CN113039225A - 树脂组合物以及光纤 - Google Patents
树脂组合物以及光纤 Download PDFInfo
- Publication number
- CN113039225A CN113039225A CN201980069815.6A CN201980069815A CN113039225A CN 113039225 A CN113039225 A CN 113039225A CN 201980069815 A CN201980069815 A CN 201980069815A CN 113039225 A CN113039225 A CN 113039225A
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- Prior art keywords
- meth
- acrylate
- resin composition
- resin layer
- inorganic oxide
- Prior art date
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- 239000011342 resin composition Substances 0.000 title claims abstract description 69
- 239000013307 optical fiber Substances 0.000 title claims description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 109
- 229920005989 resin Polymers 0.000 claims abstract description 93
- 239000011347 resin Substances 0.000 claims abstract description 92
- 239000002245 particle Substances 0.000 claims abstract description 52
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 46
- 239000000178 monomer Substances 0.000 claims abstract description 37
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000004048 modification Effects 0.000 claims abstract description 14
- 238000012986 modification Methods 0.000 claims abstract description 14
- 125000000524 functional group Chemical group 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 13
- -1 methacryloyl group Chemical group 0.000 claims description 42
- 239000003365 glass fiber Substances 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 239000011164 primary particle Substances 0.000 claims description 10
- 238000005253 cladding Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 25
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 15
- 239000002612 dispersion medium Substances 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 6
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 6
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 6
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-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 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000011800 void material Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 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
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 229920005862 polyol Polymers 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- JWYVGKFDLWWQJX-UHFFFAOYSA-N 1-ethenylazepan-2-one Chemical compound C=CN1CCCCCC1=O JWYVGKFDLWWQJX-UHFFFAOYSA-N 0.000 description 3
- 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
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229960002317 succinimide Drugs 0.000 description 3
- PGMMMHFNKZSYEP-UHFFFAOYSA-N 1,20-Eicosanediol Chemical compound OCCCCCCCCCCCCCCCCCCCCO PGMMMHFNKZSYEP-UHFFFAOYSA-N 0.000 description 2
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 2
- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-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
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 description 2
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 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
- 230000005540 biological transmission Effects 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- GHLKSLMMWAKNBM-UHFFFAOYSA-N dodecane-1,12-diol Chemical compound OCCCCCCCCCCCCO GHLKSLMMWAKNBM-UHFFFAOYSA-N 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 2
- GJBXIPOYHVMPQJ-UHFFFAOYSA-N hexadecane-1,16-diol Chemical compound OCCCCCCCCCCCCCCCCO GJBXIPOYHVMPQJ-UHFFFAOYSA-N 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 2
- 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
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 125000005641 methacryl group Chemical group 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 description 2
- AQIXEPGDORPWBJ-UHFFFAOYSA-N pentan-3-ol Chemical compound CCC(O)CC AQIXEPGDORPWBJ-UHFFFAOYSA-N 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000005056 polyisocyanate Substances 0.000 description 2
- 229920001228 polyisocyanate Polymers 0.000 description 2
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 2
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
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- 230000002194 synthesizing effect Effects 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 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 1
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- HHQAGBQXOWLTLL-UHFFFAOYSA-N (2-hydroxy-3-phenoxypropyl) prop-2-enoate Chemical compound C=CC(=O)OCC(O)COC1=CC=CC=C1 HHQAGBQXOWLTLL-UHFFFAOYSA-N 0.000 description 1
- BXSPZNVFEYWSLZ-UHFFFAOYSA-N (3-phenoxyphenyl)methyl prop-2-enoate Chemical compound C=CC(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 BXSPZNVFEYWSLZ-UHFFFAOYSA-N 0.000 description 1
- LTQBNYCMVZQRSD-UHFFFAOYSA-N (4-ethenylphenyl)-trimethoxysilane Chemical compound CO[Si](OC)(OC)C1=CC=C(C=C)C=C1 LTQBNYCMVZQRSD-UHFFFAOYSA-N 0.000 description 1
- ZBBLRPRYYSJUCZ-GRHBHMESSA-L (z)-but-2-enedioate;dibutyltin(2+) Chemical compound [O-]C(=O)\C=C/C([O-])=O.CCCC[Sn+2]CCCC ZBBLRPRYYSJUCZ-GRHBHMESSA-L 0.000 description 1
- ALVZNPYWJMLXKV-UHFFFAOYSA-N 1,9-Nonanediol Chemical compound OCCCCCCCCCO ALVZNPYWJMLXKV-UHFFFAOYSA-N 0.000 description 1
- BQTPKSBXMONSJI-UHFFFAOYSA-N 1-cyclohexylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1CCCCC1 BQTPKSBXMONSJI-UHFFFAOYSA-N 0.000 description 1
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 description 1
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 description 1
- 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
- CZZVAVMGKRNEAT-UHFFFAOYSA-N 2,2-dimethylpropane-1,3-diol;3-hydroxy-2,2-dimethylpropanoic acid Chemical compound OCC(C)(C)CO.OCC(C)(C)C(O)=O CZZVAVMGKRNEAT-UHFFFAOYSA-N 0.000 description 1
- IVIDDMGBRCPGLJ-UHFFFAOYSA-N 2,3-bis(oxiran-2-ylmethoxy)propan-1-ol Chemical compound C1OC1COC(CO)COCC1CO1 IVIDDMGBRCPGLJ-UHFFFAOYSA-N 0.000 description 1
- HDPLHDGYGLENEI-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COC(C)COCC1CO1 HDPLHDGYGLENEI-UHFFFAOYSA-N 0.000 description 1
- FVCHRIQAIOHAIC-UHFFFAOYSA-N 2-[1-[1-[1-(oxiran-2-ylmethoxy)propan-2-yloxy]propan-2-yloxy]propan-2-yloxymethyl]oxirane Chemical compound C1OC1COC(C)COC(C)COC(C)COCC1CO1 FVCHRIQAIOHAIC-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
- PRIUALOJYOZZOJ-UHFFFAOYSA-L 2-ethylhexyl 2-[dibutyl-[2-(2-ethylhexoxy)-2-oxoethyl]sulfanylstannyl]sulfanylacetate Chemical compound CCCCC(CC)COC(=O)CS[Sn](CCCC)(CCCC)SCC(=O)OCC(CC)CCCC PRIUALOJYOZZOJ-UHFFFAOYSA-L 0.000 description 1
- HHKAGFTWEFVXET-UHFFFAOYSA-N 2-heptyl-2-(hydroxymethyl)propane-1,3-diol Chemical compound CCCCCCCC(CO)(CO)CO HHKAGFTWEFVXET-UHFFFAOYSA-N 0.000 description 1
- QPXVRLXJHPTCPW-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-(4-propan-2-ylphenyl)propan-1-one Chemical compound CC(C)C1=CC=C(C(=O)C(C)(C)O)C=C1 QPXVRLXJHPTCPW-UHFFFAOYSA-N 0.000 description 1
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- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
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- VNPRJHMMOKDEDZ-UHFFFAOYSA-L 6-methylheptyl 2-[dibutyl-[2-(6-methylheptoxy)-2-oxoethyl]sulfanylstannyl]sulfanylacetate Chemical compound CC(C)CCCCCOC(=O)CS[Sn](CCCC)(CCCC)SCC(=O)OCCCCCC(C)C VNPRJHMMOKDEDZ-UHFFFAOYSA-L 0.000 description 1
- GAYWTJPBIQKDRC-UHFFFAOYSA-N 8-trimethoxysilyloctyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCCCCCCOC(=O)C(C)=C GAYWTJPBIQKDRC-UHFFFAOYSA-N 0.000 description 1
- JOVCTEPPTIOAPX-UHFFFAOYSA-N 8-trimethoxysilyloctyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCCCCCCOC(=O)C=C JOVCTEPPTIOAPX-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种树脂组合物,包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的基础树脂;以及具有紫外线固化性官能团的表面修饰无机氧化物粒子,表面修饰无机氧化物粒子中的表面修饰量为0.2mg/m2以上。
Description
技术领域
本发明涉及树脂组合物以及光纤。
本专利申请要求基于2018年11月16日提出的日本专利申请第2018-215711号的优先权,并且援引了所述日本专利申请所记载的全部记载内容。
背景技术
通常,光纤具有用于保护作为光传输体的玻璃纤维的被覆树脂层。为了减小对光纤施加侧压时发生的微小弯曲所引起的传输损耗的增加,要求光纤具有优异的侧压特性。
例如,被覆树脂层具备初级树脂层和次级树脂层。初级树脂层要求杨氏模量低、柔软性优异(例如,参照专利文献1)。另外,研究了通过使用含有以合成石英为原料的填料的紫外线固化型树脂组合物来形成树脂层,从而改善光纤的侧压特性(例如,参照专利文献2)。
现有技术文献
专利文献
专利文献1:日本特开2013-197163号公报
专利文献2:日本特开2014-219550号公报
发明内容
本发明的一个方式涉及的树脂组合物包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的基础树脂;以及具有紫外线固化性官能团的表面修饰无机氧化物粒子,表面修饰无机氧化物粒子中的表面修饰量为0.2mg/m2以上。
附图说明
[图1]图1是表示本实施方式涉及的光纤的一个例子的示意性剖面图。
具体实施方式
[本发明要解决的课题]
从提高光纤的耐孔隙特性的观点来看,据认为,通过使用含有填料的树脂组合物来形成初级树脂层,从而提高初级树脂层的强度。然而,用于初级树脂层的树脂组合物通常含有硅烷偶联剂,因此当添加填料时,树脂组合物粘度容易增加,从而适用期倾向于变短。
本发明的目的在于提供适用期长的树脂组合物,以及具备由该树脂组合物形成的初级树脂层的光纤。
[本发明的效果]
根据本发明,可以提供适用期长的光纤被覆用的树脂组合物,以及具备由该树脂组合物形成的初级树脂层的光纤。
[本发明实施方式的说明]
首先,列举本发明的实施方式的内容并进行说明。本发明的一个方式涉及的树脂组合物包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的基础树脂;以及具有紫外线固化性官能团的表面修饰无机氧化物粒子,表面修饰无机氧化物粒子中的表面修饰量为0.2mg/m2以上。
在制备树脂组合物的过程中,当将含有硅烷偶联剂的基础树脂与含有未修饰的无机氧化物粒子的溶胶混合时,硅烷偶联剂发生水解,并且在硅烷偶联剂之间以及与存在于无机氧化物粒子的表面上的羟基发生缩合反应,有时会损害树脂组合物的稳定性。与此相对,本发明人认为,本实施方式的树脂组合物通过使用特定的表面修饰无机氧化物粒子,可以抑制水解和缩合反应,从而能够延长树脂组合物的适用期。
从调节由所述树脂组合物形成的树脂层的杨氏模量的观点来看,表面修饰无机氧化物粒子中的表面修饰量可以为0.2mg/m2以上2.8mg/m2以下。
所述官能团可以是选自由丙烯酰基、甲基丙烯酰基以及乙烯基构成的组中的至少1种基团。由此,容易形成具有充分强度的树脂层。
从在树脂组合物中的分散性优异、进一步提高适用期的观点来看,无机氧化物粒子的平均一次粒径可以为650nm以下。
本发明的一个方式涉及的光纤的初级被覆材料包含所述树脂组合物。通过将本实施方式涉及的树脂组合物用于初级树脂层,可以制作出耐孔隙特性优异的光纤。
本发明的一个方式涉及的光纤具备:含有芯部和包层的玻璃纤维、与玻璃纤维接触并被覆该玻璃纤维的初级树脂层、以及被覆初级树脂层的次级树脂层,其中初级树脂层由所述树脂组合物的固化产物构成。通过将本实施方式涉及的树脂组合物应用于初级树脂层,能够提高光纤的耐孔隙特性。
[本发明实施方式的详细说明]
根据需要参照附图对本发明实施方式涉及的树脂组合物以及光纤的具体例子进行说明。需要说明的是,本发明不限于这些示例,而是由权利要求书所表示,并且意图包括与权利要求书等同的意义和范围内的所有变化。在下述说明中,在附图的说明中相同的要素标注相同的符号,并且省略重复的说明。
<树脂组合物>
本实施方式涉及的树脂组合物包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的基础树脂;以及具有紫外线固化性官能团的表面修饰无机氧化物粒子。
这里,所谓(甲基)丙烯酸酯,指的是丙烯酸酯或与其相对应的甲基丙烯酸酯。这也同样地适用于(甲基)丙烯酸。
(表面修饰无机氧化物粒子)
本实施方式涉及的表面修饰无机氧化物粒子是通过具有紫外线固化性官能团的硅烷化合物对无机氧化物粒子的表面进行处理,从而在无机氧化物粒子的表面导入紫外线固化性官能团。即,表面修饰无机氧化物粒子由无机成分和有机成分构成。官能团可以为丙烯酰基、甲基丙烯酰基或乙烯基。通过具有这样的官能团,容易形成耐孔隙特性高的树脂层。
作为具有紫外线固化性官能团的硅烷化合物,例如可以列举出:3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷、8-甲基丙烯酰氧基辛基三甲氧基硅烷、8-丙烯酰氧基辛基三甲氧基硅烷、7-辛烯基三甲氧基硅烷、对苯乙烯基三甲氧基硅烷、乙烯基三甲氧基硅烷以及乙烯基三乙氧基硅烷。
本实施方式涉及的表面修饰无机氧化物粒子分散在分散介质中。通过使用分散在分散介质中的表面修饰无机氧化物粒子,可以使表面修饰无机氧化物粒子均匀地分散在树脂组合物中,从而能够提高树脂组合物的保存稳定性。作为分散介质,只要其不妨碍树脂组合物的固化,则没有特别地限定。分散介质可以为反应性的,也可以为非反应性的。
作为反应性的分散介质,可以使用(甲基)丙烯酰基化合物、环氧化合物等单体。作为(甲基)丙烯酰基化合物,例如可以列举出:1,6-己二醇二(甲基)丙烯酸酯、EO改性双酚A二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、PO改性双酚A二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、聚四亚甲基二醇二(甲基)丙烯酸酯、2-羟基-3-苯氧基丙基(甲基)丙烯酸酯、丙二醇二缩水甘油醚的(甲基)丙烯酸加成物、三丙二醇二缩水甘油醚的(甲基)丙烯酸加成物、以及丙三醇二缩水甘油醚的(甲基)丙烯酸加成物。作为(甲基)丙烯酰基化合物,也可以使用后述单体中示例的化合物。
作为非反应性的分散介质,可以使用甲基乙基酮(MEK)等酮类溶剂;甲醇(MeOH)、丙二醇单甲醚(PGME)等醇类溶剂;或者丙二醇单甲醚醋酸酯(PGMEA)等酯类溶剂。在使用非反应性的分散介质的情况下,在将基础树脂和分散在分散介质中的表面修饰无机氧化物粒子混合后,可以除去分散介质的一部分,从而制备树脂组合物。利用X射线小角散射法测定含有表面修饰无机氧化物粒子的分散介质,在没有测定到聚集的粒子的情况下,可以认为表面修饰无机氧化物粒子以一次粒子的形式分散。
从在树脂组合物中的分散性优异、并且容易形成强韧的树脂层的方面考虑,上述表面修饰无机氧化物粒子优选为使选自由二氧化硅(氧化硅)、二氧化锆(氧化锆)、氧化铝(alumina)、氧化镁(magnesia)、氧化钛(titania)、氧化锡以及氧化锌构成的组中的至少1种经过表面处理后的粒子。从价格低廉、容易进行表面处理、具有紫外线透过性、容易对树脂层赋予适度的硬度等观点来看,更优选使用表面修饰氧化硅粒子作为本实施方式涉及的表面修饰无机氧化物粒子。
从降低初级树脂层的杨氏模量的观点来看,表面修饰无机氧化物粒子的平均一次粒径可以为650nm以下、优选为600nm以下、更优选为500nm以下、进一步优选为400nm以下。从对初级树脂层赋予强度的观点来看,表面修饰无机氧化物粒子的平均一次粒径优选为5nm以上、更优选为10nm以上。平均一次粒径例如可以利用电子显微镜照片的图像分析、光散射法、BET法等来进行测定。在一次粒子的粒径较小的情况下,分散有无机氧化物粒子的一次粒子的分散介质在目视下看起来是透明的。在一次粒子的粒径比较大(40nm以上)的情况下,分散有一次粒子的分散介质看起来是白浊的,但没有观察到沉淀物。
以树脂组合物的总量(基础树脂和表面修饰无机氧化物粒子的总量)为基准,表面修饰无机氧化物粒子的含量优选为1质量%以上45质量%以下、更优选为2质量%以上40质量%以下、进一步优选为3质量%以上35质量%以下、特别优选为5质量%以上30质量%以下。当表面修饰无机氧化物粒子的含量为1质量%以上时,容易形成强韧的树脂层。当表面修饰无机氧化物粒子的含量为45质量%以下时,可以形成杨氏模量低的树脂层。需要说明的是,也可以认为树脂组合物的总量与树脂组合物的固化产物的总量相同。以初级树脂层的总量(构成初级树脂层的树脂组合物的固化产物的总量)为基准,表面修饰无机氧化物粒子的含量优选为1质量%以上45质量%以下、更优选为2质量%以上40质量%以下、进一步优选为3质量%以上35质量%以下、特别优选为5质量%以上30质量%以下。
表面修饰无机氧化物粒子中的表面修饰量为0.2mg/m2以上、优选为0.2mg/m2以上2.8mg/m2以下、更优选为0.3mg/m2以上2.6mg/m2以下、进一步优选为0.4mg/m2以上2.4mg/m2以下、特别优选为0.6mg/m2以上2.2mg/m2以下。通过使表面修饰量在上述范围内,容易调节树脂组合物的粘度。
本说明书中的“表面修饰量”可以根据表面修饰无机氧化物粒子的比表面积和有机成分的比例来算出。上述有机成分是源自导入到表面修饰前的无机氧化物粒子中的紫外线固化性官能团的成分。例如,在表面修饰无机氧化物粒子由氧化硅粒子构成的情况下,除SiO2以外的成分成为有机成分。可以利用氮吸附BET法测定比表面积,并且利用差热/热重分析法(TG/DTA)来测定有机成分的比例。表面修饰无机氧化物粒子中的表面修饰量可以在制备树脂组合物之前将粒子从分散介质中分离出来进行测定,也可以在制备树脂组合物之后将粒子从树脂组合物中分离出来进行测定。
(基础树脂)
本实施方式涉及的基础树脂含有:氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂。
作为氨基甲酸酯(甲基)丙烯酸酯低聚物,可以使用由多元醇化合物、多异氰酸酯化合物以及含羟基的(甲基)丙烯酸酯化合物进行反应而得到的低聚物。
作为多元醇化合物,例如可以列举出:聚四亚甲基二醇、聚丙二醇以及双酚A-环氧乙烷加成二醇。多元醇化合物的数均分子量(Mn)优选为1000以上10000以下、更优选为1500以上8000以下、进一步优选为2000以上6000以下。作为多异氰酸酯化合物,例如可以列举出:2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、异佛尔酮二异氰酸酯以及二环己基甲烷4,4’-二异氰酸酯。作为含羟基的(甲基)丙烯酸酯化合物,例如可以列举出:(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丁酯、1,6-己二醇单(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、(甲基)丙烯酸2-羟丙酯以及三丙二醇单(甲基)丙烯酸酯。
作为合成氨基甲酸酯(甲基)丙烯酸酯低聚物时的催化剂,通常使用有机锡化合物。作为有机锡化合物,例如可以列举出:二月桂酸二丁基锡、二乙酸二丁基锡、马来酸二丁基锡、双(巯基乙酸2-乙基己酯)二丁基锡、双(巯基乙酸异辛酯)二丁基锡以及氧化二丁基锡。从易得性或催化性能方面来看,优选使用二月桂酸二丁基锡或二乙酸二丁基锡作为催化剂。
在合成氨基甲酸酯(甲基)丙烯酸酯低聚物时也可以使用碳原子数为5以下的低级醇。作为低级醇,例如可以列举出:甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-2-丙醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-1-丁醇、3-甲基-1-丁醇、2-甲基-2-丁醇、3-甲基-2-丁醇以及2,2-二甲基-1-丙醇。
也可以在氨基甲酸酯(甲基)丙烯酸酯低聚物的末端加成硅烷偶联剂(例如,3-巯基丙基三甲氧基硅烷)。硅烷偶联剂的加成可以在合成氨基甲酸酯(甲基)丙烯酸酯低聚物时进行或者在制备基础树脂时进行。
本实施方式涉及的基础树脂也可以进一步含有环氧(甲基)丙烯酸酯低聚物作为低聚物。作为环氧(甲基)丙烯酸酯低聚物,可以使用将具有(甲基)丙烯酰基的化合物与具有2个以上缩水甘油基的环氧树脂进行反应而得到的低聚物。
作为单体,可以使用具有1个可聚合基团的单官能单体、具有2个以上可聚合基团的多官能单体。单体也可以2种以上混合使用。
从容易形成强韧的树脂层的方面来看,可以使用具有苯氧基的单体作为单体。
作为具有苯氧基的单体,可以使用具有苯氧基的(甲基)丙烯酸酯化合物。作为具有苯氧基的(甲基)丙烯酸酯化合物,例如可以列举出:苯酚EO改性(甲基)丙烯酸酯、壬基酚EO改性(甲基)丙烯酸酯、苯酚PO改性(甲基)丙烯酸酯、壬基酚PO改性(甲基)丙烯酸酯、苯氧基乙基(甲基)丙烯酸酯、2-羟基-3-苯氧基丙基(甲基)丙烯酸酯、以及3-苯氧基苄基(甲基)丙烯酸酯。这里,EO改性是指具有由(C2H4O)n所表示的环氧乙烷基,PO改性是指具有由(C3H6O)n所表示的环氧丙烷基。n为1以上的整数。
从调节固化产物的杨氏模量的观点来看,具有苯氧基的单体可以是选自由苯酚EO改性丙烯酸酯、壬基酚EO改性丙烯酸酯、苯氧基乙基丙烯酸酯、2-羟基-3-苯氧基丙基丙烯酸酯、以及3-苯氧基苄基丙烯酸酯构成的组中的至少1种。具有苯氧基的单体也可以2种以上混合使用。
以基础树脂的总量为基准,具有苯氧基的单体的含量优选为1质量%以上60质量%以下、更优选为5质量%以上50质量%以下、进一步优选为10质量%以上40质量%以下。通过使树脂组合物在这样的范围内含有具有苯氧基的单体,可以形成作为光纤的初级被覆材料的具有适当的杨氏模量的树脂层。
作为单体,也可以使用不具有苯氧基的单体。不具有苯氧基的单体可以是单官能单体,也可以是具有2个以上可聚合基团的多官能单体。
作为不具有苯氧基的单官能单体,例如可以列举出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸仲丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸4-叔丁基环己醇酯、(甲基)丙烯酸四氢糠酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸二环戊烯酯、(甲基)丙烯酸二环戊烯氧基乙酯、(甲基)丙烯酸二环戊酯、(甲基)丙烯酸壬基酚聚乙二醇酯、(甲基)丙烯酸异冰片酯等(甲基)丙烯酸酯类单体;(甲基)丙烯酸、(甲基)丙烯酸二聚物、(甲基)丙烯酸羧基乙酯、(甲基)丙烯酸羧基戊酯、(甲基)丙烯酸ω-羧基-聚己内酯等含羧基的单体;N-丙烯酰基吗啉、N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、N-丙烯酰基哌啶、N-甲基丙烯酰基哌啶、N-丙烯酰基吡咯烷、3-(3-吡啶基)丙基(甲基)丙烯酸酯、环三羟甲基丙烷甲缩醛丙烯酸酯等含杂环的(甲基)丙烯酸酯;马来酰亚胺、N-环己基马来酰亚胺、N-苯基马来酰亚胺等马来酰亚胺系单体;(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺、N-己基(甲基)丙烯酰胺、N-甲基(甲基)丙烯酰胺、N-丁基(甲基)丙烯酰胺、N-丁基(甲基)丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-羟甲基丙烷(甲基)丙烯酰胺等N-取代酰胺系单体;(甲基)丙烯酸氨基乙酯、(甲基)丙烯酸氨基丙酯、(甲基)丙烯酸N,N-二甲基氨基乙酯、(甲基)丙烯酸叔丁基氨基乙酯等(甲基)丙烯酸氨基烷基酯系单体;N-(甲基)丙烯酰氧基亚甲基琥珀酰亚胺、N-(甲基)丙烯酰基-6-氧基六亚甲基琥珀酰亚胺、N-(甲基)丙烯酰基-8-氧基八亚甲基琥珀酰亚胺等琥珀酰亚胺系单体。
作为不具有苯氧基的多官能单体,例如可以列举出:乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、双酚A的环氧烷加成物的二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、羟基新戊酸新戊二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、1,12-十二烷二醇二(甲基)丙烯酸酯、1,14-十四烷二醇二(甲基)丙烯酸酯、1,16-十六烷二醇二(甲基)丙烯酸酯、1,20-二十烷二醇二(甲基)丙烯酸酯、异戊二醇二(甲基)丙烯酸酯、3-乙基-1,8-辛二醇二(甲基)丙烯酸酯、双酚A的EO加成物二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、三羟甲基辛烷三(甲基)丙烯酸酯、三羟甲基丙烷聚乙氧基三(甲基)丙烯酸酯、三羟甲基丙烷聚丙氧基三(甲基)丙烯酸酯、三羟甲基丙烷聚乙氧基聚丙氧基三(甲基)丙烯酸酯、三[(甲基)丙烯酰氧基乙基]异氰脲酸酯、季戊四醇三(甲基)丙烯酸酯、季戊四醇聚乙氧基四(甲基)丙烯酸酯、季戊四醇聚丙氧基四(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二三羟甲基丙烷四(甲基)丙烯酸酯、二季戊四醇四(甲基)丙烯酸酯、二季戊四醇五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯以及己内酯改性三[(甲基)丙烯酰氧基乙基]异氰脲酸酯。
作为光聚合引发剂,可以从公知的自由基光聚合引发剂当中适当地选择并使用。作为光聚合引发剂,例如可以列举出:1-羟基环己基苯基酮(Omnirad 184,IGM Resins公司制)、2,2-二甲氧基-2-苯基苯乙酮、1-(4-异丙基苯基)-2-羟基-2-甲基丙烷-1-酮、双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦、2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基-丙烷-1-酮(Omnirad 907,IGM Resins公司制)、2,4,6-三甲基苯甲酰基二苯基氧化膦(Omnirad TPO,IGM Resins公司制)以及双(2,4,6-三甲基苯甲酰基)苯基氧化膦(Omnirad819,IGM Resins公司制)。
作为硅烷偶联剂,只要其不妨碍树脂组合物的固化,则没有特别地限定。作为硅烷偶联剂,例如可以列举出:硅酸四甲酯、硅酸四乙酯、巯基丙基三甲氧基硅烷、乙烯基三氯硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基-乙氧基)硅烷、β-(3,4-环氧环己基)-乙基三甲氧基硅烷、二甲氧基二甲基硅烷、二乙氧基二甲基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基甲基二乙氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲基二甲氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷、γ-氯丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷、γ-氨基丙基三甲氧基硅烷、双-[3-(三乙氧基甲硅烷基)丙基]四硫化物、双-[3-(三乙氧基甲硅烷基)丙基]二硫化物、γ-三甲氧基甲硅烷基丙基二甲基硫代氨甲酰基四硫化物以及γ-三甲氧基甲硅烷基丙基苯并噻唑基四硫化物。另外,也可以将在氨基甲酸酯(甲基)丙烯酸酯低聚物或(甲基)丙烯酸单体的末端加成硅烷偶联剂而成的化合物用作硅烷偶联剂。
树脂组合物也可以进一步含有流平剂、消泡剂、抗氧化剂等。
从抑制在光纤中产生孔隙的方面考虑,上述树脂组合物的固化产物的杨氏模量在23℃±2℃下优选为4MPa以下、更优选为0.05MPa以上4.0MPa以下、进一步优选为0.1MPa以上3.5MPa以下、特别优选为0.3MPa以上3.0MPa以下。
本实施方式涉及的树脂组合物可以适用于光纤的初级被覆材料。通过将本实施方式涉及的树脂组合物用于初级树脂层,可以制作出耐孔隙特性和侧压特性优异的光纤。
<光纤>
图1是表示本实施方式涉及的光纤的一个例子的示意性剖面图。光纤10具备:含有芯部11和包层12的玻璃纤维13,以及设置在玻璃纤维13的外周且含有初级树脂层14和次级树脂层15的被覆树脂层16。
包层12包围着芯部11。芯部11和包层12主要包含石英玻璃等玻璃,例如,芯部11可以使用添加有锗的石英玻璃,包层12可以使用纯石英玻璃或添加有氟的石英玻璃。
在图1中,例如,玻璃纤维13的外径(D2)为125μm左右,构成玻璃纤维13的芯部11的直径(D1)为7~15μm左右。
被覆树脂层16的厚度通常为60~70μm左右。初级树脂层14和次级树脂层15的各层的厚度可以为10~50μm左右,例如,初级树脂层14的厚度可以为35μm,次级树脂层15的厚度可以为25μm。光纤10的外径可以为245~265μm左右。
另外,被覆树脂层16的厚度也可以为27~48μm左右。初级树脂层14和次级树脂层15的各层的厚度可以为10~38μm左右,例如,初级树脂层14的厚度可以为25μm,次级树脂层15的厚度可以为10μm。光纤10的外径可以为179~221μm左右。
进一步,玻璃纤维13的外径(D2)可以为100μm左右,被覆树脂层16的厚度可以为22~37μm左右。初级树脂层14和次级树脂层15的各层的厚度可以为5~32μm左右,例如,初级树脂层14的厚度可以为25μm,次级树脂层15的厚度可以为10μm。光纤10的外径可以为144~174μm左右。
次级树脂层的杨氏模量在23℃下优选为1300MPa以上、更优选为1300MPa以上2600MPa以下、进一步优选为1300MPa以上2500MPa以下。当次级树脂层的杨氏模量为1300MPa以上时,容易提高侧压特性,当其为2600MPa以下时,能够对次级树脂层赋予适度的韧性,因而在次级树脂层中难以产生裂纹等。
次级树脂层例如可以是通过使包含氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂的树脂组合物固化而形成的。次级树脂层用的树脂组合物可以使用现有公知的技术。作为氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂,可以适当地选自上述基础树脂中所示例的化合物。另外,次级树脂层用的树脂组合物也可以含有疏水性的无机氧化物粒子。疏水性的无机氧化物粒子也可以为上述表面修饰无机氧化物粒子。但是,形成次级树脂层的树脂组合物与形成初级树脂层的树脂组合物具有不同的组成。从提高次级树脂层的杨氏模量的观点来看,合成氨基甲酸酯(甲基)丙烯酸酯低聚物时所使用的多元醇化合物的Mn可以为400以上2000以下。
实施例
以下,示出了使用本发明涉及的实施例和比较例的评价试验结果并对本发明进行更详细的说明。需要说明的是,本发明不限于这些实施例。
[树脂组合物的制作]
(低聚物)
准备了使Mn为4000的聚丙二醇、异佛尔酮二异氰酸酯、丙烯酸羟乙酯以及甲醇发生反应而得到的氨基甲酸酯丙烯酸酯低聚物作为低聚物。
(单体)
准备了壬基酚EO改性丙烯酸酯(“東亞合成株式会社”的商品名“アロニックスM-113”、n≒4)、N-乙烯基己内酰胺以及1,6-己二醇二丙烯酸酯作为单体。
(光聚合引发剂)
准备了2,4,6-三甲基苯甲酰基二苯基氧化膦作为光聚合引发剂。
(硅烷偶联剂)
准备了3-巯基丙基三甲氧基硅烷作为硅烷偶联剂。
(基础树脂)
将60质量份的氨基甲酸酯丙烯酸酯低聚物、22.8质量份的壬基酚EO改性丙烯酸酯、4.8质量份的N-乙烯基己内酰胺、1.6质量份的1,6-己二醇二丙烯酸酯、2.7质量份的2,4,6-三甲基苯甲酰基二苯基氧化膦、以及0.8质量份的3-巯基丙基三甲氧基硅烷混合,从而制备了基础树脂。
(表面修饰无机氧化物粒子)
准备了含有通过对3-甲基丙烯酰氧基丙基三甲氧基硅烷进行表面处理而得的氧化硅粒子(以下,简称“氧化硅粒子”)的氧化硅溶胶(MEK分散液)作为表面修饰无机氧化物粒子。
(未修饰的氧化硅粒子)
准备了含有未修饰的氧化硅粒子的氧化硅溶胶(MEK分散液)。
(实施例1~9、比较例1和2)
将基础树脂和氧化硅溶胶混合后,除去大部分的MEK,从而以使树脂组合物中的氧化硅粒子的含量成为10质量%的方式制备了树脂组合物。
使用通过实施例和比较例所得到的树脂组合物进行了以下评价。结果如表1所示。
(表面修饰量的测定)
在树脂组合物中加入氯仿后进行离心分离,回收沉淀物。在沉淀物中加入丙酮后进行离心分离,除去上清液后,在沉淀物中再次加入丙酮后进行离心分离并除去上清液,将上述的操作进行4次,从而提取出氧化硅粒子。将用研钵捣碎后的氧化硅粒子在室温下减压干燥12小时以除去挥发性成分。在30000rpm、120分钟的条件下进行离心分离。将干燥后的氧化硅粒子在80℃下减压处理12小时,使用细孔分布测定装置(“マイクロメリティクス”制造的“ASAP-2020”),利用氮吸附BET法测定了氧化硅粒子的比表面积(m2/g)。
使用差热热重量同时分析装置(“日立ハイテクサイエンス”公司制造的“TG/DTA6300”)测定了氧化硅粒子中所含的有机成分的比例(质量%)。测定如下:将测定了重量后的氧化硅粒子在氮气下(300mL/分钟)从室温加热至850℃,然后从850℃冷却至200℃,再在空气下(100mL/分钟)从200℃加热至1000℃,测定重量变化。由氧化硅粒子的重量变化算出有机成分的比例。
根据氧化硅粒子的比表面积和有机成分的比例,通过下式算出氧化硅粒子的表面修饰量。
表面修饰量(mg/m2)=有机成分的比例/比表面积
(杨氏模量)
利用旋涂机,将树脂组合物涂布在聚对苯二甲酸乙二醇酯(PET)膜上后,使用无电极UV灯系统(D阀)(“ヘレウス”制造),在1000±100mJ/cm2的条件下使其固化,从而在PET膜上形成厚度为200±20μm的树脂层。将树脂层从PET膜上剥离,从而得到了树脂膜。
将树脂膜冲切成JIS K 7127 Type5的哑铃状,并在23±2℃、50±10%RH的条件下,使用拉伸试验机以1mm/分钟的拉伸速度、标线间隔25mm的条件下拉伸,从而得到应力-应变曲线。由切线求得杨氏模量。
(适用期)
将树脂组合物放入容器内并在60℃下保管,研究树脂组合物因粘度增加而无法涂布的时间。
[表1]
可以确认,实施例的树脂组合物可以形成适用期长、且具有初级树脂层所需要的杨氏模量的树脂层。另一方面,比较例1的树脂组合物因初始粘度过高而无法进行评价。另外,在比较例2中,在制备树脂组合物时,因未修饰的氧化硅粒子聚集而无法进行评价。
符号说明
10…光纤、11…芯部、12…包层、13…玻璃纤维、14…初级树脂层、15…次级树脂层、16…被覆树脂层。
Claims (7)
1.一种光纤被覆用的树脂组合物,包括:
含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的基础树脂;以及具有紫外线固化性官能团的表面修饰无机氧化物粒子,其中,
所述表面修饰无机氧化物粒子中的表面修饰量为0.2mg/m2以上。
2.根据权利要求1所述的树脂组合物,其中,
所述表面修饰量为0.2mg/m2以上2.8mg/m2以下。
3.根据权利要求1或权利要求2所述的树脂组合物,其中,
所述官能团为选自由丙烯酰基、甲基丙烯酰基以及乙烯基构成的组中的至少1种基团。
4.根据权利要求1至权利要求3中任意一项所述的树脂组合物,其中,
所述表面修饰无机氧化物粒子的平均一次粒径为650nm以下。
5.根据权利要求1至权利要求4中任意一项所述的树脂组合物,其中,
以所述树脂组合物的总量为基准,所述表面修饰无机氧化物粒子的含量为1质量%以上45质量%以下。
6.一种光纤的初级被覆材料,包含权利要求1至权利要求5中任意一项所述的树脂组合物。
7.一种光纤,具备:
含有芯部和包层的玻璃纤维、
与所述玻璃纤维接触并被覆该玻璃纤维的初级树脂层、以及
被覆所述初级树脂层的次级树脂层,其中,
所述初级树脂层由权利要求1至权利要求5中任意一项所述的树脂组合物的固化产物构成。
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