JP6790865B2 - 感圧式接着剤及び接着フィルム - Google Patents
感圧式接着剤及び接着フィルム Download PDFInfo
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- JP6790865B2 JP6790865B2 JP2017009743A JP2017009743A JP6790865B2 JP 6790865 B2 JP6790865 B2 JP 6790865B2 JP 2017009743 A JP2017009743 A JP 2017009743A JP 2017009743 A JP2017009743 A JP 2017009743A JP 6790865 B2 JP6790865 B2 JP 6790865B2
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- Prior art keywords
- meth
- ether
- acrylate
- polyoxyethylene
- acid
- Prior art date
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- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
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- YKCNVAVAVLAKMO-UHFFFAOYSA-N prop-2-enoic acid;2,2,4-trimethylpentane-1,3-diol Chemical compound OC(=O)C=C.CC(C)C(O)C(C)(C)CO YKCNVAVAVLAKMO-UHFFFAOYSA-N 0.000 description 1
- GVVKBARIYRBZHC-UHFFFAOYSA-N prop-2-enyl 2,2-dimethylpropanoate Chemical compound CC(C)(C)C(=O)OCC=C GVVKBARIYRBZHC-UHFFFAOYSA-N 0.000 description 1
- ZQMAPKVSTSACQB-UHFFFAOYSA-N prop-2-enyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCC=C ZQMAPKVSTSACQB-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- GHJOIQFPDMIKHT-UHFFFAOYSA-N propane-1,2,3-triol;prop-2-enoic acid Chemical compound OC(=O)C=C.OCC(O)CO GHJOIQFPDMIKHT-UHFFFAOYSA-N 0.000 description 1
- KOPQZJAYZFAPBC-UHFFFAOYSA-N propanoyl propaneperoxoate Chemical compound CCC(=O)OOC(=O)CC KOPQZJAYZFAPBC-UHFFFAOYSA-N 0.000 description 1
- YPVDWEHVCUBACK-UHFFFAOYSA-N propoxycarbonyloxy propyl carbonate Chemical compound CCCOC(=O)OOC(=O)OCCC YPVDWEHVCUBACK-UHFFFAOYSA-N 0.000 description 1
- ILVGAIQLOCKNQA-UHFFFAOYSA-N propyl 2-hydroxypropanoate Chemical compound CCCOC(=O)C(C)O ILVGAIQLOCKNQA-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 229940116422 propylene glycol dicaprate Drugs 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 description 1
- 125000001422 pyrrolinyl group Chemical group 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 125000001308 pyruvoyl group Chemical group O=C([*])C(=O)C([H])([H])[H] 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000002441 reversible effect Effects 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
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229940079781 sodium cocoyl glutamate Drugs 0.000 description 1
- 229940079842 sodium cumenesulfonate Drugs 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 229940045944 sodium lauroyl glutamate Drugs 0.000 description 1
- 229940045845 sodium myristate Drugs 0.000 description 1
- 229950005425 sodium myristyl sulfate Drugs 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 229940045870 sodium palmitate Drugs 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- IWIUXJGIDSGWDN-UQKRIMTDSA-M sodium;(2s)-2-(dodecanoylamino)pentanedioate;hydron Chemical compound [Na+].CCCCCCCCCCCC(=O)N[C@H](C([O-])=O)CCC(O)=O IWIUXJGIDSGWDN-UQKRIMTDSA-M 0.000 description 1
- QBJDFZSOZNDVDE-UHFFFAOYSA-M sodium;1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F QBJDFZSOZNDVDE-UHFFFAOYSA-M 0.000 description 1
- ZQOXGRIKWKXDIJ-UHFFFAOYSA-M sodium;1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F ZQOXGRIKWKXDIJ-UHFFFAOYSA-M 0.000 description 1
- HMGYIWSXCDCHRF-UHFFFAOYSA-M sodium;2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,9-heptadecafluorononanoate Chemical compound [Na+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F HMGYIWSXCDCHRF-UHFFFAOYSA-M 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- PFIOPNYSBSJFJJ-UHFFFAOYSA-M sodium;2-octylbenzenesulfonate Chemical compound [Na+].CCCCCCCCC1=CC=CC=C1S([O-])(=O)=O PFIOPNYSBSJFJJ-UHFFFAOYSA-M 0.000 description 1
- QEKATQBVVAZOAY-UHFFFAOYSA-M sodium;4-propan-2-ylbenzenesulfonate Chemical compound [Na+].CC(C)C1=CC=C(S([O-])(=O)=O)C=C1 QEKATQBVVAZOAY-UHFFFAOYSA-M 0.000 description 1
- AIMUHNZKNFEZSN-UHFFFAOYSA-M sodium;decane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCS([O-])(=O)=O AIMUHNZKNFEZSN-UHFFFAOYSA-M 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 description 1
- QWSZRRAAFHGKCH-UHFFFAOYSA-M sodium;hexane-1-sulfonate Chemical compound [Na+].CCCCCCS([O-])(=O)=O QWSZRRAAFHGKCH-UHFFFAOYSA-M 0.000 description 1
- HRQDCDQDOPSGBR-UHFFFAOYSA-M sodium;octane-1-sulfonate Chemical compound [Na+].CCCCCCCCS([O-])(=O)=O HRQDCDQDOPSGBR-UHFFFAOYSA-M 0.000 description 1
- JUQGWKYSEXPRGL-UHFFFAOYSA-M sodium;tetradecanoate Chemical compound [Na+].CCCCCCCCCCCCCC([O-])=O JUQGWKYSEXPRGL-UHFFFAOYSA-M 0.000 description 1
- UPUIQOIQVMNQAP-UHFFFAOYSA-M sodium;tetradecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCOS([O-])(=O)=O UPUIQOIQVMNQAP-UHFFFAOYSA-M 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229940100515 sorbitan Drugs 0.000 description 1
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- 239000001593 sorbitan monooleate Substances 0.000 description 1
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- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
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- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
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- 239000007921 spray Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- WYKYCHHWIJXDAO-UHFFFAOYSA-N tert-butyl 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)C WYKYCHHWIJXDAO-UHFFFAOYSA-N 0.000 description 1
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- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 description 1
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- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- DTIFFPXSSXFQCJ-UHFFFAOYSA-N tetrahexylazanium Chemical compound CCCCCC[N+](CCCCCC)(CCCCCC)CCCCCC DTIFFPXSSXFQCJ-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
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
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- JOXIMZWYDAKGHI-UHFFFAOYSA-M toluene-4-sulfonate Chemical compound CC1=CC=C(S([O-])(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-M 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
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- MQVCTPXBBSKLFS-UHFFFAOYSA-N tri(propan-2-yloxy)-propylsilane Chemical compound CCC[Si](OC(C)C)(OC(C)C)OC(C)C MQVCTPXBBSKLFS-UHFFFAOYSA-N 0.000 description 1
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- LADGBHLMCUINGV-UHFFFAOYSA-N tricaprin Chemical compound CCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCC)COC(=O)CCCCCCCCC LADGBHLMCUINGV-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
- UOLQNMPEUKDNCD-UHFFFAOYSA-N tricosyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCCOC(=O)C=C UOLQNMPEUKDNCD-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([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])[H] 0.000 description 1
- ZLGWXNBXAXOQBG-UHFFFAOYSA-N triethoxy(3,3,3-trifluoropropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)F ZLGWXNBXAXOQBG-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- MEJYOZOPFBOWNM-UHFFFAOYSA-N triethyl(heptyl)azanium Chemical compound CCCCCCC[N+](CC)(CC)CC MEJYOZOPFBOWNM-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- DFJSZWHUOKADCX-UHFFFAOYSA-N triisocyanato(methyl)silane Chemical compound O=C=N[Si](C)(N=C=O)N=C=O DFJSZWHUOKADCX-UHFFFAOYSA-N 0.000 description 1
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- AQZSPJRLCJSOED-UHFFFAOYSA-M trimethyl(octyl)azanium;chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(C)C AQZSPJRLCJSOED-UHFFFAOYSA-M 0.000 description 1
- WNWMJFBAIXMNOF-UHFFFAOYSA-N trimethyl(propyl)silane Chemical compound CCC[Si](C)(C)C WNWMJFBAIXMNOF-UHFFFAOYSA-N 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
- SZYJELPVAFJOGJ-UHFFFAOYSA-N trimethylamine hydrochloride Chemical compound Cl.CN(C)C SZYJELPVAFJOGJ-UHFFFAOYSA-N 0.000 description 1
- LAGQNGWYNLUQRI-UHFFFAOYSA-N trioctylmethylammonium bis(trifluoromethylsulfonyl)imide Chemical compound FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F.CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC LAGQNGWYNLUQRI-UHFFFAOYSA-N 0.000 description 1
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 1
- OLTVTFUBQOLTND-UHFFFAOYSA-N tris(2-methoxyethoxy)-methylsilane Chemical compound COCCO[Si](C)(OCCOC)OCCOC OLTVTFUBQOLTND-UHFFFAOYSA-N 0.000 description 1
- KYJXEJLEWKXHOC-UHFFFAOYSA-N tris(3-methoxypropoxy)-methylsilane Chemical compound COCCCO[Si](C)(OCCCOC)OCCCOC KYJXEJLEWKXHOC-UHFFFAOYSA-N 0.000 description 1
- RHZZVWTVJHZKAH-UHFFFAOYSA-K trisodium;naphthalene-1,2,3-trisulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(S([O-])(=O)=O)=C(S([O-])(=O)=O)C(S(=O)(=O)[O-])=CC2=C1 RHZZVWTVJHZKAH-UHFFFAOYSA-K 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- IFNXAMCERSVZCV-UHFFFAOYSA-L zinc;2-ethylhexanoate Chemical compound [Zn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O IFNXAMCERSVZCV-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Description
この表面保護フィルムを貼着した光学部材等の積層体が、簡単に剥離できるだけでなく、高温下、又は高温高湿条件下等の過酷な環境下でも発泡、浮き・剥がれが生じないようにするため、アクリル系樹脂、シリコーン樹脂、またはポリウレタン系樹脂を含む感圧式接着剤が用いられてきた。
尚、本明細書では、水酸基を有するエチレン性不飽和化合物(a1)単位、炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)単位、及び水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)単位を、それぞれ、化合物(a1)、化合物(a2)、及び化合物(a3)と略記することがある。
また、「(メタ)アクリル」、「(メタ)アクリロイル」、「(メタ)アクリル酸」、「(メタ)アクリレート」、「(メタ)アクリロイルオキシ」、及び「(メタ)アリル」と表記した場合には、特に説明がない限り、それぞれ、「アクリルまたはメタクリル」、「アクリロイルまたはメタクリロイル」、「アクリル酸またはメタクリル酸」、「アクリレートまたはメタクリレート」、「アクリロイルオキシまたはメタクリロイルオキシ」、及び「アリルまたはメタリル」を表すものとする。
以下、感圧式接着剤の構成成分について具体的に説明する。
水酸基を有する共重合体(A)は、構成する単量体単位として、水酸基を有するエチレン性不飽和化合物(a1)単位、炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)単位、水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)単位を含有する樹脂であり、これら単量体混合物を重合して製造した樹脂である。
化合物(a1)は、その構造中に、水酸基と、エチレン性不飽和二重結合基とを有する化合物であり、水酸基とエチレン性二重結合基とを有し、エチレンオキサイドユニットを有しない化合物(a1−1)と、エチレンオキサイドユニットを有する化合物(a1−2)に類別することができる。ここで、エチレンオキサイドユニットとは、エチレンオキサイド(EO)の繰り返し単位が2以上であることを示す。
次に、炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)について説明する。
炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)は、疎水性を示す非極性単量体であり、ガラス板等の極性被着体に対して、微粘領域で十分な接着性を発現することが可能となる。ここで「極性基」とは、極性を有する基を指し、主として、ハメット(Hammett)の置換基定数、パラ効果σpが−0.20〜0.24の範囲外の基を意味する。ただし、エステル基およびビニルエーテル基は、極性基から除外して取り扱うものとする。
炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)としては、直鎖状長鎖アルキル基を有することが好ましいが、直鎖状長鎖アルキル基を有することで分子配向により疑似結晶性を示すため、凝集力が向上し、高温高湿条件下等の過酷な環境下でも発泡、浮き・剥がれが生じない耐久性を維持することができる。直鎖状長鎖アルキル基としては、炭素数14〜24の直鎖状長鎖アルキル基が好ましく、また、炭素数14〜24の分岐アルキル基も併用することが可能である。
続いて、水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)について説明する。
水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)は、親水性が高い、高極性部位を有するため、高温条件下等の過酷な環境下でも発泡、浮き・剥がれが生じない高耐熱性を維持でき、また高い分子内凝集力を有するため、本発明の感圧式接着剤を使用した感圧接着フィルムをガラス板等の極性の高い被着体に対して貼着した場合には、優れた濡れ広がり性を示すことが可能となる。尚、水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)は、上で説明した炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)を除くものである。
また、化合物(a3)は、芳香環を有しないことが好ましい。芳香環を含有していないために著しい黄変もなく、良好なの耐久性を発現することが可能となる。
さらに、エチレンオキサイドユニットにおけるエチレンオキサイド(EO)付加モル数としては、2〜30モルの範囲が好ましい。付加モル数が上記の範囲にあると適度な極性を保ちつつ、接着フィルムの白化を抑制し、また接着フィルムの接着層表面に配向しやすいため、微粘領域での接着性と貼着後の耐久性が著しく向上するという利点がある。
続いて、その他エチレン性不飽和化合物(a4)について説明する。
その他エチレン性不飽和化合物(a4)は、上記化合物(a1)、化合物(a2)及び化合物(a3)以外のエチレン性不飽和化合物である。
化合物(a4)を構成単量体の一部として使用することにより、共重合体(A)を構成する単量体単位である化合物(a1)、化合物(a2)または化合物(a3)との共重合反応の効率化を図ることが容易となることがある。また、共重合体(A)を容易に低粘度化できるとともに、塗工時の作業性を向上させることが容易となることがある。
さらに、共重合体(A)の重量平均分子量(Mw)を適度に制御可能としたり、接着層のガラス転移温度(以下、Tgと称す)を制御させて粘着性(タックとも称す)を低減したり、接着層の凝集力を向上させて、耐熱性や耐水性等の耐性の良好な接着層を形成することが可能となることがある。
化合物(a4)のなかでも、単独重合体(ホモポリマーとも称す)のTgが、−80〜0℃であり、炭素数2〜13のアルキル基を有するα,β−不飽和二重結合基含有化合物(a4−1)を共重合反応の単量体単位として使用することが好ましい。化合物(a4−1)を共重合反応の単量体単位として使用することにより、共重合体(A)のタックを制御でき、また接着フィルムの濡れ広がり性を向上することが可能となるため、表面保護フィルムとして、より好適に使用することが可能となる。
<FOX式>1/Tg=W1/Tg1+W2/Tg2+…+Wi/Tgi+…+Wn/Tgn
〔上記FOX式は、n種のα,β−不飽和二重結合基含有化合物からなる重合体を構成する各化合物の単独重合体のガラス転移温度をTgi(K)とし、各化合物の質量分率を、Wiとしており、(W1+W2+…+Wi+…Wn=1)である。〕
次に、水酸基と反応し得る官能基を有する反応性化合物(B)について説明する。
本明細書において水酸基と反応し得る官能基を有する反応性化合物(B)(以下、反応性化合物(B)と称す。)は、共重合体(A)100質量部に対し、0.1〜50質量部含有することが必要であり、1〜30質量部がより好ましい。反応性化合物(B)がこの範囲であると、共重合体(A)に含有されている水酸基との架橋反応により耐熱性や耐湿熱性が向上するだけでなく、過酷な環境下での接着層の浮き、剥がれ、あるいは発泡を抑えることができ、表面保護フィルムへの適用が可能となる。
反応性化合物(B)は、例えば、ポリイソシアネート(b1)、シラン化合物(b2)、メチロールメラミン系化合物(b3)等が挙げられる。反応性化合物(B)は、これらの中でも架橋性を付与るために、ポリウレタン樹脂(A)の水酸基と反応し得る官能基を分子内に2個以上有する化合物が好ましく用いられる。
特にポリイソシアネート(b1)は、架橋反応後の接着性や後述の基材(G)への密着性に優れていることから好ましく用いられる。
錫系化合物は、例えば、ジブチル錫ジクロライド、ジブチル錫オキサイド、ジブチル錫ジブロマイド、ジブチル錫ジマレエート、ジブチル錫ジラウレート(別名:DBTDL)、ジブチル錫ジアセテート、ジブチル錫スルファイド、トリブチル錫スルファイド、トリブチル錫オキサイド、トリブチル錫アセテート、トリエチル錫エトキサイド、トリブチル錫エトキサイド、ジオクチル錫オキサイド、トリブチル錫クロライド、トリブチル錫トリクロロアセテート、2−エチルヘキサン酸錫等が挙げられる。
非錫系化合物は、例えば、ジブチルチタニウムジクロライド、テトラブチルチタネート、ブトキシチタニウムトリクロライドなどのチタン系、オレイン酸鉛、2−エチルヘキサン酸鉛、安息香酸鉛、ナフテン酸鉛などの鉛系化合物、2−エチルヘキサン酸鉄、鉄2,4−ペンタジオネートなどの鉄系化合物、安息香酸コバルト、2−エチルヘキサン酸コバルトなどのコバルト系、ナフテン酸亜鉛、2−エチルヘキサン酸亜鉛などの亜鉛系化合物、ナフテン酸ジルコニウム等が挙げられる。
これらの中でも反応性や衛生性の点でジアザビシクロウンデセン(別名:DBU)、ジブチル錫ジラウレート(別名:DBTDL)、2−エチルヘキサン酸錫等が好ましい。
触媒は、単独または2種類以上が併用できる。
これらの中でも被着体に対する濡れ広がり性の点で、芳香環を有しないシラン化合物が好ましい。
また、シラン化合物(b2)は、共重合体(A)の水酸基との縮合反応や、基材表面への密着性向上の点で、メチルトリメトキシシラン、メチルトリエトキシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン等のアルキル系アルコキシシラン、3−メルカプトプロピルトリメトキシラン、3−メルカプトプロピルトリエトキシシラン等のメルカプト系アルコキシシラン、3−グリシドキシプロピルトリメトキシシラン、3−グリシドキシプロピルトリエトキシシラン、2−(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等のエポキシ系アルコキシシラン、3−(2−イミダゾリン−1−イル)プロピルトリエトキシシラン等のイミダゾール系アルコキシシラン、3−アミノプロピルトリメトキシシラン、3−アミノプロピルトリエトキシシラン、3−アミノプロピルメチルジメトキシシラン、3−アミノプロピルメチルジエトキシシラン、3−アミノプロピルエチルジエトキシシラン、3−アミノプロピルジメチルエトキシシラン、2−シクロヘキシルアミノエチルチオメチルトリメトキシシラン、トリメチルシリルジメチルアミン等のアミノ系アルコキシシラン、3−イソシアネートプロピルトリエトキシシラン等のイソシアネート系アルコキシシランが好ましい。シラン化合物(b2)は、単独または2種類以上を併用できる。
これらの中でも共重合体(A)の水酸基との縮合反応や、基材表面への密着性向上の点から、ペンタメトキシメチロールメラミン、ヘキサメトキシメチルメラミンが好ましい。
メチロールメラミン系化合物(b3)は、単独または2種類以上を併用できる。
次に、界面活性剤(C)について説明する。
本発明の感圧式接着剤は、上記必須成分に加えて、界面活性剤(C)を含むことが必須である。
界面活性剤(C)は、共重合体(A)の極性部位と非極性部位の相溶化に寄与し、感圧式接着剤の白化抑制、さらに接着フィルムの白化を抑制することが可能となる。また、接着層に可塑効果を付与し、接着フィルムのガラス板等の被着体への濡れ広がり性をさらに向上させることができる。また、接着フィルムを被着体に貼着後、剥離時の剥離を軽くすることや接着面同士の自着性を低減することが可能となるため作業性が向上する。また、被着体に糊残り等の汚染を抑制することができる。
ここで、HLBとは、界面活性剤の水と油(水に不溶性の有機化合物)への親和性の程度を表す値であり、計算によって決定する方法がいくつか提案されているが、ノニオン性界面活性剤(c4)のHLB値は、以下の川上法にて計算されたものである。
<川上法>
HLB=7+11.7×log(親水部の化学式量の総和/親油部の化学式量の総和)
さらに、イオン性化合物(D)について説明する。
本願の感圧式接着剤の一実施形態において、感圧式接着剤は、上記必須成分に加えて、さらにイオン性化合物(D)を含んでもよい。なお、共重合体(A)、水酸基と反応し得る官能基を有する反応性化合物(B)、および界面活性剤(C)以外の成分を任意成分という。但し、イオン性化合物(D)は、界面活性剤(C)を除く。
イオン性化合物(D)は、常温(25℃)で液状、または固体状のイオン性化合物である。イオン性化合物(D)は、アルカリ金属の無機塩、アルカリ金属の有機塩等がを挙げられる。また、イオン性化合物(D)は、塩化アンモニウム、塩化アルミニウム、塩化銅、塩化第一鉄、塩化第二鉄、硫酸アンモニウム等も挙げられる。これらの中でもアルカリ金属塩、液状イオン性化合物、固体状イオン性化合物が好ましく、アルカリ金属塩、液状イオン性化合物がより好ましい。
イオン性化合物(D)は、単独または2種類以上を併用できる。
本発明の感圧式接着剤の一実施形態において、本発明による効果を損なわない範囲であれば、感圧式接着剤には、上記必須成分に加えて、その他成分(P)を適宜配合することも可能である。その他成分(P)は、例えば、重合硬化収縮率低減、熱膨張率低減、寸法安定性向上、弾性率向上、酸化還元抑制、粘度調整、熱伝導率向上、強度向上、靭性向上、および着色向上等の観点から、有機又は無機の添加剤や充填剤を配合することができる。充填剤は、ポリマー、セラミックス、金属、金属酸化物、金属塩、および染顔料等から構成される。充填剤の形状は、例えば、粒子状および繊維状等が好ましい。また、添加剤は、酸化防止剤、難燃化剤、保存安定剤、光安定剤、紫外線吸収剤、チクソトロピー付与剤、分散安定剤、流動性付与剤、増粘剤、保湿剤、pH調整剤、レベリング剤、加水分解抑制剤および消泡剤等が挙げられ、添加する方法は、通常混合に加え、ポリマーブレンド又はポリマーアロイとして、感圧式接着剤中に、溶解、半溶解又はミクロ分散させることも可能である。
次に感圧式接着剤について説明する。「感圧式接着剤」とは、慣用的には粘着剤とも称し、接着剤の固化によらず、粘稠な性質を有し、常温で短時間、圧力を加えるだけで接着する接着剤のことを意味する。本発明の感圧式接着剤は、上で述べた共重合体(A)、水酸基と反応し得る官能基を有する反応性化合物(B)および界面活性剤(C)を含む事が特徴であり、必要に応じて、任意成分であるイオン性化合物(D)及びその他成分(P)を適宜配合したものである。
次に接着フィルムについて、説明する。本発明の接着フィルム(感圧式接着フィルムとも称す)は、後述の基材(G)上に上記の感圧式接着剤からなる接着層が形成されたものであり、表面を剥離処理したフィルム状基材(剥離ライナーとも称す)が積層されていても良い。接着フィルムを製造する場合、常法にしたがって適当な方法で、後述の基材に感圧式接着剤を塗工した後、感圧式接着剤が有機溶剤や水等の液状媒体を含有する場合には、加熱等の方法により液状媒体を除去したり、感圧式接着剤が揮発すべき液状媒体を含有しない場合は、溶融状態にある接着層を冷却して固化したりして、基材の上に接着層を形成することができる。例えば、剥離ライナーの剥離処理面に感圧式接着剤を塗工、乾燥し、基材を貼り合わせて作成する方法、または剥離ライナー以外の基材に感圧式接着剤を直接塗工、乾燥し、接着層の表面に剥離ライナーの剥離処理面を貼り合わせて作成する方法が挙げられる。
透明フィルム(H)が、保護フィルムとして用いられる場合、接着層を形成しない反対の面には、脂肪酸アミド、ポリエチレンイミン、長鎖アルキル系添加剤等を添加して離型処理を行ったり、シリコーン系、長鎖アルキル系、フッ素系などの任意の適切な剥離剤からなるコート層を設けたりすることができる。
(合成例1)
反応槽、攪拌機、温度計、還流冷却器、滴下装置、窒素導入管を備えた重合反応装置の反応槽及び滴下装置に、下記単量体、重合開始剤及び有機溶剤をそれぞれ下記の比率で仕込んだ。
アクリル酸ステアリル(a2) 15.07部
メタクリル酸セチル(a2) 57.24部
メチルエチルケトン(有機溶剤) 12.84部
V65(重合開始剤) 0.05部
[滴下装置]
アクリル酸2−ヒドロキシエチル(a1−1) 3.24部
メトキシポリオキシエチレンアクリレート(a3) 4.48部
アクリル酸エチル(a4−1) 19.53部
酢酸エチル(有機溶剤) 12.84部
V65(重合開始剤) 0.05部
表1に記載した材料を合成例1と同様に、化合物(a2)、有機溶剤及び重合開始剤は重合槽に仕込み、化合物(a1)、化合物(a3)、化合物(a4)、有機溶剤及び重合開始剤は滴下装置に仕込んで、それぞれ共重合体(A)および共重合体(A)ではない共重合体を合成した。これらの内、合成例1〜12、15〜25、28〜35で得られた共重合体が共重合体(A)であり、合成例13、14、26、及び27で得られた共重合体が共重合体(A)ではない共重合体である。得られた共重合体溶液の溶液外観、不揮発分濃度(NV)、溶液粘度(Vis)、共重合体の水酸基価(OHV)、共重合体の重量平均分子量(Mw)及びガラス転移温度(Tg)を、後述の方法に従って求め、結果を表1に示した。また、酸価(AV)の測定方法についても記載した。尚、表1に記載された単量体として使用した化合物は、重合槽への仕込み量と滴下装置への仕込み量との合計値(部)を表す。
各合成例で得られた共重合体溶液の外観を25℃の条件下で、目視にて観察した。無色透明であれば良好である。
各合成例で得られた共重合体の溶液、約1gを金属容器に秤量し、150℃オーブン中にて20分間乾燥して、残分を秤量して残率計算をし、不揮発分濃度(固形分)とした(単位:%)。
各合成例で得られた共重合体溶液を25℃でB型粘度計(東機産業社製 TV−22)にて、ローターNo3、回転速度0.5〜100rpm、1分間回転の条件で測定し、溶液粘度(mPa・s)とした。
数平均分子量(Mn)と重量平均分子量(Mw)の測定は、昭和電工社製GPC(ゲルパーミエーションクロマトグラフィー)を用いた。数平均分子量(Mn)と重量平均分子量(Mw)の決定は、標準物質であるポリスチレンの換算値とした。
装置名:昭和電工社製GPC(ゲルパーミエーションクロマトグラフィー)「ShodexGPC System−21」
カラム:東ソー社製GMHXL:4本、東ソー社製HXL-H:1本を直列に連結した。
移動相溶媒 : テトラヒドロフラン(THF)
流量 : 1.0ml/分
カラム温度 : 40℃
共栓三角フラスコ中に試料約1gを精密に量り採り、トルエン/エタノール(容量比:トルエン/エタノール=2/1)混合液100mlを加えて溶解した。次いで、アセチル化剤(無水酢酸25gをピリジンで溶解し、容量100mlとした溶液)を5ml加え、1時間攪拌した。これに、フェノールフタレイン試液を指示薬として加え、30秒間保持した。その後、溶液が淡紅色を呈するまで0.1Nアルコール性水酸化カリウム溶液で滴定した。
水酸基価は次式により求めた。水酸基価は樹脂の乾燥状態の数値とした(単位:mgKOH/g)。
水酸基価(mgKOH/g)=[{(b−a)×F×28.25}/S]/(不揮発分濃度/100)+D
ただし、S:試料の採取量(g)
a:0.1Nアルコール性水酸化カリウム溶液の消費量(ml)
b:空実験の0.1Nアルコール性水酸化カリウム溶液の消費量(ml)
F:0.1Nアルコール性水酸化カリウム溶液の力価
D:酸価(mgKOH/g)
共栓三角フラスコ中に試料約1gを精密に量り採り、トルエン/エタノール(容積比:トルエン/エタノール=2/1)混合液100mlを加えて溶解した。これに、フェノールフタレイン試液を指示薬として加え、30秒間保持した後、溶液が淡紅色を呈するまで0.1Nアルコール性水酸化カリウム溶液で滴定した。
酸価は次式により求めた。酸価は樹脂の乾燥状態の数値とした(単位:mgKOH/g)。
酸価(mgKOH/g)={(5.611×a×F)/S}/(不揮発分濃度/100)
ただし、S:試料の採取量(g)
a:0.1Nアルコール性水酸化カリウム溶液の消費量(ml)
F:0.1Nアルコール性水酸化カリウム溶液の力価
ロボットDSC(示差走査熱量計、セイコーインスツルメンツ社製「RDC220」)に「SSC5200ディスクステーション」(セイコーインスツルメンツ社製)を接続して、測定に使用した。
試料約10mgをアルミニウムパンに入れ、秤量して示差走査熱量計にセットし、試料を入れない同タイプのアルミニウムパンをリファレンスとして、100℃の温度で5分間保持した後、液体窒素を用いて−120℃まで急冷した。その後、昇温速度10℃/分で昇温し、得られたDSCチャートからガラス転移温度(Tg、単位:℃)を決定した。
・化合物(a1−1)
2HEA:アクリル酸2−ヒドロキシエチル、4HBA:アクリル酸4−ヒドロキシブチル、TPMA:テトラプロピレングリコールモノメタクリレート、ESTA:6−{2−(アクリロイルオキシ)エトキシ}−6−オキソヘキシル 6−ヒドロキシヘキサノエート、HPPA:アクリル酸2−ヒドロキシ−3−フェノキシプロピル
・化合物(a1−2)
DEGA:ジエチレングリコールモノアクリレート、EOMA:ポリオキシエチレンモノメタクリレート(EO付加モル数:5)、TEGVE:トリエチレングリコールモノビニルエーテル
CeMA:メタクリル酸セチル、StA:アクリル酸ステアリル、ArA:アクリル酸アラキジル、BeA:アクリル酸ベヘニル、FDEA:アクリル酸2−パーフルオロドデシルエチル
・炭素数25以上のアルキル基を有するエチレン性不飽和化合物
McA:アクリル酸ミリシル
・炭素数14〜24のアルキル基と極性基の双方を有するエチレン性不飽和化合物
HDOA:アクリリック 8−(3−ヘキサデシルオキシラン−2−イル)オクタノイックアンヒドライド(下記構造の化合物)
MO9A:メトキシポリオキシエチレンアクリレート(EO付加モル数:9)、MO9MA:メトキシポリオキシエチレンメタクリレート(EO付加モル数:9)、OEPMA:オクチルオキシポリオキシエチレンポリオキシプロピレンメタクリレート(EO付加モル数:8、PO付加モル数:6)、PHEOA:フェノキシポリオキシエチレンモノアクリレート(EO付加モル数:2)、TEBVE:トリエチレングリコールブチルビニルエーテル
・化合物(a4−1)
EA:アクリル酸エチル、BA:アクリル酸n−ブチル、2EHA:アクリル酸2−エチルヘキシル、LMA:メタクリル酸ラウリル
・化合物(a4−2)
MA:アクリル酸メチル、MMA:メタクリル酸メチル、PHEA:アクリル酸フェノキシエチル、MPOA:メトキシポリオキシプロピレンアクリレート(PO付加モル数:9)
V65:2,2’−アゾビス(2,4−ジメチルバレロニトリル) [和光純薬工業社製「V65」]、PBO:t−ブチルパーオキシ−2−エチルヘキサノエート [日油社製「パーブチルO」]
・有機溶剤
ACE:アセトン、MEK:メチルエチルケトン、MEAC:酢酸メチル、EAC:酢酸エチル、TOL:トルエン
得られた共重合体と反応性化合物(B)を表2に記載した質量比(部)に従い、共重合体100部に対して、必要に応じて任意成分を、表2に挙げた質量比(部)で配合し、有機溶剤として酢酸エチルを加えて不揮発分濃度を50%になるように調整し、感圧式接着剤を得た。得られた感圧式接着剤を各基材に塗工、乾燥、養生はおよび貼り合わせを施し、接着フィルムを作成し、以下の方法で評価した。それぞれの結果を表3に示す。
得られた感圧式接着剤について、配合後、25℃における粘度を1時間おきに8時間後まで、B型粘度計(東機産業社製TV−22)を用い、ローターNo.3、25℃、12rpm、1分間回転の条件で測定し、ポットライフを3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:8時間までの粘度上昇率が50%未満。良好。
△:8時間までの粘度上昇率が50%以上〜100%未満。実用上使用可能。
×:8時間未満で溶液層の分離や濁りが発生したり、ゲル化したり、または粘度上昇率が100%以上と認められる。実用不可。
ここで、粘度上昇率は、下記の方法で算出した。
粘度上昇率(%)=100×{(8時間保存後の粘度)−(調整直後の粘度)}/(調整直後の粘度)
得られた感圧式接着剤を、基材として厚さ38μmの剥離処理されたポリエチレンテレフタレートフィルム(セラピールMF:東レフィルム加工社製)(以下、「剥離ライナー」という。)上に、乾燥後の厚さが25μmになるように塗工し、100℃で2分間熱風乾燥することで接着層を形成した。次いで、上記塗工面に100μm厚のポリエチレンテレフタレートフィルム(PETフィルム)を貼り合せて、100μm厚PETフィルム/接着層/剥離ライナーで構成された接着フィルムを作製した。そして剥離ライナーを剥がした後の接着層表面(塗工面)の状態を目視にて観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:平滑な塗工面が得られた。良好。
△:塗工面の端部に若干のハジキや発泡が認められる。実用上使用可。
×:塗工面にハジキ、発泡やスジ引きが認められた。不良。
得られた感圧式接着剤を、上記剥離ライナー上に、乾燥後の厚さが50μmになるように塗工し、100℃で2分間熱風乾燥することで接着層を形成した。次いで、別途用意した剥離ライナーを接着層に貼り合せて、接着層が剥離ライナーで挟持された接着フィルムを作製し、23℃相対湿度50%の環境下で7日間養生した。
次に、両方の剥離ライナーを取り除き、接着層単体の外観を目視判定するとともに、ヘイズを「NDH−300A(日本電色工業社製)」で測定した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:曇り等が観察されず、かつHAZE:0.5未満。良好。
△:曇り等は観察されないが、HAZE:0.5以上2未満、実用上支障無く使用できる。
×:曇りが観察される、またはHAZE:2以上。不良。
上記、《塗工性の評価》と同じ方法により作成した各接着フィルムを、23℃相対湿度50%の環境下で7日間養生した。その後、幅100mm×長さ100mmに裁断し、これを20枚重ね、40℃−60Kg/cm2の条件で1時間プレスした際の接着フィルム端部からの接着層のはみ出しの様子を以下のように3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:接着層のはみ出しが観測されない。良好。
△:0.3mm未満の接着層のはみ出しが観測されるが、実用上使用可能。
×:0.3mm以上の接着層のはみ出しが観測される。不良。
得られた感圧式接着剤を、基材として厚さ50μmのポリエチレンテレフタレートフィルム(PETフィルム)上に、乾燥後の厚さが15μmになるように塗工し、100℃で2分間熱風乾燥することで、接着層を形成した。次いで、塗工面に38μmの剥離ライナー(セラピールMF:東レフィルム加工社製)を貼り合せて、50μm厚PETフィルム/接着層/剥離ライナーの構成の接着フィルムを作製し、23℃相対湿度50%の環境下で7日間養生した。そして、この接着フィルムを、幅100mm×長さ100mmに裁断して測定試料とした。次に、厚み2mm×幅150mm×長さ150mmのフロートガラス板に、上記接着フィルムの剥離ライナーを剥がした接着層の一辺のみをフロートガラス板に45°傾けた状態で接触させ、その後、手を離し、上記試料全面が、ガラス板に接触する(ガラス板に濡れ広がる)のに要した時間(秒)を濡れ広がり性として、以下の3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:濡れ広がる時間が2秒未満。良好。
△:濡れ広がる時間が2秒以上、4秒未満。実用上使用可能。
×:濡れ広がる時間が4秒以上。不良。
上記、《濡れ広がり性の評価》と同じ方法により作成した各接着フィルムを、幅25mm×長さ100mmに裁断し、剥離ライナーを剥がし、露出した接着層を厚さ1.2mmの無アルカリガラス板に23℃、相対湿度50%の環境下で、ラミネータを用いて貼着した。続いて、50℃、5気圧の条件のオートクレーブ内に20分間保持して測定試料を得た。上記測定試料を、23℃で1日間放置した後に、23℃、相対湿度50%の環境下で、引張試験機(オリエンテック社製「テンシロン」)を用いて、剥離速度300mm/分、剥離角度180度の条件で剥離強度を測定した(貼合せ1日後の剥離強度測定)。また、上記測定試料を、23℃、相対湿度50%の環境下で14日間放置した後に、同様の方法で剥離強度を測定した(貼合せ14日後の剥離強度測定)。この剥離強度を接着力として3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:接着力が10.0(mN/25mm)未満。良好。
△:接着力が10.0(mN/25mm)以上15.0(mN/25mm)未満。実用可。
×:接着力が15.0(mN/25mm)以上。不良で実用不可。
上記、《濡れ広がり性の評価》と同じ方法により作成した各接着フィルムを、25mm×150mmの大きさに裁断し、剥離ライナーを剥がし、厚さ2mmのフロートガラス板にラミネータを用いて貼り付け、50℃で5気圧の条件のオートクレーブ内に20分保持させて、接着フィルムとガラス板との光学積層体を得た。
この積層体の接着フィルムを180度方向に50mm/分の速度で引き剥がし、剥離後のガラス表面の曇りを目視で観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:曇りがなく、実用上全く問題がない。非常に良好。
△:若干曇りが認められるが、実用上問題ない。良好。
×:全面的に感圧式接着剤の転着が認められ、実用不可である。
耐熱性試験として、上記《濡れ広がり性の評価》と同じ方法により作成した接着フィルムを、幅100mm×長さ100mmに裁断した。次いで、接着フィルムの剥離ライナーを剥がし、露出した接着層を厚さ1.2mmの無アルカリガラス板の片面に、50℃雰囲気下で5Kg/cm2の圧力を加え、20分間オートクレーブ内に保持して貼り合せた後、80℃の雰囲気中に500時間放置した。放置後、25℃に戻し、接着フィルムの浮き・剥がれ、発泡の発生状態を目視で観察し、3段階で評価した。
耐湿熱性試験として、耐熱性試験と同様に試料を作製し、60℃−相対湿度90%の恒温恒湿槽に500時間放置した。。放置後、25℃に戻し、接着フィルムの浮き・剥がれ、発泡の発生状態を目視で観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
発泡とは、接着層とガラスとの界面(周辺端部以外)に比較的大きな気泡が発生している状態である。
浮き・剥がれとは、偏光フィルム接着フィルムがガラスから浮き上がり、剥がれてしまっている状態である。
それぞれの評価基準は以下の通りである。
○:発泡、浮き・剥がれが全く発生せず。良好。
△:直径0.5mm以下の発泡、浮き、剥がれのいずれかの軽微な発生が認められるが、実用上使用可能。
×:全面的に発泡、浮き、剥がれ等、顕著な発生が認められる。実用上使用不可。
・共重合体
表1記載の各合成例で得られた化合物(合成例1〜35)
・水酸基と反応し得る官能基を有する反応性化合物(B)
HDI/TMP:ヘキサメチレンジイソシアネートのトリメチロールプロパンアダクト体、HDI/Nu:ヘキサメチレンジイソシアネートのイソシアヌレート環を有する3量体、IPDI/TMP:3−イソシアネートメチル−3,5,5−トリメチルシクロヘキシルイソシアネートのトリメチロールプロパンアダクト体、XDI/TMP:キシリレンジイソシネートのトリメチロールプロパンアダクト体、MAS:3−アミノプロピルトリメトキシシラン、EPS:3−グリシドキシプロピルトリメトキシシラン、PMMM:ペンタメトキシメチロールメラミン
EOLAA:ポリオキシエチレンラウリルエーテル硫酸アンモニウム(EO付加モル数:8)、EOLPA:ポリオキシエチレンオレイルエーテルリン酸アンモニウム(EO付加モル数:10)、PD104:2−メチル−1-ブテン−ポリオキシエチレンポリオキシブチレンエーテルスルホン酸アンモニウム(EO付加モル数:15,BO付加モル数:6)[花王社製「ラムテルPD−104」]、SR20:ポリオキシエチレン−1−(アリルオキシメチル)アルキルエーテルグリセリンスルホン酸エステル(EO付加モル数:20)[アデカ社製「アデカソープSR20」]、OLA オレイン酸アンモニウム、
CLDMA:塩化ドデシルトリメチルアンモニウム、DAMSB:ドデシルアミノメチルジメチルスルホプロピルベタイン、EOLA:ポリオキシエチレンラウリルエーテル(EO付加モル数:4)
OPFI:1−オクチル−4−メチルピリジニウムビス(トリフルオロメタンスルホニル)イミド、PAFI:トリエチルプロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド
・その他成分(P)
AO50:フェノール系酸化防止剤 [アデカ社製「アデカスタブ AO−50」]
また、実施例12〜15、22〜25、29、34、48〜51、58〜61、65、66、78及び80〜86においては、各評価の「△」評価(実用可能レベル)が10項目中4〜10個であり、「×」評価(不良レベル)が一つもないため、実用上支障なく使用することが可能である。
これに対して、比較例1〜5では、光学特性、加工性、濡れ広がり性、剥離強度、再剥離性、耐熱性、及び耐湿熱性のいずれかが極端に劣ることがわかる。
Claims (10)
- 水酸基を有する共重合体(A)、水酸基と反応し得る官能基を有する反応性化合物(B)、及び界面活性剤(C)とを含み、
共重合体(A)を構成する単量体単位として、水酸基を有するエチレン性不飽和化合物(a1)単位、炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)単位、及び水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)単位を含有する、感圧式接着剤。 - 前記共重合体(A)は、重量平均分子量100,000〜2,000,000であり、
前記共重合体(A)100質量部に対して、前記水酸基と反応し得る官能基を有する反応性化合物(B)0.1〜50質量部を含み、前記界面活性剤(C)0.1〜100質量部を含む、請求項1記載の感圧式接着剤。 - 前記共重合体(A)の水酸基価が、1〜60mgKOH/gある、請求項1または2記載の感圧式接着剤。
- 前記炭素数14〜24のアルキル基を有し、極性基を有しないエチレン性不飽和化合物(a2)が、芳香環を有しない、請求項1〜3いずれか1項に記載の感圧式接着剤。
- 前記共重合体(A)を構成する単量体単位100質量%中に、水酸基を有しないエチレンオキサイドユニットを有するエチレン性不飽和化合物(a3)単位を0.1〜50質量%を含む、請求項1〜4いずれか1項に記載の感圧式接着剤。
- 前記反応性化合物(B)が、ポリイソシアネート(b1)を含む、請求項1〜5いずれか1項に記載の感圧式接着剤。
- 前記界面活性剤(C)が、アニオン性界面活性剤(c1)である、請求項1〜6のいずれか1項に記載の感圧式接着剤。
- 前記アニオン性界面活性剤(c1)が、スルホン酸エステル塩、硫酸エステル塩、及びリン酸エステル塩からなる群より選ばれる一種以上を含む、請求項7に記載の感圧式接着剤。
- 基材(G)および、請求項1〜8いずれか1項に記載の感圧式接着剤からなる接着層を備えた、感圧式接着フィルム。
- 光学フィルム、請求項1〜8いずれか1項に記載の感圧式接着剤からなる接着層、およびガラスを備えた、光学積層体。
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