicarbonate was added to initiate polymerization.
- TFE tetrafluoroethylene
- the resulting powder was melt-extruded at 360°C with a screw extruder (trade name: PCM46, manufactured by Ikegai Co., Ltd.) to obtain TFE/PPVE copolymer pellets.
- a screw extruder (trade name: PCM46, manufactured by Ikegai Co., Ltd.) to obtain TFE/PPVE copolymer pellets.
- the PPVE content was measured by the method described above.
- the obtained pellets were placed in a vacuum vibration reactor VVD-30 (manufactured by Okawara Seisakusho Co., Ltd.) and heated to 160°C. After evacuation, F2 gas diluted to 20 % by volume with N2 gas was introduced to atmospheric pressure. After 0.5 hours from the introduction of the F2 gas, the chamber was once evacuated, and the F2 gas was introduced again. Further, after 0.5 hours, the chamber was evacuated again and F 2 gas was introduced again. Thereafter, the F 2 gas introduction and evacuation operations were continued once an hour, and the reaction was carried out at a temperature of 160° C. for 5 hours. After completion of the reaction, the interior of the reactor was sufficiently replaced with N2 gas to complete the fluorination reaction. Using the fluorinated pellets, various physical properties were measured by the methods described above.
- Comparative example 3 1.79 kg of PPVE, 6.61 kg of methanol, 0.051 kg of a 50% methanol solution of di-n-propylperoxydicarbonate, and 0.042 kg of PPVE were added for every 1 kg of TFE supplied, vacuum vibration reactor. Fluorinated pellets were obtained in the same manner as in Comparative Example 2 except that the temperature was changed to 210°C and the reaction was changed to 210°C for 10 hours to obtain 41.0 kg of dry powder.
- Comparative example 4 2.37 kg of PPVE, 1.47 kg of methanol, and 0.052 kg of PPVE were added for every 1 kg of TFE supplied, the temperature of the vacuum vibration reactor was raised to 210° C., and the reaction was carried out at 210° C. for 10 hours. Fluorinated pellets were obtained in the same manner as in Comparative Example 2, except that 43.0 kg of dry powder was obtained.
- Comparative example 5 Fluorination was carried out in the same manner as in Comparative Example 2 except that 2.43 kg of PPVE, 1.22 kg of methanol, and 0.053 kg of PPVE were added for each 1 kg of TFE supplied, and 43.1 kg of dry powder was obtained. No pellets were obtained.
- Comparative example 6 2.37 kg of PPVE, 2.85 kg of methanol, 0.051 kg of a 50% methanol solution of di-n-propylperoxydicarbonate, and 0.052 kg of PPVE were added for every 1 kg of TFE supplied, and a vacuum vibration reactor was added. Fluorinated pellets were obtained in the same manner as in Comparative Example 2 except that the heating temperature was changed to 170° C. and the reaction was changed to 170° C. for 5 hours to obtain 43.0 kg of dry powder.
- Example 1 2.24 kg of PPVE, 0.83 kg of methanol, and 0.049 kg of PPVE were added for every 1 kg of TFE supplied, the temperature of the vacuum vibration reactor was raised to 180° C., and the reaction was carried out at 180° C. for 10 hours. Fluorinated pellets were obtained in the same manner as in Comparative Example 2, except that 42.9 kg of dry powder was obtained.
- Example 2 2.37 kg of PPVE, 0.76 kg of methanol, and 0.052 kg of PPVE were added for every 1 kg of TFE supplied. Fluorinated pellets were obtained in the same manner as in Comparative Example 2, except that 43.0 kg of dry powder was obtained.
- Example 3 2.49 kg of PPVE, 0.83 kg of methanol, and 0.054 kg of PPVE were added for every 1 kg of TFE supplied, the temperature of the vacuum vibration reactor was raised to 210° C., and the reaction was carried out at 210° C. for 10 hours. Fluorinated pellets were obtained in the same manner as in Comparative Example 2, except that 43.1 kg of dry powder was obtained. Using the pellets obtained in Examples and Comparative Examples, various physical properties were measured by the methods described above. Table 3 shows the results.
- Wear amount (mg) M1-M2 M1: Specimen weight after 1000 rotations (mg) M2: Specimen weight after 5000 rotations (mg)
- Carbon dioxide permeation coefficient A sheet-like specimen having a thickness of about 0.1 mm was produced using a pellet and heat press molding machine. Using the obtained test piece, according to the method described in JIS K7126-1: 2006, using a differential pressure type gas permeation meter (L100-5000 type gas permeation meter, manufactured by Systech Illinois), carbon dioxide permeability is measured. I made a measurement. Values for carbon dioxide permeability were obtained at a permeation area of 50.24 cm 2 , test temperature of 70° C., and test humidity of 0% RH. Using the obtained carbon dioxide permeability and the thickness of the test piece, the carbon dioxide permeability coefficient was calculated from the following equation.
- GTR Carbon dioxide permeability (cm 3 /(m 2 ⁇ 24 h ⁇ atm))
- d test piece thickness (mm)
- the creep resistance was measured according to the method described in ASTM D395 or JIS K6262:2013.
- a molded body having an outer diameter of 13 mm and a height of 8 mm was produced using a pellet and a heat press molding machine.
- a test piece having an outer diameter of 13 mm and a height of 6 mm was produced.
- the prepared test piece was compressed to a compressive deformation rate of 25% at room temperature using a compressing device. While the compressed test piece was fixed to the compression device, it was allowed to stand in an electric furnace at 80° C. for 72 hours. The compression device was removed from the electric furnace, and after cooling to room temperature, the test piece was removed.
- a sheet having a small load deflection rate at 80° C. has excellent thermal rigidity.
- Load deflection rate (%) a2/a1 x 100
- a1 Specimen thickness before test (mm)
- a2 Amount of deflection at 80°C (mm)
- the three notch test pieces obtained were attached to a stress crack test jig according to ASTM D1693, heated at 150 ° C. for 24 hours in an electric furnace, and then the notch and its surroundings were visually observed and the number of cracks was counted. rice field. A sheet that does not crack has excellent thermal deformation resistance even after being immersed in a chemical solution.
- ⁇ The number of cracks is 0
- ⁇ The number of cracks is 1 or more
- a copper conductor having a conductor diameter of 0.50 mm was extruded and coated with the copolymer with the following coating thickness using a 30 mm ⁇ wire coating molding machine (manufactured by Tanabe Plastic Machinery Co., Ltd.) to obtain a coated wire.
- the wire covering extrusion molding conditions are as follows.
- spark A spark tester (DENSOK HIGH FREQ SPARK TESTER) was installed online in the wire coating line, and the presence or absence of defects in the wire coating was evaluated at a voltage of 1500V. A case where no spark was observed after continuous molding for 1 hour was evaluated as a pass ( ⁇ ), and a case where a spark was detected was evaluated as a failure (x).
- a cylindrical test piece with a diameter of 2 mm was produced by melt-molding the pellets.
- the prepared test piece was set in a 6 GHz cavity resonator manufactured by Kanto Denshi Applied Development Co., Ltd., and measured with a network analyzer manufactured by Agilent Technologies.
- the dielectric loss tangent (tan ⁇ ) at 20° C. and 6 GHz was obtained by analyzing the measurement results with analysis software “CPMA” manufactured by Kanto Denshi Applied Development Co., Ltd. on a PC connected to a network analyzer.
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Abstract
Description
Rf-O-CF=CF2 (I)
(式中、Rfは、炭素数1~5のパーフルオロアルキル基を表す。)で表されるパーフルオロ(アルキルビニルエーテル)とからなるテトラフルオロエチレン共重合体であって、不安定末端基が炭素数106個あたり10~100個であり、前記不安定末端基のうち-COF及び/又は-COOHが炭素数106個あたり合計で10~100個であることを特徴とするテトラフルオロエチレン共重合体が記載されている。
I:吸光度
K:補正係数
t:フィルムの厚さ(mm)
ジノルマルプロピルパーオキシジカーボネート、ジイソプロピルパーオキシジカーボネート、ジsec-ブチルパーオキシジカーボネート、ジ-2-エトキシエチルパーオキシジカーボネートなどのジアルキルパーオキシカーボネート類;
t-ブチルパーオキシイソブチレート、t-ブチルパーオキシピバレートなどのパーオキシエステル類;
ジt-ブチルパーオキサイドなどのジアルキルパーオキサイド類;
ジ[フルオロ(またはフルオロクロロ)アシル]パーオキサイド類;
などが代表的なものとしてあげられる。
食品包装用フィルム、食品製造工程で使用する流体移送ラインのライニング材、パッキン、シール材、シート等の食品製造装置用流体移送部材;
薬品用の薬栓、包装フィルム、薬品製造工程で使用される流体移送ラインのライニング材、パッキン、シール材、シート等の薬液移送部材;
化学プラントや半導体工場の薬液タンクや配管の内面ライニング部材;
自動車の燃料系統並びに周辺装置に用いられるO(角)リング・チューブ・パッキン、バルブ芯材、ホース、シール材等、自動車のAT装置に用いられるホース、シール材等の燃料移送部材;
自動車のエンジン並びに周辺装置に用いられるキャブレターのフランジガスケット、シャフトシール、バルブステムシール、シール材、ホース等、自動車のブレーキホース、エアコンホース、ラジエーターホース、電線被覆材等のその他の自動車部材;
半導体製造装置のO(角)リング、チューブ、パッキン、バルブ芯材、ホース、シール材、ロール、ガスケット、ダイヤフラム、継手等の半導体装置用薬液移送部材;
塗装設備用の塗装ロール、ホース、チューブ、インク用容器等の塗装・インク用部材;
飲食物用のチューブ又は飲食物用ホース等のチューブ、ホース、ベルト、パッキン、継手等の飲食物移送部材、食品包装材、ガラス調理機器;
廃液輸送用のチューブ、ホース等の廃液輸送用部材;
高温液体輸送用のチューブ、ホース等の高温液体輸送用部材;
スチーム配管用のチューブ、ホース等のスチーム配管用部材;
船舶のデッキ等の配管に巻き付けるテープ等の配管用防食テープ;
電線被覆材、光ファイバー被覆材、太陽電池の光起電素子の光入射側表面に設ける透明な表面被覆材および裏面剤等の各種被覆材;
ダイヤフラムポンプのダイヤフラムや各種パッキン類等の摺動部材;
農業用フィルム、各種屋根材・側壁等の耐侯性カバー;
建築分野で使用される内装材、不燃性防火安全ガラス等のガラス類の被覆材;
家電分野等で使用されるラミネート鋼板等のライニング材;
各単量体単位の含有量は、NMR分析装置(たとえば、ブルカーバイオスピン社製、AVANCE300 高温プローブ)により測定した。
ASTM D1238に従って、メルトインデクサーG-01(東洋精機製作所社製)を用いて、372℃、5kg荷重下で内径2.1mm、長さ8mmのノズルから10分間あたりに流出するポリマーの質量(g/10分)を求めた。
共重合体のペレットを、コールドプレスにより成形して、厚さ0.25~0.30mmのフィルムを作製した。このフィルムをフーリエ変換赤外分光分析装置〔FT-IR(Spectrum One、パーキンエルマー社製)〕により40回スキャンし、分析して赤外吸収スペクトルを得、完全にフッ素化されて官能基が存在しないベーススペクトルとの差スペクトルを得た。この差スペクトルに現れる特定の官能基の吸収ピークから、下記式(A)に従って試料における炭素原子1×106個あたりの官能基数Nを算出した。
N=I×K/t (A)
I:吸光度
K:補正係数
t:フィルムの厚さ(mm)
参考までに、本開示における官能基について、吸収周波数、モル吸光係数および補正係数を表2に示す。モル吸光係数は低分子モデル化合物のFT-IR測定データから決定したものである。
示差走査熱量計(商品名:X-DSC7000、日立ハイテクサイエンス社製)を用いて、昇温速度10℃/分で200℃から350℃までの1度目の昇温を行い、続けて、冷却速度10℃/分で350℃から200℃まで冷却し、再度、昇温速度10℃/分で200℃から350℃までの2度目の昇温を行い、2度目の昇温過程で生ずる溶融曲線ピークから融点を求めた。
174L容積のオートクレーブに純水51.8Lを投入し、充分に窒素置換を行った後、パーフルオロシクロブタン40.9kgとパーフルオロ(プロピルビニルエーテル)(PPVE)2.75kgを仕込み、系内の温度を35℃、攪拌速度を200rpmに保った。次いで、テトラフルオロエチレン(TFE)を0.64MPaまで圧入した後、ジ-n-プロピルパーオキシジカーボネートの50%メタノール溶液0.103kgを投入して重合を開始した。重合の進行とともに系内圧力が低下するので、TFEを連続供給して圧力を一定にし、PPVEをTFEの供給1kg毎に0.058kg追加投入した。TFEの追加投入量が40.9kgに達したところで重合を終了させた。未反応のTFEを放出して、オートクレーブ内を大気圧に戻した後、得られた反応生成物を水洗、乾燥して43.3kgの粉末を得た。
174L容積のオートクレーブに純水51.8Lを投入し、充分に窒素置換を行った後、パーフルオロシクロブタン40.9kgとパーフルオロ(プロピルビニルエーテル)(PPVE)2.05kとメタノール2.12kgを仕込み、系内の温度を35℃、攪拌速度を200rpmに保った。次いで、テトラフルオロエチレン(TFE)を0.64MPaまで圧入した後、ジ-n-プロピルパーオキシジカーボネートの50%メタノール溶液0.103kgを投入して重合を開始した。重合の進行とともに系内圧力が低下するので、TFEを連続供給して圧力を一定にし、PPVEをTFEの供給1kg毎に0.046kg追加投入した。TFEの追加投入量が40.9kgに達したところで重合を終了させた。未反応のTFEを放出して、オートクレーブ内を大気圧に戻した後、得られた反応生成物を水洗、乾燥して42.8kgの粉末を得た。
PPVEを1.79kg、メタノールを6.61kg、ジ-n-プロピルパーオキシジカーボネートの50%メタノール溶液を0.051kg、PPVEをTFEの供給1kg毎に0.042kg追加投入、真空振動式反応装置の昇温温度を210℃、反応を210℃の温度下で10時間に変更し、乾燥粉末41.0kgを得た以外は、比較例2と同様にして、フッ素化したペレットを得た。
PPVEを2.37kg、メタノールを1.47kg、PPVEをTFEの供給1kg毎に0.052kg追加投入、真空振動式反応装置の昇温温度を210℃、反応を210℃の温度下で10時間に変更し、乾燥粉末43.0kgを得た以外は、比較例2と同様にして、フッ素化したペレットを得た。
PPVEを2.43kg、メタノールを1.22kg、PPVEをTFEの供給1kg毎に0.053kg追加投入に変更し、乾燥粉末43.1kgを得た以外は、比較例2と同様にして、フッ素化していないペレットを得た。
PPVEを2.37kg、メタノールを2.85kg、ジ-n-プロピルパーオキシジカーボネートの50%メタノール溶液を0.051kg、PPVEをTFEの供給1kg毎に0.052kg追加投入、真空振動式反応装置の昇温温度を170℃、反応を170℃の温度下で5時間に変更し、乾燥粉末43.0kgを得た以外は、比較例2と同様にして、フッ素化したペレットを得た。
PPVEを2.24kg、メタノールを0.83kg、PPVEをTFEの供給1kg毎に0.049kg追加投入、真空振動式反応装置の昇温温度を180℃、反応を180℃の温度下で10時間に変更し、乾燥粉末42.9kgを得た以外は、比較例2と同様にして、フッ素化したペレットを得た。
PPVEを2.37kg、メタノールを0.76kg、PPVEをTFEの供給1kg毎に0.052kg追加投入、真空振動式反応装置の昇温温度を210℃、反応を210℃の温度下で10時間に変更し、乾燥粉末43.0kgを得た以外は、比較例2と同様にして、フッ素化したペレットを得た。
PPVEを2.49kg、メタノールを0.83kg、PPVEをTFEの供給1kg毎に0.054kg追加投入、真空振動式反応装置の昇温温度を210℃、反応を210℃の温度下で10時間に変更し、乾燥粉末43.1kgを得た以外は、比較例2と同様にして、フッ素化したペレットを得た。
実施例および比較例で得られたペレットを用いて、上記した方法により、各種物性を測定した。結果を表3に示す。
ペレットおよびヒートプレス成形機を用いて、厚さ約0.2mmのシート状試験片を作製し、これから10cm×10cmの試験片を切り出した。テーバー摩耗試験機(No.101 特型テーバー式アブレーションテスター、安田精機製作所社製)の試験台に作製した試験片を固定し、試験片表面温度150℃、荷重500g、摩耗輪CS-10(研磨紙#240で20回転研磨したもの)、回転速度60rpmの条件で、テーバー摩耗試験機を用いて摩耗試験を行った。1000回転後の試験片重量を計量し、同じ試験片でさらに5000回転試験後に試験片重量を計量した。次式により、摩耗量を求めた。
摩耗量(mg)=M1-M2
M1:1000回転後の試験片重量(mg)
M2:5000回転後の試験片重量(mg)
ペレットおよびヒートプレス成形機を用いて、厚さ約0.1mmのシート状試験片を作製した。得られた試験片を用い、JIS K7126-1:2006に記載の方法に従って、差圧式ガス透過度計(L100-5000型ガス透過度計、Systech illinois社製)を用いて、二酸化炭素透過度の測定を行った。透過面積50.24cm2、試験温度70℃、試験湿度0%RHでの二酸化炭素透過度の数値を得た。得られた二酸化炭素透過度と試験片厚みを用いて、次式より二酸化炭素透過係数を算出した。
二酸化炭素透過係数(cm3・mm/(m2・24h・atm))=GTR×d
GTR:二酸化炭素透過度(cm3/(m2・24h・atm))
d:試験片厚み(mm)
ペレットおよびヒートプレス成形機を用いて、厚さ約0.2mmのシート状試験片を作製した。試験カップ(透過面積12.56cm2)内にジメチルカーボネート(DMC)を10g入れ、シート状試験片で覆い、PTFEガスケットを挟んで締め付け、密閉した。シート状試験片とDMCが接するようにして、温度60℃で30日間保持した後取出し、室温で1時間放置後に質量減少量を測定した。次式により、DMC透過度(g・cm/m2)を求めた。
電解液透過度(g・cm/m2)=質量減少量(g)×シート状試験片の厚さ(cm)/透過面積(m2)
耐クリープ性の測定は、ASTM D395またはJIS K6262:2013に記載の方法に準じた。ペレットおよびヒートプレス成形機を用いて、外径13mm、高さ8mmの成形体を作製した。得られた成形体を切削することにより、外径13mm、高さ6mmの試験片を作製した。作製した試験片を、圧縮装置を用いて、常温で圧縮変形率25%まで圧縮した。圧縮した試験片を圧縮装置に固定したまま、電気炉内に静置し、80℃、72時間放置した。電気炉から圧縮装置を取り出し、室温まで冷却後、試験片を取り外した。回収した試験片を室温で30分放置した後、回収した試験片の高さを測定し、次式により復元割合を求めた。
復元割合(%)=(t2-t1)/t3×100
t1:スペーサーの高さ(mm)
t2:圧縮装置から取り外した試験片の高さ(mm)
t3:圧縮変形させた高さ(mm)
上記の試験においては、t1=4.5mm、t3=1.5mmである。
ペレットおよびヒートプレス成形機を用いて、厚さ約2mmのシート状試験片を作製し、これから80×10mmの試験片を切り出し、電気炉にて100℃で20時間加熱した。得られた試験片を用いた以外は、JIS K-K 7191-1に記載の方法に準じて、ヒートディストーションテスター(安田精機製作所社製)にて、試験温度30~150℃、昇温速度120℃/時間、曲げ応力1.8MPa、フラットワイズ法の条件にて試験を行った。次式により荷重たわみ率を求めた。80℃での荷重たわみ率が小さいシートは、熱時剛性に優れている。
荷重たわみ率(%)=a2/a1×100
a1:試験前の試験片厚み(mm)
a2:80℃でのたわみ量(mm)
ペレットおよびヒートプレス成形機を用いて、厚さ約2mmのシートを作製した。13.5mm×38mmの長方形ダンベルを用いて、得られたシートを打ち抜くことにより、3個の試験片を得た。得られた各試験片の長辺の中心に、ASTM D1693に準じて、19mm×0.45mmの刃でノッチを入れた。100mLポータブルリアクタ(TVS1型、耐圧ガラス工業社製)に、ノッチ試験片3個とジメチルスルホキシド25gを入れ、電気炉にて150℃で20時間加熱後、ノッチ試験片を取り出した。得られたノッチ試験片3個をASTM D1693に準じた応力亀裂試験治具に取り付け、電気炉にて150℃で24時間加熱した後、ノッチおよびその周辺を目視で観察し、亀裂の数を数えた。亀裂が生じないシートは、薬液に浸漬された後でも耐熱変形性が優れている。
○:亀裂の数が0個である
×:亀裂の数が1個以上である
射出成形機(住友重機械工業社製、SE50EV-A)を使用し、シリンダ温度を390℃、金型温度を170℃、射出速度50mm/sとして、共重合体を射出成形した。金型として、HPM38にCrめっきを施した金型(100mm×100mm×2.5mmt)を用いた。射出成形体の表面を目視で観察し、表面平滑性を以下の基準で評価した。
2:表面に荒れが観察されず平滑である
1:金型のゲート付近に位置していた部分の表面のみに荒れが観察される
0:表面の大部分に荒れが観察される
30mmφ電線被覆成形機(田辺プラスチック機械社製)により、導体径0.50mmの銅導体上に、下記被覆厚みで共重合体を押出被覆し、被覆電線を得た。電線被覆押出成形条件は以下の通りである。
a)心導体:導体径0.50mm
b)被覆厚み:0.15mm
c)被覆電線径:0.80mm
d)電線引取速度:150m/分
e)押出条件:
・シリンダー軸径=30mm,L/D=22の単軸押出成形機
・ダイ(内径)/チップ(外径)=8.0mm/5.0mm
押出機の設定温度:バレル部C-1(330℃)、バレル部C-2(360℃)、バレル部C-3(375℃)、ヘッド部H(390℃)、ダイ部D-1(405℃)、ダイ部D-2(395℃)。心線予備加熱は80℃に設定した。
電線府被覆成形を連続的に行い、1時間で1回以上、被覆切れが起こった場合を連続成形不可(×)、被覆切れが起こらなかった場合、連続成形可(○)とした。
電線被覆ラインにオンラインでスパークテスタ(DENSOK HIGH FREQ SPARK TESTER)を設置し、電圧1500Vで、電線被覆の欠損の有無を評価した。1時間連続成形してスパークがゼロの場合を合格(○)、スパークが検出された場合を不合格(×)とした。
ペレットを、溶融成形することにより、直径2mmの円柱状の試験片を作製した。作製した試験片を、関東電子応用開発社製6GHz用空洞共振器にセットし、アジレントテクノロジー社製ネットワークアナライザで測定した。測定結果を、ネットワークアナライザに接続されたPC上の関東電子応用開発社製解析ソフト「CPMA」で解析することにより、20℃、6GHzでの誘電正接(tanδ)を求めた。
Claims (4)
- テトラフルオロエチレン単位およびパーフルオロ(プロピルビニルエーテル)単位を含有し、
パーフルオロ(プロピルビニルエーテル)単位の含有量が、全単量体単位に対して、4.6~5.2質量%であり、
372℃におけるメルトフローレートが、22.0~28.0g/10分であり、
官能基数が、主鎖炭素数106個あたり、50個以下である
共重合体。 - 請求項1に記載の共重合体を含有する射出成形体。
- 請求項1に記載の共重合体を含有する被覆層を備える被覆電線。
- 請求項1に記載の共重合体を含有する成形体であって、前記成形体が、マイクロチューブ、容器、配管部材、または電線被覆である成形体。
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