WO2020255829A1 - 樹脂組成物、光ファイバのセカンダリ被覆材料、光ファイバ及び光ファイバの製造方法 - Google Patents
樹脂組成物、光ファイバのセカンダリ被覆材料、光ファイバ及び光ファイバの製造方法 Download PDFInfo
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- WO2020255829A1 WO2020255829A1 PCT/JP2020/022886 JP2020022886W WO2020255829A1 WO 2020255829 A1 WO2020255829 A1 WO 2020255829A1 JP 2020022886 W JP2020022886 W JP 2020022886W WO 2020255829 A1 WO2020255829 A1 WO 2020255829A1
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- WIPO (PCT)
- Prior art keywords
- meth
- acrylate
- resin composition
- optical fiber
- resin layer
- Prior art date
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- 239000011342 resin composition Substances 0.000 title claims abstract description 65
- 239000013307 optical fiber Substances 0.000 title claims description 52
- 239000011248 coating agent Substances 0.000 title claims description 26
- 238000000576 coating method Methods 0.000 title claims description 26
- 238000000034 method Methods 0.000 title claims description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000463 material Substances 0.000 title claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 100
- 150000001875 compounds Chemical class 0.000 claims abstract description 30
- 239000003999 initiator Substances 0.000 claims abstract description 15
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims description 103
- 239000011347 resin Substances 0.000 claims description 103
- -1 methacryloyl group Chemical group 0.000 claims description 30
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 29
- 239000003365 glass fiber Substances 0.000 claims description 20
- 229920000642 polymer Polymers 0.000 claims description 13
- 125000004122 cyclic group Chemical group 0.000 claims description 10
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims description 6
- 125000005073 adamantyl group Chemical group C12(CC3CC(CC(C1)C3)C2)* 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 91
- 239000002245 particle Substances 0.000 description 30
- 239000000178 monomer Substances 0.000 description 21
- 239000002612 dispersion medium Substances 0.000 description 18
- 230000005540 biological transmission Effects 0.000 description 14
- 239000003921 oil Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
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- 239000011164 primary particle Substances 0.000 description 10
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- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 7
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- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 5
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- 239000004593 Epoxy Substances 0.000 description 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 4
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 description 4
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- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 3
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- 230000000903 blocking effect Effects 0.000 description 3
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- 230000000052 comparative effect Effects 0.000 description 3
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- 230000003287 optical effect Effects 0.000 description 3
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- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 description 2
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- 239000007983 Tris buffer Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
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- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 description 2
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- LFOXEOLGJPJZAA-UHFFFAOYSA-N [(2,6-dimethoxybenzoyl)-(2,4,4-trimethylpentyl)phosphoryl]-(2,6-dimethoxyphenyl)methanone Chemical compound COC1=CC=CC(OC)=C1C(=O)P(=O)(CC(C)CC(C)(C)C)C(=O)C1=C(OC)C=CC=C1OC LFOXEOLGJPJZAA-UHFFFAOYSA-N 0.000 description 1
- YSCDKUPSJMMGGT-UHFFFAOYSA-L [dibutyl-[2-(6-methylheptylsulfanyl)acetyl]oxystannyl] 2-(6-methylheptylsulfanyl)acetate Chemical compound CC(C)CCCCCSCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CSCCCCCC(C)C YSCDKUPSJMMGGT-UHFFFAOYSA-L 0.000 description 1
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 description 1
- KORSJDCBLAPZEQ-UHFFFAOYSA-N dicyclohexylmethane-4,4'-diisocyanate Chemical compound C1CC(N=C=O)CCC1CC1CCC(N=C=O)CC1 KORSJDCBLAPZEQ-UHFFFAOYSA-N 0.000 description 1
- OTARVPUIYXHRRB-UHFFFAOYSA-N diethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](C)(OCC)CCCOCC1CO1 OTARVPUIYXHRRB-UHFFFAOYSA-N 0.000 description 1
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical group O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 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
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- KPSSIOMAKSHJJG-UHFFFAOYSA-N neopentyl alcohol Chemical compound CC(C)(C)CO KPSSIOMAKSHJJG-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 125000005581 pyrene group Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- XLKZJJVNBQCVIX-UHFFFAOYSA-N tetradecane-1,14-diol Chemical compound OCCCCCCCCCCCCCCO XLKZJJVNBQCVIX-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 description 1
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-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
- 125000002221 trityl group Chemical group [H]C1=C([H])C([H])=C([H])C([H])=C1C([*])(C1=C(C(=C(C(=C1[H])[H])[H])[H])[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 229940042596 viscoat Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/10—Epoxy resins modified by unsaturated compounds
-
- 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
- C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
- C08F299/02—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/104—Coating to obtain optical fibres
- C03C25/1065—Multiple coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/28—Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C03C25/285—Acrylic resins
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/32—Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/42—Coatings containing inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/465—Coatings containing composite materials
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
- C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
-
- 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
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
-
- 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
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
- C08F290/067—Polyurethanes; Polyureas
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/02395—Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Definitions
- the present disclosure relates to resin compositions, secondary coating materials for optical fibers, optical fibers and methods for producing optical fibers.
- This application claims priority based on Japanese Application No. 2019-11478 filed on June 19, 2019, and incorporates all the contents described in the Japanese application.
- an optical fiber has a coating resin layer for protecting a glass fiber which is an optical transmitter.
- An optical fiber is required to have excellent lateral pressure characteristics in order to reduce an increase in transmission loss induced by minute bending generated when a lateral pressure is applied to the optical fiber.
- the coating resin layer can be formed by using an ultraviolet curable resin composition containing a photopolymerizable compound, a photopolymerization initiator, and the like.
- an ultraviolet curable resin composition containing a photopolymerizable compound e.g., a photopolymerization initiator, and the like.
- Patent Document 1 it is studied to improve the lateral pressure characteristics of an optical fiber by forming a resin layer using an ultraviolet curable resin composition containing a filler made of synthetic quartz as a raw material.
- the resin composition according to one aspect of the present disclosure contains a photopolymerizable compound containing urethane (meth) acrylate and polyrotaxane, and a photopolymerization initiator, and the content of polyrotaxane is the total amount of the photopolymerizable compound. As a reference, it is 0.05% by mass or more and 11% by mass or less.
- FIG. 1 is a schematic cross-sectional view showing an example of an optical fiber according to the present embodiment.
- the coating resin layer generally includes a primary resin layer and a secondary resin layer.
- the resin composition forming the secondary resin layer is required to improve the lateral pressure characteristics of the optical fiber by increasing Young's modulus.
- increasing the Young's modulus of the secondary resin layer causes a decrease in the toughness of the resin layer, which causes cracks in the resin layer during screening of the optical fiber, which causes an increase in loss in the reliability test.
- the optical fiber is often used by being housed in a cable in a state of being immersed in a jelly containing oil. When the optical fiber is immersed in jelly, the coating resin layer absorbs oil, the adhesion of the coating resin layer to the glass fiber is reduced, and the transmission characteristics may be deteriorated. Therefore, the coating resin layer is required to have excellent oil resistance.
- An object of the present disclosure is to provide a resin composition having excellent oil resistance and capable of forming a resin layer capable of improving the lateral pressure characteristics of an optical fiber, and an optical fiber having excellent oil resistance and lateral pressure characteristics.
- the resin composition according to one aspect of the present disclosure contains a photopolymerizable compound containing urethane (meth) acrylate and polyrotaxane, and a photopolymerization initiator, and the content of polyrotaxane is the total amount of the photopolymerizable compound. As a reference, it is 0.05% by mass or more and 11% by mass or less.
- Polyrotaxane is a compound composed of a linear polymer and a cyclic molecule.
- the linear polymer is skewered into the opening of the cyclic molecule and has blocking groups at both ends so that the cyclic molecule is not detached.
- the cyclic molecule may have a UV curable group.
- the polyrotaxane may contain a cyclic molecule having at least one ultraviolet curable group selected from the group consisting of an acryloyl group, a methacryloyl group and a vinyl group.
- the polyrotaxane may contain a linear polymer having an adamantyl group because it is easy to improve the toughness of the resin layer.
- the resin composition according to the present embodiment may further contain an inorganic oxide from the viewpoint of producing an optical fiber having further excellent oil resistance and lateral pressure characteristics.
- the secondary coating material for the optical fiber according to one aspect of the present disclosure includes the above resin composition.
- a resin layer having excellent oil resistance can be formed.
- the optical fiber according to one aspect of the present disclosure includes a glass fiber including a core and a clad, a primary resin layer that is in contact with the glass fiber and coats the glass fiber, and a secondary resin layer that coats the primary resin layer.
- the resin layer is made of a cured product of the above resin composition.
- the method for producing an optical fiber according to one aspect of the present disclosure includes a coating step of applying the above resin composition to the outer periphery of a glass fiber composed of a core and a clad, and a resin composition by irradiating ultraviolet rays after the coating step. Includes a curing step of curing an object. As a result, a resin layer having an excellent balance between strength and toughness can be formed, and an optical fiber having excellent oil resistance and lateral pressure characteristics can be produced.
- the resin composition according to the present embodiment contains a photopolymerizable compound containing urethane (meth) acrylate and polyrotaxane, and a photopolymerization initiator.
- the polyrotaxane according to the present embodiment is a compound composed of a linear polymer and a cyclic molecule.
- the polyrotaxane may be UV curable.
- polyrotaxane has an ultraviolet curable group, it can form a covalent bond with a photopolymerizable compound such as urethane (meth) acrylate.
- the linear polymer has a linear main chain and a blocking group bonded to both ends of the main chain.
- the polymer constituting the main chain of the linear polymer include polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, polypropylene glycol, polyisobutylene, polyisobutylene, polybutadiene, polytetrahydrofuran, polydimethylsiloxane, polyacrylamide, and polyolefin.
- polyester examples of the blocking group include a dinitrophenyl group, an adamantyl group, a trityl group, a fluorescein group, and a pyrene group.
- the linear polymer preferably has a main chain based on polyethylene glycol and an adamantyl group as a sealing group.
- the weight average molecular weight (Mw) of the linear polymer is preferably 3000 or more and 80,000 or less, more preferably 5000 or more and 60,000 or less, and further preferably 10,000 or more and 40,000 or less.
- Examples of the cyclic molecule include a cyclodextrin compound and a crown ether compound.
- the cyclic molecule may have an ultraviolet curable group, and examples of the ultraviolet curable group include an acryloyl group, a metaacryloyl group, and a vinyl group.
- the Mw of the polyrotaxane according to the present embodiment is preferably 100,000 or more and 1500,000 or less, more preferably 140000 or more and 130000 or less, and further preferably 160000 or more and 120000 or less. Mw can be measured by the GPC method.
- SELM superpolymers As polyrotaxane, SELM superpolymers “SM3403P”, “SM2403P”, “SM1303P”, “SA3403P”, “SA2403P”, “SA1303”, “SA2405P-10”, “SA2405P-20”, Advanced Soft Materials Co., Ltd.
- Commercially available products such as “SA1305P-10” and “SA1305P-20” can be used.
- the content of polyrotaxane is 0.05% by mass or more, preferably 0.08% by mass or more, preferably 0.1% by mass or more, based on the total amount of the photopolymerizable compounds. More preferred. In order to improve the strength of the resin layer, the content of polyrotaxane is 11% by mass or less, preferably 10.5% by mass or less, and more preferably 10% by mass or less, based on the total amount of the photopolymerizable compounds.
- the urethane (meth) acrylate an oligomer obtained by reacting a polyol compound, a polyisocyanate compound and a hydroxyl group-containing (meth) acrylate compound can be used.
- the (meth) acrylate means an acrylate or a methacrylate corresponding thereto. The same applies to (meth) acrylic acid.
- Examples of the polyol compound include polytetramethylene glycol, polypropylene glycol and bisphenol A / ethylene oxide-added diol.
- Examples of the polyisocyanate compound include 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, isophorone diisocyanate, and dicyclohexylmethane 4,4'-diisocyanate.
- Examples of the hydroxyl group-containing (meth) acrylate compound include 2-hydroxyethyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 1,6-hexanediol mono (meth) acrylate, pentaerythritol tri (meth) acrylate, and the like. Examples thereof include 2-hydroxypropyl (meth) acrylate and tripropylene glycol mono (meth) acrylate.
- An organic tin compound is generally used as a catalyst for synthesizing urethane (meth) acrylate.
- the organotin compound include dibutyltin dilaurate, dibutyltin diacetate, dibutyltinmalate, dibutyltinbis (2-ethylhexyl mercaptoacetate), dibutyltinbis (isooctyl mercaptoacetate), and dibutyltin oxide. From the viewpoint of easy availability or catalytic performance, it is preferable to use dibutyltin dilaurate or dibutyltin diacetate as the catalyst.
- a lower alcohol having 5 or less carbon atoms may be used when synthesizing urethane (meth) acrylate.
- the lower alcohol include methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-2-propanol, 1-pentanol, 2-pentanol, 3-pentanol, and the like. Examples include 2-methyl-1-butanol, 3-methyl-1-butanol, 2-methyl-2-butanol, 3-methyl-2-butanol, and 2,2-dimethyl-1-propanol.
- the photopolymerizable compound according to the present embodiment may further contain an epoxy (meth) acrylate.
- an epoxy (meth) acrylate an oligomer obtained by reacting an epoxy resin having two or more glycidyl groups with a compound having a (meth) acryloyl group can be used.
- the photopolymerizable compound according to the present embodiment may further contain a photopolymerizable compound (hereinafter, referred to as "monomer") other than polyrotaxane, urethane (meth) acrylate and epoxy (meth) acrylate.
- a photopolymerizable compound hereinafter, referred to as "monomer”
- the monomer a monofunctional monomer having one polymerizable group and a polyfunctional monomer having two or more polymerizable groups can be used. Two or more kinds of monomers may be mixed and used.
- Examples of the monofunctional monomer include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, n-butyl (meth) acrylate, s-butyl (meth) acrylate, and tert-butyl (meth) acrylate.
- Aminoalkyl (meth) acrylate monomers such as aminopropyl acrylate, N, N-dimethylaminoethyl (meth) acrylate, tert-butylaminoethyl (meth) acrylate; N- (meth) acryloyloxymethylene succinimide , N- (meth) Acrylamide-6-oxyhexamethylene succinimide, N- (meth) acrylate-8-oxyoctamethylene succinimide and other succinimide-based monomers.
- polyfunctional monomer examples include ethylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, polypropylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, and tripropylene glycol di (meth) acrylate.
- Di (meth) acrylate of alkylene oxide adduct of bisphenol A tetraethylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate of hydroxypivalate, 1,4-butanediol di (meth) acrylate, 1,6 -Hexanediol di (meth) acrylate, 1,9-nonanediol di (meth) acrylate, 1,12-dodecanediol di (meth) acrylate, 1,14-tetradecanediol di (meth) acrylate, 1,16-hexadecane EO addition of diol di (meth) acrylate, 1,20-eicosane diol di (meth) acrylate, isopentyl diol di (meth) acrylate, 3-ethyl-1,8-octane diol di (meth) acrylate, bisphenol A
- Photopolymerization initiator As the photopolymerization initiator, it can be appropriately selected and used from known radical photopolymerization initiators. Examples of the photopolymerization initiator include 1-hydroxycyclohexylphenyl ketone (Omnirad 184, manufactured by IGM Resins), 2,2-dimethoxy-2-phenylacetophenone, 1- (4-isopropylphenyl) -2-hydroxy-2-.
- Methylpropan-1-one bis (2,6-dimethoxybenzoyl) -2,4,4-trimethylpentylphosphine oxide, 2-methyl-1- [4- (methylthio) phenyl] -2-morpholino-propane-1 -On (Omnirad 907, manufactured by IGM Resins), 2,4,6-trimethylbenzoyldiphenylphosphine oxide (Omnirad TPO, manufactured by IGM Resins), and bis (2,4,6-trimethylbenzoyl) phenylphosphine oxide (Omnirad). 819, manufactured by IGM Resins).
- the resin composition according to the present embodiment may further contain hydrophobic inorganic oxide particles.
- the surface of the inorganic oxide particles is hydrophobically treated.
- the hydrophobic treatment according to the present embodiment means that a hydrophobic group is introduced on the surface of the inorganic oxide particles.
- the inorganic oxide particles into which a hydrophobic group has been introduced are excellent in dispersibility in the resin composition.
- the hydrophobic group is a reactive group such as a (meth) acryloyl group or a vinyl group, or a non-reactive group such as an aliphatic hydrocarbon group (for example, an alkyl group) or an aromatic hydrocarbon group (for example, a phenyl group). It may be a group. When the inorganic oxide particles have a reactive group, it becomes easy to form a resin layer having a high Young's modulus.
- the inorganic oxide particles according to this embodiment are dispersed in a dispersion medium.
- the inorganic oxide particles can be uniformly dispersed in the resin composition, and the storage stability of the resin composition can be improved.
- the dispersion medium is not particularly limited as long as it does not inhibit the curing of the resin composition.
- the dispersion medium may be reactive or non-reactive.
- a monomer such as a (meth) acryloyl compound or an epoxy compound
- examples of the (meth) acryloyl compound include 1,6-hexanediol di (meth) acrylate, EO-modified bisphenol A di (meth) acrylate, polyethylene glycol di (meth) acrylate, and PO-modified bisphenol A di (meth) acrylate. Examples thereof include polypropylene glycol di (meth) acrylate and polytetramethylene glycol di (meth) acrylate.
- the (meth) acryloyl compound the compound exemplified by the above-mentioned monomer may be used.
- a ketone solvent such as methyl ethyl ketone (MEK), an alcohol solvent such as methanol (methanol), or an ester solvent such as propylene glycol monomethyl ether acetate (PGMEA) may be used.
- MEK methyl ethyl ketone
- methanol methanol
- PMEA propylene glycol monomethyl ether acetate
- the base resin and the inorganic oxide particles dispersed in the dispersion medium may be mixed, and then a part of the dispersion medium may be removed to prepare a resin composition.
- an optical microscope magnification of about 100 times
- the inorganic oxide particles dispersed in the dispersion medium exist in a dispersed state in the resin layer even after the resin composition is cured.
- a reactive dispersion medium used, the inorganic oxide particles are mixed with the resin composition together with the dispersion medium and incorporated into the resin layer while maintaining the dispersed state.
- a non-reactive dispersion medium used, at least a part of the dispersion medium volatilizes from the resin composition and disappears, but the inorganic oxide particles remain in the resin composition in a dispersed state and the cured resin layer. Also exists in a dispersed state.
- the inorganic oxide particles existing in the resin layer are observed in a state in which the primary particles are dispersed when observed with an electron microscope.
- the inorganic oxide particles are silicon dioxide (silica), zirconium dioxide (zirconia), aluminum oxide (alumina), magnesium oxide (alumina) because they have excellent dispersibility in the resin composition and easily form a tough resin layer. It is preferable that the particles contain at least one species from the group consisting of magnesia), titanium oxide (titania), tin oxide and zinc oxide. Hydrophobic silica particles are used as the inorganic oxide particles according to the present embodiment from the viewpoints of excellent low cost, easy surface treatment, ultraviolet transmission, and easy to impart appropriate hardness to the resin layer. It is more preferable to use it.
- the average primary particle size of the inorganic oxide particles may be 200 nm or less, 100 nm or less, 50 nm or less, or 30 nm or less. From the viewpoint of increasing the Young's modulus of the secondary resin layer, the average primary particle size of the inorganic oxide particles may be 1 nm or more, 5 nm or more, or 10 nm or more.
- the average primary particle size can be measured by, for example, image analysis of electron micrographs, a light scattering method, a BET method, or the like.
- the dispersion medium in which the primary particles of the inorganic oxide are dispersed looks transparent visually when the particle size of the primary particles is small. When the particle size of the primary particles is relatively large (40 nm or more), the dispersion medium in which the primary particles are dispersed appears cloudy, but no sediment is observed.
- the content of the inorganic oxide particles is 1% by mass or more and 60% by mass or less, 5% by mass or more and 50% by mass or less, or 10% by mass or more and 40% by mass or less based on the total amount of the photopolymerizable compound and the inorganic oxide particles. It may be.
- the content of the inorganic oxide particles is 1% by mass or more, the Young's modulus of the resin layer can be easily increased.
- the content of the inorganic oxide particles is 60% by mass or less, it becomes easy to impart toughness to the resin composition.
- the resin composition may further contain a silane coupling agent, a leveling agent, an antifoaming agent, an antioxidant, a sensitizer and the like.
- the silane coupling agent is not particularly limited as long as it does not interfere with the curing of the resin composition.
- examples of the silane coupling agent include tetramethyl silicate, tetraethyl silicate, mercaptopropyltrimethoxysilane, vinyltrichlorosilane, vinyltriethoxysilane, vinyltris ( ⁇ -methoxy-ethoxy) silane, and ⁇ - (3,4-epylcyclohexyl).
- -Ethyltrimethoxysilane dimethoxydimethylsilane, diethoxydimethylsilane, 3-acryloxypropyltrimethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -glycidoxypropylmethyldiethoxysilane, ⁇ -methacryloxypropyl Trimethoxysilane, N- ( ⁇ -aminoethyl) - ⁇ -aminopropyltrimethoxysilane, N- ( ⁇ -aminoethyl) - ⁇ -aminopropyltrimethyldimethoxysilane, N-phenyl- ⁇ -aminopropyltrimethoxysilane, ⁇ -Chloropropyltrimethoxysilane, ⁇ -mercaptopropyltrimethoxysilane, ⁇ -aminopropyltrimethoxysilane, bis- [3- (triethoxysilyl) prop
- the resin composition according to this embodiment can be suitably used as a secondary coating material for an optical fiber.
- a coated resin layer having excellent lateral pressure characteristics can be formed.
- FIG. 1 is a schematic cross-sectional view showing an example of an optical fiber according to the present embodiment.
- the optical fiber 10 includes a glass fiber 13 including a core 11 and a clad 12, and a coating resin layer 16 including a primary resin layer 14 and a secondary resin layer 15 provided on the outer periphery of the glass fiber 13.
- the clad 12 surrounds the core 11.
- the core 11 and the clad 12 mainly contain glass such as quartz glass.
- glass such as quartz glass.
- quartz glass to which germanium is added can be used for the core 11, and pure quartz glass or quartz to which fluorine is added to the clad 12. Glass can be used.
- the outer diameter (D2) of the glass fiber 13 is about 100 ⁇ m to 125 ⁇ m, and the diameter (D1) of the core 11 constituting the glass fiber 13 is about 7 ⁇ m to 15 ⁇ m.
- the thickness of the coating resin layer 16 is usually about 22 ⁇ m to 70 ⁇ m.
- the thickness of each of the primary resin layer 14 and the secondary resin layer 15 may be about 5 ⁇ m to 50 ⁇ m.
- the thickness of each layer of the primary resin layer 14 and the secondary resin layer 15 is about 10 ⁇ m to 50 ⁇ m.
- the thickness of the primary resin layer 14 may be 35 ⁇ m, and the thickness of the secondary resin layer 15 may be 25 ⁇ m.
- the outer diameter of the optical fiber 10 may be about 245 ⁇ m to 265 ⁇ m.
- the thickness of each layer of the primary resin layer 14 and the secondary resin layer 15 is about 10 ⁇ m to 38 ⁇ m.
- the thickness of the primary resin layer 14 may be 25 ⁇ m, and the thickness of the secondary resin layer 15 may be 10 ⁇ m.
- the outer diameter of the optical fiber 10 may be about 179 ⁇ m to 221 ⁇ m.
- the thickness of each layer of the primary resin layer 14 and the secondary resin layer 15 is about 5 ⁇ m to 32 ⁇ m.
- the thickness of the primary resin layer 14 may be 25 ⁇ m, and the thickness of the secondary resin layer 15 may be 10 ⁇ m.
- the outer diameter of the optical fiber 10 may be about 144 ⁇ m to 174 ⁇ m.
- the resin composition according to this embodiment can be applied to a secondary resin layer.
- the secondary resin layer can be formed by curing the above resin composition. Thereby, the lateral pressure characteristic of the optical fiber can be improved.
- the method for producing an optical fiber according to the present embodiment is a coating step of applying the above resin composition to the outer periphery of a glass fiber composed of a core and a clad, and a coating step of applying ultraviolet rays after the coating step to apply the resin composition. Includes a curing step of curing.
- the Young's modulus of the secondary resin layer is preferably 1150 MPa or more and 2700 MPa or less, more preferably 1200 MPa or more and 2000 MPa or less, and further preferably 1300 MPa or more and 1800 MPa or less at 23 ° C.
- the Young's modulus of the secondary resin layer is 1150 MPa or more, the lateral pressure characteristics are easily improved, and when it is 2700 MPa or less, appropriate toughness can be imparted to the secondary resin layer, so that cracks or the like are less likely to occur in the secondary resin layer.
- the primary resin layer 14 can be formed by curing, for example, a resin composition containing a urethane (meth) acrylate, a monomer, a photopolymerization initiator and a silane coupling agent.
- a resin composition for the primary resin layer a conventionally known technique can be used.
- the urethane (meth) acrylate, monomer, photopolymerization initiator and silane coupling agent may be appropriately selected from the compounds exemplified in the above base resin.
- the resin composition forming the primary resin layer has a composition different from that of the base resin forming the secondary resin layer.
- multiple optical fibers are arranged in parallel and integrated with ribbon resin to form an optical fiber ribbon.
- the resin composition according to the present disclosure can also be used as a resin for ribbons. As a result, the oil resistance and lateral pressure characteristics of the optical fiber ribbon can be improved as in the case of the optical fiber.
- Urethane acrylate (UA) obtained by reacting polypropylene glycol, 2,4-tolylene diisocyanate and hydroxyethyl acrylate having a molecular weight of 1000 and epoxy acrylate (EA) were prepared.
- 2-phenoxyethyl acrylate (POA, trade name "Light acrylate PO-A” of Kyoeisha Chemical Co., Ltd.), isobornyl acrylate (trade name “IBXA” of Osaka Organic Chemical Industry Co., Ltd.), and tripropylene glycol.
- Diacrylate (TPGDA, trade name "Viscoat # 310HP” of Osaka Organic Industry Co., Ltd.) was prepared.
- Photopolymerization initiator As a photopolymerization initiator, 1-hydroxycyclohexylphenyl ketone and 2,4,6-trimethylbenzoyldiphenylphosphine oxide were prepared.
- Inorganic oxide particles As the inorganic oxide particles, a silica sol having a methacryloyl group and hydrophobic silica particles having an average primary particle size of 10 to 15 nm dispersed in MEK was prepared.
- Resin composition Polyrotaxane, urethane acrylate, epoxy acrylate, monomer and photopolymerization initiator were mixed in the blending amounts shown in Table 1 or Table 2 to prepare resin compositions of Examples 1 to 10 and Comparative Examples 1 to 3. Further, the resin composition of Example 11 was prepared by further mixing silica sol so as to have the content of silica particles shown in Table 2 and removing most of MEK as a dispersion medium under reduced pressure.
- the numerical value of polyrotaxane is the content (% by mass) based on the total amount of the photopolymerizable compound
- the numerical value of urethane acrylate, epoxy acrylate and monomer is that of urethane acrylate, epoxy acrylate and monomer.
- the content (% by mass) is based on the total amount
- the numerical value of the silica particles is the content (% by mass) based on the total amount of the photopolymerizable compound and the silica particles.
- urethane acrylate 75 parts by mass of urethane acrylate, 12 parts by mass of nonylphenol EO modified acrylate, 6 parts by mass of N-vinylcaprolactam, 2 parts by mass of 1,6-hexanediol diacrylate, 1 part by mass of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, And 1 part by mass of 3-mercaptopropyltrimethoxysilane were mixed to prepare a resin composition for the primary resin layer.
- a resin composition for a primary resin layer and a resin composition of Example or Comparative Example are applied to the outer periphery of a glass fiber having a diameter of 125 ⁇ m composed of a core and a clad for a secondary resin layer, and then irradiated with ultraviolet rays.
- the resin composition was cured to form a primary resin layer having a thickness of 35 ⁇ m and a secondary resin layer having a thickness of 25 ⁇ m on the outer periphery thereof to prepare an optical fiber.
- the line speed was 1500 m / min.
- the transmission loss of light having a wavelength of 1550 nm when an optical fiber was wound in a single layer on a bobbin having a diameter of 280 mm covered with sandpaper was measured by an OTDR (Optical Time Domain Reflectometer) method. Further, the transmission loss of light having a wavelength of 1550 nm when the optical fiber was wound in a single layer on a bobbin having a diameter of 280 mm without sandpaper was measured by the OTDR method.
- the difference in the measured transmission loss was obtained, and the case where the transmission loss difference was 0.6 dB / km or less was judged as the lateral pressure characteristic "OK", and the case where the transmission loss difference was more than 0.6 dB / km was judged as the lateral pressure characteristic "NG”. ..
- the optical fiber was immersed in a jelly heated to 85 ° C. for 60 days so that the entire coating resin layer was completely immersed.
- a jelly was obtained by adding a thickener to a mineral oil having a molecular weight of about 300 to 600.
- the transmission characteristics of the signal having a wavelength of 1550 nm were measured under the respective temperature conditions of 23 ° C. and ⁇ 40 ° C., and the transmission loss at 23 ° C. and ⁇ 40 ° C. was evaluated.
- "A” 0 when the difference (transmission loss difference) obtained by subtracting the transmission loss at 23 ° C from the transmission loss at -40 ° C is 0.05 dB / km or less (the transmission loss is smaller at -40 ° C).
- a case exceeding 0.05 dB / km was evaluated as "B".
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Abstract
Description
本出願は、2019年6月19日出願の日本出願第2019-113478号に基づく優先権を主張し、前記日本出願に記載された全ての記載内容を援用するものである。
被覆樹脂層は、一般にプライマリ樹脂層及びセカンダリ樹脂層を備えている。セカンダリ樹脂層を形成する樹脂組成物には、ヤング率を高めることで光ファイバの側圧特性を向上することが求められる。しかしながら、セカンダリ樹脂層の高ヤング率化は、樹脂層の靭性低下を引き起こすため、光ファイバのスクリーニング時に樹脂層に割れが生じ、信頼性試験におけるロス増の原因となる。また、光ファイバは、オイルを含んだジェリーに浸漬された状態でケーブルに収納されて使用されることが多い。光ファイバをジェリーに浸漬すると、被覆樹脂層がオイルを吸収し、ガラスファイバに対する被覆樹脂層の密着力が低下し、伝送特性が低下することがある。そのため、被覆樹脂層には、耐油性に優れることが求められる。
本開示によれば、耐油性に優れ、光ファイバの側圧特性を向上することができる樹脂層を形成できる樹脂組成物、及び、耐油性及び側圧特性に優れる光ファイバを提供することができる。
最初に、本開示の実施形態の内容を列記して説明する。本開示の一態様に係る樹脂組成物は、ウレタン(メタ)アクリレート及びポリロタキサンを含む光重合性化合物と、光重合開始剤と、を含有し、ポリロタキサンの含有量が、光重合性化合物の総量を基準として0.05質量%以上11質量%以下である。
本開示の実施形態に係る樹脂組成物及び光ファイバの具体例を、必要により図面を参照しつつ説明する。なお、本発明はこれらの例示に限定されず、特許請求の範囲によって示され、特許請求の範囲と均等の意味及び範囲内でのすべての変更が含まれることが意図される。以下の説明では、図面の説明において同一の要素には同一の符号を付し、重複する説明を省略する。
本実施形態に係る樹脂組成物は、ウレタン(メタ)アクリレート及びポリロタキサンを含む光重合性化合物と、光重合開始剤とを含有する。
本実施形態に係るポリロタキサンは、直鎖状高分子と環状分子とから構成される化合物である。ポリロタキサンは、紫外線硬化性であってもよい。ポリロタキサンが紫外線硬化性基を有する場合、ウレタン(メタ)アクリレート等の光重合性化合物と共有結合を形成することができる。
光重合開始剤としては、公知のラジカル光重合開始剤の中から適宜選択して使用することができる。光重合開始剤として、例えば、1-ヒドロキシシクロヘキシルフェニルケトン(Omnirad 184、IGM Resins社製)、2,2-ジメトキシ-2-フェニルアセトフェノン、1-(4-イソプロピルフェニル)-2-ヒドロキシ-2-メチルプロパン-1-オン、ビス(2,6-ジメトキシベンゾイル)-2,4,4-トリメチルペンチルホスフィンオキサイド、2-メチル-1-[4-(メチルチオ)フェニル]-2-モルホリノ-プロパン-1-オン(Omnirad 907、IGM Resins社製)、2,4,6-トリメチルベンゾイルジフェニルホスフィンオキシド(Omnirad TPO、IGM Resins社製)、及びビス(2,4,6-トリメチルベンゾイル)フェニルホスフィンオキシド(Omnirad 819、IGM Resins社製)が挙げられる。
本実施形態に係る樹脂組成物は、疎水性の無機酸化物粒子を更に含有してよい。無機酸化物粒子は、その表面が疎水処理されている。本実施形態に係る疎水処理とは、無機酸化物粒子の表面に疎水性の基が導入されていることをいう。疎水性の基が導入された無機酸化物粒子は、樹脂組成物中の分散性に優れている。疎水性の基は、(メタ)アクリロイル基、ビニル基等の反応性基、又は、脂肪族炭化水素基(例えば、アルキル基)、芳香族炭化水素基(例えば、フェニル基)等の非反応性基であってもよい。無機酸化物粒子が反応性基を有する場合、ヤング率が高い樹脂層を形成し易くなる。
図1は、本実施形態に係る光ファイバの一例を示す概略断面図である。光ファイバ10は、コア11及びクラッド12を含むガラスファイバ13と、ガラスファイバ13の外周に設けられたプライマリ樹脂層14及びセカンダリ樹脂層15を含む被覆樹脂層16とを備えている。
(光重合性化合物)
アクリロイル基を有するポリロタキサンとして、アドバンスト・ソフトマテリアルズ株式会社の商品名「SA1303」(直鎖状高分子のMw:11000)、「SA2403P」(直鎖状高分子のMw:20000)、及び「SA3403P(直鎖状高分子のMw:35000)」を準備した。
光重合開始剤として、1-ヒドロキシシクロヘキシルフェニルケトン及び2,4,6-トリメチルベンゾイルジフェニルホスフィンオキシドを準備した。
無機酸化物粒子として、メタクリロイル基を有し、平均一次粒径が10~15nmである疎水性シリカ粒子がMEKに分散されたシリカゾルを準備した。
表1又は表2に示す配合量で、ポリロタキサン、ウレタンアクリレート、エポキシアクリレート、モノマー及び光重合開始剤を混合して、実施例1~10及び比較例1~3の樹脂組成物を作製した。また、実施例11の樹脂組成物は、表2に示すシリカ粒子の含有量となるように、シリカゾルを更に混合し、分散媒であるMEKの大部分を減圧除去して作製した。
スピンコータを用いて、樹脂組成物をポリエチレンテレフタレート(PET)フィルムの上に塗布した後、無電極UVランプシステム(ヘレウス製の「VPS600(Dバルブ)」)を用いて、1000±100mJ/cm2の条件で硬化させ、PETフィルム上に厚み200±20μmの樹脂層を形成した。樹脂層をPETフィルムから剥がし、樹脂フィルムを得た。樹脂フィルムをJIS K 7127 タイプ5のダンベル形状に打ち抜き、23±2℃、50±10%RHの条件下で、引張試験機を用いて1mm/分の引張速度、標線間25mmの条件で引張り、応力-歪み曲線を得た。2.5%割線によりヤング率を求めた。
(プライマリ樹脂層用の樹脂組成物)
オリゴマーとして、分子量4000のポリプロピレングリコール、イソホロンジイソシアネート、ヒドロキシエチルアクリレート及びメタノールを反応させて得られるウレタンアクリレートを準備した。ウレタンアクリレートを75質量部、ノニルフェノールEO変性アクリレート12質量部、N-ビニルカプロラクタム6質量部、1,6-ヘキサンジオールジアクリレート2質量部、2,4,6-トリメチルベンゾイルジフェニルホスフィンオキシド1質量部、及び3-メルカプトプロピルトリメトキシシラン1質量部を混合して、プライマリ樹脂層用の樹脂組成物を作製した。
コア及びクラッドから構成される直径125μmのガラスファイバの外周に、プライマリ樹脂層用の樹脂組成物と、実施例又は比較例の樹脂組成物をセカンダリ樹脂層用として塗布し、その後、紫外線を照射させることで樹脂組成物を硬化させ、厚さ35μmのプライマリ樹脂層とその外周に厚さ25μmのセカンダリ樹脂層を形成して光ファイバを作製した。線速は1500m/分とした。
サンドペーパーで表面を覆った280mm径のボビンに、光ファイバを単層状に巻き付けた時の1550nmの波長の光の伝送損失を、OTDR(Optical Time Domain Reflectometer)法により測定した。また、サンドペーパーのない280mm径のボビンに、光ファイバを単層状に巻き付けた時の1550nmの波長の光の伝送損失を、OTDR法により測定した。測定した伝送損失の差を求め、伝送損失差が0.6dB/km以下の場合を側圧特性「OK」と、伝送損失差が0.6dB/km超の場合を側圧特性「NG」と判断した。
光ファイバを、被覆樹脂層全体が完全に浸るように85℃に加熱したジェリーに60日間浸漬した。分子量が300~600程度の鉱油に増粘剤を添加したものをジェリーとした。23℃と-40℃のそれぞれの温度条件下で、波長1550nmの信号の伝送特性を測定し、23℃と-40℃とでの伝送損失の評価を行った。-40℃での伝送損失から23℃での伝送損失を引いた差(伝送損失差)が0.05dB/km以下(-40℃の方が伝送損失が小さい)の場合を「A」、0.05dB/km超の場合を「B」と評価した。
11 コア
12 クラッド
13 ガラスファイバ
14 プライマリ樹脂層
15 セカンダリ樹脂層
16 被覆樹脂層
Claims (7)
- ウレタン(メタ)アクリレート及びポリロタキサンを含む光重合性化合物と、光重合開始剤と、を含有する樹脂組成物であり、
前記ポリロタキサンの含有量が、前記光重合性化合物の総量を基準として0.05質量%以上11質量%以下である、光ファイバ被覆用の樹脂組成物。 - 前記ポリロタキサンが、アクリロイル基、メタクリロイル基及びビニル基からなる群より選ばれる少なくとも1種の紫外線硬化性基を有する環状分子を含む、請求項1に記載の樹脂組成物。
- 前記ポリロタキサンが、アダマンチル基を有する直鎖状高分子を含む、請求項1又は2に記載の樹脂組成物。
- 無機酸化物を更に含有する、請求項1から請求項3のいずれか一項に記載の樹脂組成物。
- 請求項1から請求項4のいずれか一項に記載の樹脂組成物を含む、光ファイバのセカンダリ被覆材料。
- コア及びクラッドを含むガラスファイバと、
前記ガラスファイバに接して前記ガラスファイバを被覆するプライマリ樹脂層と、
前記プライマリ樹脂層を被覆するセカンダリ樹脂層と、を備え、
前記セカンダリ樹脂層が、請求項1から請求項4のいずれか一項に記載の樹脂組成物の硬化物からなる、光ファイバ。 - コア及びクラッドを含むガラスファイバの外周に、請求項1から請求項4のいずれか一項に記載の樹脂組成物を塗布する塗布工程と、
前記塗布工程の後に紫外線を照射することにより前記樹脂組成物を硬化させる硬化工程と、
を含む、光ファイバの製造方法。
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