WO2022123969A1 - 樹脂組成物、光ファイバ及び光ファイバの製造方法 - Google Patents
樹脂組成物、光ファイバ及び光ファイバの製造方法 Download PDFInfo
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- WO2022123969A1 WO2022123969A1 PCT/JP2021/040597 JP2021040597W WO2022123969A1 WO 2022123969 A1 WO2022123969 A1 WO 2022123969A1 JP 2021040597 W JP2021040597 W JP 2021040597W WO 2022123969 A1 WO2022123969 A1 WO 2022123969A1
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- WIPO (PCT)
- Prior art keywords
- meth
- acrylate
- optical fiber
- resin composition
- resin layer
- Prior art date
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 72
- 239000011342 resin composition Substances 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 113
- 150000001875 compounds Chemical class 0.000 claims abstract description 42
- 239000011248 coating agent Substances 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 26
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims description 97
- 229920005989 resin Polymers 0.000 claims description 97
- -1 methacryloyl group Chemical group 0.000 claims description 39
- 239000003365 glass fiber Substances 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 24
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 22
- 229920000642 polymer Polymers 0.000 claims description 16
- 125000004122 cyclic group Chemical group 0.000 claims description 14
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 3
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical group C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 87
- 239000011800 void material Substances 0.000 description 20
- 239000002612 dispersion medium Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000000178 monomer Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 229920005862 polyol Polymers 0.000 description 13
- 150000003077 polyols Chemical class 0.000 description 13
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- 229920001223 polyethylene glycol Polymers 0.000 description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 7
- 230000000903 blocking effect Effects 0.000 description 7
- 229920001451 polypropylene glycol Polymers 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 125000005073 adamantyl group Chemical group C12(CC3CC(CC(C1)C3)C2)* 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 5
- 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 5
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 5
- 239000005056 polyisocyanate Substances 0.000 description 5
- 229920001228 polyisocyanate Polymers 0.000 description 5
- 239000011164 primary particle Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 4
- 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
- QPRQEDXDYOZYLA-UHFFFAOYSA-N 2-methylbutan-1-ol Chemical compound CCC(C)CO QPRQEDXDYOZYLA-UHFFFAOYSA-N 0.000 description 3
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 125000001165 hydrophobic group Chemical group 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229920000909 polytetrahydrofuran Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical group C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 2
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 2
- PGMMMHFNKZSYEP-UHFFFAOYSA-N 1,20-Eicosanediol Chemical compound OCCCCCCCCCCCCCCCCCCCCO PGMMMHFNKZSYEP-UHFFFAOYSA-N 0.000 description 2
- JWYVGKFDLWWQJX-UHFFFAOYSA-N 1-ethenylazepan-2-one Chemical compound C=CN1CCCCCC1=O JWYVGKFDLWWQJX-UHFFFAOYSA-N 0.000 description 2
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 description 2
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 2
- MXLMTQWGSQIYOW-UHFFFAOYSA-N 3-methyl-2-butanol Chemical compound CC(C)C(C)O MXLMTQWGSQIYOW-UHFFFAOYSA-N 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 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
- 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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- 150000002009 diols Chemical class 0.000 description 2
- GHLKSLMMWAKNBM-UHFFFAOYSA-N dodecane-1,12-diol Chemical compound OCCCCCCCCCCCCO GHLKSLMMWAKNBM-UHFFFAOYSA-N 0.000 description 2
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- 239000004615 ingredient Substances 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
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- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 2
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 2
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 2
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- AURYLBASVGNSON-UHFFFAOYSA-N (2,5-dioxopyrrolidin-3-ylidene)methyl prop-2-enoate Chemical compound C=CC(=O)OC=C1CC(=O)NC1=O AURYLBASVGNSON-UHFFFAOYSA-N 0.000 description 1
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
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- HIDBROSJWZYGSZ-UHFFFAOYSA-N 1-phenylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC=C1 HIDBROSJWZYGSZ-UHFFFAOYSA-N 0.000 description 1
- RESPXSHDJQUNTN-UHFFFAOYSA-N 1-piperidin-1-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCCCC1 RESPXSHDJQUNTN-UHFFFAOYSA-N 0.000 description 1
- WLPAQAXAZQUXBG-UHFFFAOYSA-N 1-pyrrolidin-1-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCCC1 WLPAQAXAZQUXBG-UHFFFAOYSA-N 0.000 description 1
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- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 1
- IAMASUILMZETHW-UHFFFAOYSA-N 2-(2-hydroxyethoxy)-1-phenoxyethanol;prop-2-enoic acid Chemical compound OC(=O)C=C.OCCOCC(O)OC1=CC=CC=C1 IAMASUILMZETHW-UHFFFAOYSA-N 0.000 description 1
- WMYINDVYGQKYMI-UHFFFAOYSA-N 2-[2,2-bis(hydroxymethyl)butoxymethyl]-2-ethylpropane-1,3-diol Chemical compound CCC(CO)(CO)COCC(CC)(CO)CO WMYINDVYGQKYMI-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
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- RZVINYQDSSQUKO-UHFFFAOYSA-N 2-phenoxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC1=CC=CC=C1 RZVINYQDSSQUKO-UHFFFAOYSA-N 0.000 description 1
- BYPFICORERPGJY-UHFFFAOYSA-N 3,4-diisocyanatobicyclo[2.2.1]hept-2-ene Chemical compound C1CC2(N=C=O)C(N=C=O)=CC1C2 BYPFICORERPGJY-UHFFFAOYSA-N 0.000 description 1
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- 125000006181 4-methyl benzyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1C([H])([H])[H])C([H])([H])* 0.000 description 1
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- CCOQPGVQAWPUPE-UHFFFAOYSA-N 4-tert-butylcyclohexan-1-ol Chemical compound CC(C)(C)C1CCC(O)CC1 CCOQPGVQAWPUPE-UHFFFAOYSA-N 0.000 description 1
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- ZMDDERVSCYEKPQ-UHFFFAOYSA-N Ethyl (mesitylcarbonyl)phenylphosphinate Chemical compound C=1C=CC=CC=1P(=O)(OCC)C(=O)C1=C(C)C=C(C)C=C1C ZMDDERVSCYEKPQ-UHFFFAOYSA-N 0.000 description 1
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- MBXULDRFQBQSSK-UHFFFAOYSA-N N'-[3-[methoxy-[(2-methylpropan-2-yl)oxy]silyl]propyl]ethane-1,2-diamine Chemical compound NCCNCCC[SiH](OC(C)(C)C)OC MBXULDRFQBQSSK-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- ZXZSYHLGFSXNNU-UHFFFAOYSA-N [[methyl(4-trimethoxysilylbutyl)carbamothioyl]trisulfanyl] N-methyl-N-(4-trimethoxysilylbutyl)carbamodithioate Chemical class CO[Si](CCCCN(C(=S)SSSSC(N(C)CCCC[Si](OC)(OC)OC)=S)C)(OC)OC ZXZSYHLGFSXNNU-UHFFFAOYSA-N 0.000 description 1
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-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
- 150000001298 alcohols Chemical class 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 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
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-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
- 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
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 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
- 239000011521 glass Substances 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
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 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
- 238000002156 mixing Methods 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
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-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
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 229920000728 polyester Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920000098 polyolefin 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
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- 125000005581 pyrene group Chemical group 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 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
- 150000004756 silanes Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 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
- 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 class 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
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-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
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
-
- 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
-
- 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
- C03C25/326—Polyureas; Polyurethanes
-
- 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
- C03C25/47—Coatings containing composite materials containing particles, fibres or flakes, e.g. in a continuous phase
-
- 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
- C03C25/62—Surface treatment of fibres or filaments made from glass, minerals or slags by application of electric or wave energy; by particle radiation or ion implantation
- C03C25/6206—Electromagnetic waves
- C03C25/6226—Ultraviolet
-
- 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
-
- 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
- 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
- C09D133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- 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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
Definitions
- the present disclosure relates to a resin composition for primary coating of an optical fiber, an optical fiber and a method for producing the optical fiber.
- the optical fiber is provided with a coating resin layer for protecting the 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 of the optical fiber 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
- Patent Document 1 it is studied to improve the lateral pressure characteristics of an optical fiber by forming a coated resin layer using an ultraviolet curable resin composition containing a filler made of synthetic quartz as a raw material.
- the resin composition for primary coating of an optical fiber contains a photopolymerizable compound, a photopolymerization initiator and a silane coupling agent, and the photopolymerizable compound is a urethane (meth) acrylate.
- the content of the polyrotaxan is 0.05% by mass or more and 11% by mass or less based on the total amount of the photopolymerizable compound, including the polyrotaxan having an ultraviolet curable property.
- the optical fiber according to one embodiment of the present disclosure includes a glass fiber including a core and a clad, a primary resin layer in contact with the glass fiber and covering the glass fiber, and a secondary resin layer covering the primary resin layer.
- the resin layer contains a cured product of the above resin composition.
- the method for producing an optical fiber according to one embodiment of the present disclosure includes a coating step of applying the above resin composition to the outer periphery of a glass fiber including a core and a clad, and a coating step of applying ultraviolet rays after the coating step to apply the resin composition. It comprises a curing step of curing.
- FIG. 1 is a schematic cross-sectional view showing an example of an optical fiber according to the present embodiment.
- the coated resin layer of the optical fiber generally includes a primary resin layer and a secondary resin layer. From the viewpoint of improving the lateral pressure characteristics of the optical fiber, it is desirable to reduce the Young's modulus of the primary resin layer. However, lowering the Young's modulus of the primary resin layer causes a decrease in the strength of the primary resin layer, which causes cross-linking breakage in the primary resin layer when screening the optical fiber, which causes an increase in loss in the reliability test of the optical fiber. Voids are likely to occur.
- a resin composition capable of forming a primary resin layer capable of improving the lateral pressure characteristics and void resistance characteristics of an optical fiber, and an optical fiber having excellent lateral pressure characteristics and void resistance characteristics are provided. Can be done.
- the resin composition for primary coating of an optical fiber contains a photopolymerizable compound, a photopolymerization initiator and a silane coupling agent, and the photopolymerizable compound is a urethane (meth) acrylate.
- the content of the polyrotaxan is 0.05% by mass or more and 11% by mass or less based on the total amount of the photopolymerizable compound, including the polyrotaxan having an ultraviolet curable property.
- Such a resin composition can form a primary resin layer capable of improving the lateral pressure characteristics and void resistance characteristics of the optical fiber. That is, since the primary resin layer formed by using the above-mentioned resin composition has a low Young's modulus, the lateral pressure characteristics of the optical fiber can be improved, and the stress applied to the optical fiber at the time of screening is made uniform to reduce the stress. By relaxing it, cross-linking and cutting in the primary resin layer can be suppressed, so that the void resistance characteristics of the optical fiber can be improved.
- the polyrotaxan contains 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. But it may be.
- the polyrotaxane may contain a linear polymer having an adamantane group from the viewpoint of further improving the lateral pressure characteristics and void resistance characteristics of the optical fiber.
- the resin composition may further contain inorganic oxide particles from the viewpoint of further improving the lateral pressure characteristics and void resistance characteristics of the optical fiber.
- 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 in contact with the glass fiber and covering the glass fiber, and a secondary resin layer covering the primary resin layer.
- the resin layer contains a cured product of the above resin composition.
- Such an optical fiber is excellent in lateral pressure characteristics and void resistance characteristics.
- 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 including a core and a clad, and a coating step of applying ultraviolet rays after the coating step to apply the resin composition. It comprises a curing step of curing.
- the resin composition according to the present embodiment contains a photopolymerizable compound, a photopolymerization initiator, and a silane coupling agent, and may further contain other components if necessary. Hereinafter, each component will be described in detail.
- Photopolymerizable compounds include urethane (meth) acrylates and UV curable polyrotaxanes.
- the urethane (meth) acrylate according to the present embodiment is not particularly limited as long as it is a urethane (meth) acrylate that can be used as a photopolymerizable compound in the resin composition for primary coating.
- the urethane (meth) acrylate is, for example, a reaction product of a polyol, a polyisocyanate, a hydroxyl group-containing (meth) acrylate, and one or more compounds selected from a monohydric alcohol and an active hydrogen-containing silane compound, if necessary. There may be.
- the (meth) acrylate means an acrylate or a methacrylate corresponding thereto. The same applies to (meth) acrylic acid.
- polystyrene resin examples include a polyether polyol, a polyester polyol, a polycaprolactone polyol, a polycarbonate polyol, a polybutadiene polyol, and a bisphenol A / ethylene oxide-added diol.
- polyether polyol examples include polytetramethylene ether glycol, polyethylene glycol, and polypropylene glycol. These polyols may be used alone or in combination of two or more. From the viewpoint of easily adjusting the Young's modulus of the primary resin layer, it is preferable to use at least one selected from the group consisting of polypropylene glycol, polytetramethylene ether glycol, and polycarbonate polyol as the polyol.
- the number average molecular weight (Mn) of the polyol is preferably 2000 or more and 20,000 or less, more preferably 2400 or more and 19000 or less, and 2800 or more and 18,000 or less. Is more preferable.
- polyisocyanate examples include 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, isophorone diisocyanate, dicyclohexylmethane diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, xylylene diisocyanate, hydrogenated xylylene diisocyanate, 1 , 5-Naphthalenediocyanate, norbornene diisocyanate, 1,5-pentamethylene diisocyanate, tetramethylxylylene diisocyanate, trimethylhexamethylene diisocyanate and the like. These polyisocyanates may be used alone or in combination of two or more.
- Examples of the hydroxyl group-containing (meth) acrylate include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, caprolactone (meth) acrylate, and 2-hydroxy-3-.
- Examples thereof include propandi (meth) acrylate and pentaerythritol tri (meth) acrylate.
- hydroxyl group-containing (meth) acrylates may be used alone or in combination of two or more.
- the hydroxyl group-containing (meth) acrylate it is preferable to use at least one selected from the group consisting of 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, and 2-hydroxybutyl (meth) acrylate.
- Examples of the monohydric alcohol include methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-2-propanol, 1-pentanol, 2-pentanol and 3-pentanol. , 2-Methyl-1-butanol, 3-methyl-1-butanol, 2-methyl-2-butanol, and 3-methyl-2-butanol. These monohydric alcohols may be used alone or in combination of two or more.
- Urethane (meth) acrylate reduces the proportion of (meth) acryloyloxy group at the end, which is a photopolymerizable group, by introducing a group based on a monohydric alcohol at the end of the urethane bond, and the Young's modulus of the primary resin layer. Can be reduced.
- Examples of the active hydrogen-containing silane compound include N-2- (aminoethyl) -3-aminopropylmethyldimethoxysilane, N-2- (aminoethyl) -3-aminopropyltrimethoxysilane, and 3-aminopropyltrimethoxy.
- active hydrogen-containing silane compounds may be used alone or in combination of two or more.
- Urethane (meth) acrylate reduces the terminal (meth) acryloyloxy group, which is a photopolymerizable group, by introducing a group based on an active hydrogen-containing silane compound at the end of the urethane bond, and the Young's modulus of the primary resin layer. Can be reduced, and the adhesion between the primary resin layer and the glass fiber can be improved.
- a method for synthesizing a urethane (meth) acrylate for example, one or more selected from a hydroxyl group-containing (meth) acrylate (if necessary, a monohydric alcohol and an active hydrogen-containing silane compound) after reacting a polyol with a polyisocyanate.
- Method of reacting with (a compound) of Method of reacting examples thereof include a method of simultaneously reacting a polyol, a polyisocyanate, and a hydroxyl group-containing (meth) acrylate (one or more compounds selected from a monohydric alcohol and an active hydrogen-containing silane compound, if necessary).
- an organotin compound and an amine compound may be 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.
- the Mn of the urethane (meth) acrylate is preferably 5,000 or more and 40,000 or less, more preferably 8,000 or more and 38,000 or less, and more preferably 10,000 or more and 37,000 or less, from the viewpoint of obtaining a young ratio suitable for the primary resin layer. Is more preferable.
- the content of urethane (meth) acrylate may be 10 parts by mass or more, 20 parts by mass or more, 30 parts by mass or more, or 40 parts by mass or more, based on 100 parts by mass of the total amount of the resin composition, and 90 parts by mass. It may be less than or equal to 80 parts by mass or less.
- Ultraviolet curable 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 to prevent the cyclic molecule from detaching.
- the cyclic molecule has an ultraviolet curable group. Since polyrotaxane has an ultraviolet curable group, it can form a covalent bond with a photopolymerizable compound such as urethane (meth) acrylate.
- urethane (meth) acrylate By introducing such a structure based on polyrotaxane into the primary resin layer, it is possible to suppress cross-linking in the primary resin layer by making the stress applied to the optical fiber uniform and relaxing the stress at the time of screening, and the optical fiber. Void resistance can be improved.
- 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, polyisoprene, 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 an adamantyl group as a blocking group, and has a main chain based on polyethylene glycol and adamantyl as a blocking group. It is more preferable to have a group.
- the polyrotaxane preferably contains a linear polymer having an adamantyl group as a blocking group, and contains a main chain based on polyethylene glycol and a linear polymer having an adamantyl group as a blocking group. Is more preferable.
- 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.
- the Mw of the linear polymer may be 35,000 or less, 30,000 or less, or 25,000 or less.
- the cyclic molecule examples include a cyclodextrin compound having an ultraviolet curable group and a crown ether compound having an ultraviolet curable group.
- the ultraviolet curable group contained in the cyclic molecule include an acryloyl group, a metaacryloyl group, and a vinyl group.
- the polyrotaxan contains 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.
- a cyclic molecule having at least one ultraviolet curable group selected from an acryloyl group and a methacryloyl group it is more preferable to contain a cyclic molecule having an acryloyl group.
- the (meth) of the polyrotaxane can further improve the lateral pressure property and the void resistance property of the optical fiber.
- the equivalent amount of the acryloyl group is preferably 2000 g / eq or more, more preferably 2500 g / eq or more, and further preferably 3000 g / eq or more.
- the Mw of polyrotaxane 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.
- the Mw of polyrotaxane may be 1,000,000 or less, 800,000 or less, 600,000 or less, or 500,000 or less. Mw can be measured by the GPC method.
- CELM Super Polymers "SM3403P”, “SM2403P”, “SM1303P”, “SM2405P-10”, “SM2405P-20”, “SM1305P-10”, “SM1305P-10” of Advanced Soft Materials Co., Ltd. , “SA3403P”, “SA2403P”, “SA1303P”, “SA2405P-10”, “SA2405P-20”, “SA1305P-10”, “SA1305P-20” and the like can be used.
- the content of polyrotaxane is 0.05% by mass or more and 11% by mass or less based on the total amount of the photopolymerizable compound from the viewpoint of improving the lateral pressure characteristics and void resistance characteristics of the optical fiber. From the viewpoint of further improving the void resistance of the optical fiber, the content of polyrotaxane is preferably 0.08% by mass or more, more preferably 0.1% by mass or more, based on the total amount of the photopolymerizable compound. .. From the viewpoint of further improving the lateral pressure characteristics of the optical fiber, the content of polyrotaxane is preferably 10% by mass or less, more preferably 8% by mass or less, and 6% by mass or less based on the total amount of the photopolymerizable compound.
- the content of polyrotaxane is 5% by mass or less, 4.5% by mass or less, 4% by mass or less, 3.5% by mass or less, 3% by mass or less, 2.5% by mass based on the total amount of photopolymerizable compounds. Hereinafter, it may be 2% by mass or less or 1.5% by mass or less.
- the photopolymerizable compound according to the present embodiment may further contain a photopolymerizable compound (hereinafter referred to as "monomer") other than urethane (meth) acrylate and polyrotaxane.
- a photopolymerizable compound hereinafter referred to as "monomer”
- a monofunctional monomer having one polymerizable group and a polyfunctional monomer having two or more polymerizable groups can be used.
- one type may be used alone, or two or more types may be used in combination.
- 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) acrylamide-8-oxyoctamethylene succinimide and the like.
- 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 trimethylolpropane 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, a known radical photopolymerization initiator can be appropriately selected and used. Examples of the photopolymerization initiator include 1-hydroxycyclohexylphenylketone (trade name: Omnirad 184, manufactured by IGM Resins), 2,2-dimethoxy-2-phenylacetophenone (trade name: Omnirad 651, manufactured by IGM Resins), and the like.
- silane coupling agent examples include tetramethylsilicate, tetraethylsilicate, mercaptopropyltrimethoxysilane, vinyltrichlorosilane, vinyltriethoxysilane, vinyltris ( ⁇ -methoxy-ethoxy) silane, and ⁇ - (3,4-epoxycyclohexyl).
- the resin composition according to the present embodiment may further contain inorganic oxide particles, a photoacid generator, a leveling agent, a defoaming agent, an antioxidant, an ultraviolet absorber and the like.
- the inorganic oxide particles may be hydrophobic inorganic oxide particles whose surface is hydrophobically treated.
- Hydrophobic treatment means that a hydrophobic group is introduced on the surface of the inorganic oxide particles.
- Inorganic oxide particles into which a hydrophobic group has been introduced are excellent in dispersibility in a resin composition.
- the hydrophobic group may be a reactive group such as a (meth) acryloyl group or a vinyl group, and may be an aliphatic hydrocarbon group (for example, an alkyl group), an aromatic hydrocarbon group (for example, a phenyl group) or the like. It may be a non-reactive group.
- Inorganic oxide particles may be 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 a reactive dispersion medium or a non-reactive dispersion medium.
- 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 state of being dispersed 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 the dispersed state is maintained.
- 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 dispersed state in the resin composition and the cured resin layer. It also exists in a dispersed state.
- the inorganic oxide particles present 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 include silicon dioxide (silica), zirconium dioxide (zirconia), aluminum oxide (alumina), magnesium oxide (magnesia), titanium oxide (titania), and oxidation. It is preferable that the particles contain at least one selected from the group consisting of tin and zinc oxide, and it is more preferable to use hydrophobic silica particles.
- the average primary particle size of the inorganic oxide particles may be 200 nm or less, 100 nm or less, or 80 nm or less, and may be 10 nm or more, 20 nm or more, or 30 nm or more.
- the average primary particle size can be measured by, for example, image analysis of an electron micrograph, a light scattering method, a BET method, or the like.
- 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. May be.
- the optical fiber according to the present embodiment 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.
- 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 coated 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 or pure quartz glass to which germanium is added can be used for the core 11, and pure quartz glass or pure quartz glass or pure quartz glass can be used for the clad 12. Quartz glass to which fluorine is added 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
- 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 8 ⁇ m to 38 ⁇ m.
- the thickness of the primary resin layer 14 may be 25 ⁇ m
- the thickness of the secondary resin layer 15 may be 10 ⁇ m.
- the outer diameter of the optical fiber 10 may be about 173 ⁇ 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
- 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 primary resin layer 14 contains a cured product of the resin composition according to the present embodiment.
- the primary resin layer 14 can be obtained by curing the resin composition according to the present embodiment. By providing such a primary resin layer 14, it is possible to improve the lateral pressure characteristics and the void resistance characteristics of the optical fiber.
- the Young's modulus of the primary resin layer 14 is preferably 0.8 MPa or less at 23 ° C. ⁇ 2 ° C., and more preferably 0.5 MPa or less.
- the Young's modulus of the primary resin layer 14 can be measured by the Pullout Modulus (POM) method at 23 ° C. Two points of the optical fiber were fixed by two chuck devices, the coated resin layer (primary resin layer and secondary resin layer) portion between the two chuck devices was removed, and then one chuck device was fixed and fixed. Gently move the other chuck device in the opposite direction of the chuck device.
- the length of the part sandwiched between the moving chuck devices in the optical fiber is L
- the moving amount of the chuck is Z
- the outer diameter of the primary resin layer is Dp
- the outer diameter of the glass fiber is Df
- the Poisson's ratio of the primary resin layer is n.
- the secondary resin layer 15 can be formed by curing, for example, a resin composition containing a photopolymerizable compound containing urethane (meth) acrylate, a photopolymerization initiator, and the like.
- the photopolymerizable compound and the photopolymerization initiator are not particularly limited, and can be appropriately selected and used from the above-mentioned photopolymerizable compounds and photopolymerization initiators.
- the resin composition forming the secondary resin layer can be prepared by using a conventionally known technique. However, the resin composition forming the secondary resin layer has a different composition from the resin composition forming the primary resin layer.
- the method for manufacturing an optical fiber according to the present embodiment includes a coating step of applying the resin composition according to the present embodiment to the outer periphery of a glass fiber including a core and a clad, and a resin composition by irradiating ultraviolet rays after the coating step. It includes a curing step of curing an object.
- a coating step of applying the resin composition according to the present embodiment to the outer periphery of a glass fiber including a core and a clad and a resin composition by irradiating ultraviolet rays after the coating step. It includes a curing step of curing an object.
- the resin composition according to the present embodiment as the resin composition for primary coating, it is possible to manufacture an optical fiber having excellent lateral pressure characteristics and void resistance characteristics. ..
- polyrotaxane having ultraviolet curability As polyrotaxane having ultraviolet curability, the trade name "SA1305P-20” (Mw: 200,000; linear polymer Mw: 11000; acryloyl group equivalent: 3500 g / eq) and "SA2405P-" of Advanced Soft Materials Co., Ltd. 20 ”(Mw: 400,000; linear polymer Mw: 20000; acryloyl group equivalent: 4000 g / eq) was prepared.
- SA1305P-20 Mw: 200,000; linear polymer Mw: 11000; acryloyl group equivalent: 3500 g / eq
- SA2405P- of Advanced Soft Materials Co., Ltd. 20
- These polyrotaxanes are polyrotaxanes comprising a cyclic molecule having an acryloyl group and a linear polymer having an adamantyl group.
- Nonylphenol EO-modified acrylate manufactured by Toa Synthetic Co., Ltd., trade name: Aronix M-113
- N-vinylcaprolactam and 1,6-hexanediol diacrylate were prepared as monomers.
- silane coupling agent 3-Mercaptopropyltrimethoxysilane was prepared as a silane coupling agent.
- a silica sol obtained by dispersing hydrophobic silica particles having a non-reactive propyl group on the surface and having an average primary particle size of 40 nm or more and 60 nm or less in methanol was prepared.
- the numerical value of polyrotaxane is the content (% by mass) based on the total amount of the photopolymerizable compound
- the numerical value of each component of the photopolymerizable compound and 3-mercaptopropyltrimethoxysilane is The content (% by mass) based on the total amount of each component of the photopolymerizable compound and 3-mercaptopropyltrimethoxysilane
- the numerical value of the silica particles is the content based on the total amount of the photopolymerizable compound and the silica particles.
- the amount (% by mass), and the numerical value of the photopolymerization initiator is the content (% by mass) based on the total amount of the photopolymerizable compounds.
- a resin composition for primary coating and a resin composition for secondary coating were applied to the outer periphery of a glass fiber having a diameter of 125 ⁇ m composed of a core and a clad, respectively.
- each resin composition was cured by irradiating with ultraviolet rays to form a coated resin layer provided with a primary resin layer and a secondary resin layer, and an optical fiber was produced.
- the thickness of the primary resin layer was 35 ⁇ m
- the thickness of the secondary resin layer was 25 ⁇ m.
- the line speed was 1500 m / min.
- the Young's modulus of the primary resin layer was measured by the Pullout Modulus (POM) method at 23 ° C.
Abstract
Description
本出願は、2020年12月7日出願の日本出願第2020-202628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。
光ファイバの被覆樹脂層は、一般にプライマリ樹脂層とセカンダリ樹脂層とを備えている。光ファイバの側圧特性を向上させる観点から、プライマリ樹脂層のヤング率を低減することが望ましい。しかしながら、プライマリ樹脂層の低ヤング率化は、プライマリ樹脂層の強度低下を引き起こすため、光ファイバをスクリーニングする際にプライマリ樹脂層内の架橋切断が生じ、光ファイバにおいて信頼性試験におけるロス増の原因となるボイドが発生し易くなる。
本開示によれば、光ファイバの側圧特性及び耐ボイド特性を向上させることができるプライマリ樹脂層を形成することができる樹脂組成物、並びに、側圧特性及び耐ボイド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光ファイバのプライマリ被覆用の樹脂組成物は、光重合性化合物と光重合開始剤とシランカップリング剤とを含有し、光重合性化合物が、ウレタン(メタ)アクリレートと紫外線硬化性を有するポリロタキサンとを含み、ポリロタキサンの含有量は、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、本開示はこれらの例示に限定されず、請求の範囲によって示され、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、光重合性化合物と光重合開始剤とシランカップリング剤とを含有し、必要に応じてその他の成分を更に含有してもよい。以下、各成分について詳述する。
光重合性化合物は、ウレタン(メタ)アクリレートと紫外線硬化性を有するポリロタキサンとを含む。
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(商品名: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(商品名:Omnirad 651、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(商品名:Omnirad TPO、IGM Resins社製)、エチル(2,4,6-トリメチルベンゾイル)-フェニルホスフィネート(商品名:Omnirad TPO-L、IGM Resins社製)、2-ベンジル-2-ジメチルアミノ-4’-モルホリノブチロフェノン(商品名:Omnirad 369、IGM Resins社製)、2-ジメチルアミノ-2-(4-メチル-ベンジル)-1-(4-モルホリン-4-イル-フェニル)-ブタン-1-オン(商品名:Omnirad 379、IGM Resins社製)、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(商品名:Omnirad 819、IGM Resins社製)及び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(商品名:Omnirad 907、IGM Resins社製)が挙げられる。光重合開始剤は、1種を単独で用いてもよく、2種以上を組み合わせて用いてもよい。
シランカップリング剤としては、例えば、テトラメチルシリケート、テトラエチルシリケート、メルカプトプロピルトリメトキシシラン、ビニルトリクロロシラン、ビニルトリエトキシシラン、ビニルトリス(β-メトキシ-エトキシ)シラン、β-(3,4-エポキシシクロヘキシル)-エチルトリメトキシシラン、ジメトキシジメチルシラン、ジエトキシジメチルシラン、3-アクリロキシプロピルトリメトキシシラン、γ-グリシドキシプロピルトリメトキシシラン、γ-グリシドキシプロピルメチルジエトキシシラン、γ-メタクリロキシプロピルトリメトキシシラン、N-(β-アミノエチル)-γ-アミノプロピルトリメトキシシラン、N-(β-アミノエチル)-γ-アミノプロピルトリメチルジメトキシシラン、N-フェニル-γ-アミノプロピルトリメトキシシラン、γ-クロロプロピルトリメトキシシラン、γ-メルカプトプロピルトリメトキシシラン、γ-アミノプロピルトリメトキシシラン、ビス-[3-(トリエトキシシリル)プロピル]テトラスルフィド、ビス-[3-(トリエトキシシリル)プロピル]ジスルフィド、γ-トリメトキシシリルプロピルジメチルチオカルバミルテトラスルフィド、及びγ-トリメトキシシリルプロピルベンゾチアジルテトラスルフィドが挙げられる。これらのシランカップリング剤は、1種を単独で用いてもよく、2種以上を組み合わせて用いてもよい。
本実施形態に係る樹脂組成物は、無機酸化物粒子、光酸発生剤、レベリング剤、消泡剤、酸化防止剤、紫外線吸収剤等を更に含有してもよい。
本実施形態に係る光ファイバは、コア及びクラッドを含むガラスファイバと、ガラスファイバに接して該ガラスファイバを被覆するプライマリ樹脂層と、プライマリ樹脂層を被覆するセカンダリ樹脂層と、を備えている。
ヤング率(MPa)=((1+n)W/πLZ)×ln(Dp/Df)
本実施形態に係る光ファイバの製造方法は、コア及びクラッドを含むガラスファイバの外周に、本実施形態に係る樹脂組成物を塗布する塗布工程と、塗布工程の後に紫外線を照射することにより樹脂組成物を硬化させる硬化工程と、を備える。本実施形態に係る光ファイバの製造方法は、プライマリ被覆用の樹脂組成物として本実施形態に係る樹脂組成物を使用することにより、側圧特性及び耐ボイド特性に優れる光ファイバを製造することができる。
(光重合性化合物)
ウレタン(メタ)アクリレートとして、数平均分子量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、2-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(UA)を準備した。得られたウレタンアクリレートの数平均分子量は、15000であった。
光重合開始剤として、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)を準備した。
シランカップリング剤として、3-メルカプトプロピルトリメトキシシランを準備した。
無機酸化物粒子として、表面に非反応性のプロピル基を有し、平均一次粒径が40nm以上60nm以下である疎水性シリカ粒子が、メタノールに分散されて得られるシリカゾルを準備した。
下記表1及び表2に示す配合量で各成分を混合して、各試験例のプライマリ被覆用の樹脂組成物を得た。試験例1~8は実施例に相当し、試験例9~11は比較例に相当する。
数平均分子量600のポリプロピレングリコール、2,4-トリレンジイソシアネート及び2-ヒドロキシエチルアクリレートを反応させて得られたウレタンアクリレート(Mn:1300)を35質量部、エポキシアクリレートを30質量部、イソボルニルアクリレート(大阪有機化学工業株式会社、商品名「IBXA」)を15質量部、フェノキシエチルアクリレート(共栄社化学株式会社、商品名「ライトアクリレートPO-A」)18質量部、1-ヒドロキシシクロヘキシルフェニルケトンを1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を1質量部混合して、セカンダリ被覆用の樹脂組成物を得た。
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、プライマリ被覆用の樹脂組成物とセカンダリ被覆用の樹脂組成物とをそれぞれ塗布した。次いで、紫外線を照射することでそれぞれの樹脂組成物を硬化させ、プライマリ樹脂層及びセカンダリ樹脂層を備える被覆樹脂層を形成し、光ファイバを作製した。プライマリ樹脂層の厚さを35μm、セカンダリ樹脂層の厚さを25μmとした。線速は1500m/分とした。
プライマリ樹脂層のヤング率は、23℃でのPullout Modulus(POM)法により測定した。
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「A」、伝送損失差が0.6dB/km超の場合を「B」と評価した。
10mの光ファイバを85℃で湿度85%の条件下で120日間保管した後、-40℃に16時間置いて、直径10μm以上のボイドの有無を顕微鏡で観察した。光ファイバ1m当たりのボイドの数が1個未満の場合を「A」、ボイドの数が1~2個の場合を「B」、ボイドの数が2個を超える場合を「C」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
D1 コア11の直径
D2 ガラスファイバ13の外径
Claims (6)
- 光重合性化合物と光重合開始剤とシランカップリング剤とを含有し、
前記光重合性化合物が、ウレタン(メタ)アクリレートと紫外線硬化性を有するポリロタキサンとを含み、
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、光ファイバのプライマリ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又は請求項2に記載の樹脂組成物。
- 無機酸化物粒子を更に含有する、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。
- 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、
前記プライマリ樹脂層が、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を含む、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、を備える、光ファイバの製造方法。
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