JP2016138206A - 粘着フィルム - Google Patents
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- Publication number
- JP2016138206A JP2016138206A JP2015014868A JP2015014868A JP2016138206A JP 2016138206 A JP2016138206 A JP 2016138206A JP 2015014868 A JP2015014868 A JP 2015014868A JP 2015014868 A JP2015014868 A JP 2015014868A JP 2016138206 A JP2016138206 A JP 2016138206A
- Authority
- JP
- Japan
- Prior art keywords
- film
- polyester
- acid
- meth
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002313 adhesive film Substances 0.000 title abstract description 24
- 239000010410 layer Substances 0.000 claims abstract description 118
- 229920006267 polyester film Polymers 0.000 claims abstract description 50
- 239000012790 adhesive layer Substances 0.000 claims abstract description 33
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims abstract description 14
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000013638 trimer Substances 0.000 abstract description 71
- 238000000034 method Methods 0.000 abstract description 60
- 238000010438 heat treatment Methods 0.000 abstract description 41
- 230000008569 process Effects 0.000 abstract description 15
- 239000012298 atmosphere Substances 0.000 abstract description 5
- 230000006866 deterioration Effects 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 114
- -1 polyethylene terephthalate Polymers 0.000 description 88
- 229920000728 polyester Polymers 0.000 description 68
- 239000011248 coating agent Substances 0.000 description 50
- 238000000576 coating method Methods 0.000 description 50
- 239000000178 monomer Substances 0.000 description 48
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 47
- 238000001556 precipitation Methods 0.000 description 40
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 39
- 150000001875 compounds Chemical class 0.000 description 37
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 35
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 31
- 239000003431 cross linking reagent Substances 0.000 description 27
- 239000002245 particle Substances 0.000 description 27
- 239000012948 isocyanate Substances 0.000 description 24
- 239000000203 mixture Substances 0.000 description 24
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 23
- 239000000243 solution Substances 0.000 description 23
- 229920000642 polymer Polymers 0.000 description 21
- 239000002585 base Substances 0.000 description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 13
- 150000002513 isocyanates Chemical class 0.000 description 13
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 229920005862 polyol Polymers 0.000 description 12
- 238000012545 processing Methods 0.000 description 12
- 229920000877 Melamine resin Polymers 0.000 description 11
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 11
- 150000003077 polyols Chemical class 0.000 description 11
- 230000003405 preventing effect Effects 0.000 description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 10
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 9
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 9
- 125000003504 2-oxazolinyl group Chemical group O1C(=NCC1)* 0.000 description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
- 125000000217 alkyl group Chemical group 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 7
- 229920001577 copolymer Polymers 0.000 description 7
- 238000011282 treatment Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000004970 Chain extender Substances 0.000 description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 150000001718 carbodiimides Chemical class 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000005056 polyisocyanate Substances 0.000 description 6
- 229920001228 polyisocyanate Polymers 0.000 description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 6
- 239000002344 surface layer Substances 0.000 description 6
- 229920002554 vinyl polymer Polymers 0.000 description 6
- 229920000178 Acrylic resin Polymers 0.000 description 5
- 239000004925 Acrylic resin Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000007689 inspection Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 238000006068 polycondensation reaction Methods 0.000 description 5
- 229920001225 polyester resin Polymers 0.000 description 5
- 239000004645 polyester resin Substances 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 5
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000004593 Epoxy Chemical class 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 229920005601 base polymer Polymers 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 4
- 239000001530 fumaric acid Substances 0.000 description 4
- 239000002346 layers by function Substances 0.000 description 4
- 230000000670 limiting effect Effects 0.000 description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 4
- 239000011976 maleic acid Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229920000515 polycarbonate Polymers 0.000 description 4
- 239000004417 polycarbonate Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 4
- MTZUIIAIAKMWLI-UHFFFAOYSA-N 1,2-diisocyanatobenzene Chemical compound O=C=NC1=CC=CC=C1N=C=O MTZUIIAIAKMWLI-UHFFFAOYSA-N 0.000 description 3
- ZXHZWRZAWJVPIC-UHFFFAOYSA-N 1,2-diisocyanatonaphthalene Chemical compound C1=CC=CC2=C(N=C=O)C(N=C=O)=CC=C21 ZXHZWRZAWJVPIC-UHFFFAOYSA-N 0.000 description 3
- VZXPHDGHQXLXJC-UHFFFAOYSA-N 1,6-diisocyanato-5,6-dimethylheptane Chemical compound O=C=NC(C)(C)C(C)CCCCN=C=O VZXPHDGHQXLXJC-UHFFFAOYSA-N 0.000 description 3
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 3
- 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 3
- SXIFAEWFOJETOA-UHFFFAOYSA-N 4-hydroxy-butyl Chemical group [CH2]CCCO SXIFAEWFOJETOA-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 description 3
- OMRDSWJXRLDPBB-UHFFFAOYSA-N N=C=O.N=C=O.C1CCCCC1 Chemical compound N=C=O.N=C=O.C1CCCCC1 OMRDSWJXRLDPBB-UHFFFAOYSA-N 0.000 description 3
- HDONYZHVZVCMLR-UHFFFAOYSA-N N=C=O.N=C=O.CC1CCCCC1 Chemical compound N=C=O.N=C=O.CC1CCCCC1 HDONYZHVZVCMLR-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 3
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 3
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 3
- 239000001361 adipic acid Substances 0.000 description 3
- 235000011037 adipic acid Nutrition 0.000 description 3
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 230000000903 blocking effect Effects 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
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- KIQKWYUGPPFMBV-UHFFFAOYSA-N diisocyanatomethane Chemical compound O=C=NCN=C=O KIQKWYUGPPFMBV-UHFFFAOYSA-N 0.000 description 3
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- 150000002291 germanium compounds Chemical class 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 150000002334 glycols Chemical class 0.000 description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 3
- 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 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 3
- 150000007974 melamines Chemical class 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
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- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
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- 239000004814 polyurethane Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
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- 238000004544 sputter deposition Methods 0.000 description 3
- 150000003440 styrenes Chemical class 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- 150000005846 sugar alcohols Polymers 0.000 description 3
- 150000003609 titanium compounds Chemical class 0.000 description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 3
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 3
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- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
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- 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
- ZGDSDWSIFQBAJS-UHFFFAOYSA-N 1,2-diisocyanatopropane Chemical compound O=C=NC(C)CN=C=O ZGDSDWSIFQBAJS-UHFFFAOYSA-N 0.000 description 2
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- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 2
- LTMRRSWNXVJMBA-UHFFFAOYSA-L 2,2-diethylpropanedioate Chemical compound CCC(CC)(C([O-])=O)C([O-])=O LTMRRSWNXVJMBA-UHFFFAOYSA-L 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 description 2
- IAXFZZHBFXRZMT-UHFFFAOYSA-N 2-[3-(2-hydroxyethoxy)phenoxy]ethanol Chemical compound OCCOC1=CC=CC(OCCO)=C1 IAXFZZHBFXRZMT-UHFFFAOYSA-N 0.000 description 2
- DSKYSDCYIODJPC-UHFFFAOYSA-N 2-butyl-2-ethylpropane-1,3-diol Chemical compound CCCCC(CC)(CO)CO DSKYSDCYIODJPC-UHFFFAOYSA-N 0.000 description 2
- KANZWHBYRHQMKZ-UHFFFAOYSA-N 2-ethenylpyrazine Chemical compound C=CC1=CN=CC=N1 KANZWHBYRHQMKZ-UHFFFAOYSA-N 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
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Landscapes
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Paints Or Removers (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
【解決手段】 ポリエステルフィルムの少なくとも片面に、下引き層と粘着層とを順次設けたフィルムであって、前記下引き層が、スチレン構造および(メタ)アクリル酸構造を有する樹脂を含有することを特徴とする粘着フィルム。
【選択図】 なし
Description
ポリエステル1gを精秤し、フェノール/テトラクロロエタン=50/50(重量比)の混合溶媒100mlを加えて溶解させ、30℃で測定した。
遠心沈降式粒度分布測定装置(株式会社島津製作所社製SA−CP3型)を使用して測定した等価球形分布における積算(重量基準)50%の値を平均粒径とした。
ポリエステル原料を約200mg秤量し、クロロホルム/HFIP(ヘキサフルオロ−2−イソプロパノル)の比率3:2の混合溶媒2mlに溶解させる。溶解後、クロロホルム20mlを追加した後、メタノール10mlを少しずつ加える。沈殿物を濾過により除去し、更に、沈殿物をクロロホルム/メタノールの比率2:1の混合溶媒で洗浄し、濾液・洗浄液を回収し、エバポレーターにより濃縮、その後、乾固させる。乾固物をDMF(ジメチルホルムアミド)25mlに溶解後、この溶液を液体クロマトグラフィー(株式会社島津製作所製「LC−7A」)に供給して、DMF中のエステル環状三量体量を求め、この値をクロロホルム/HFIP混合溶媒に溶解させたポリエステル原料量で割って、含有エステル環状三量体量(重量%)とする。DMF中のエステル環状三量体量は、標準試料ピーク面積と測定試料ピーク面積のピーク面積比より求めた(絶対検量線法)。
移動相A:アセトニトリル
移動相B:2%酢酸水溶液
カラム:三菱化学株式会社製「MCI GEL ODS 1HU」
カラム温度:40℃
流速:1ml/分
検出波長:254nm
(3)の方法で得られたポリエステル原料に含有される含有エステル環状三量体量を基に算出した。
塗布層の表面をRuO4で染色し、エポキシ樹脂中に包埋した。その後、超薄切片法により作成した切片をRuO4で染色し、塗布層断面をTEM(株式会社日立ハイテクノロジーズ製 H−7650、加速電圧100V)を用いて測定した。なお、膜厚は粒子の部分を含まない箇所で測定した。
サンプルの測定面がむき出しとなる状態でケント紙と重ねて固定し、窒素雰囲気下で、180℃で30分間放置して熱処理を行う。
まず粘着層を加工する前のポリエステルフィルムの、本発明の下引き層が設けられた面とは反対側の面に下記塗布剤組成からなる塗布剤を、硬化後の厚さが3μmになるように塗布し、80℃に設定した熱風乾燥式オーブンにて1分間乾燥させた。次いで、紫外線を照射して、硬化させ、ハードコート層を形成した。
《塗布剤組成》
ジペンタエリスリトールヘキサアクリレート80重量部、2−ヒドロキシ−3−フェノキシプロピルアクリレート20重量部、光重合開始剤(商品名:イルガキュア184、チバスペシャルティケミカルズ株式会社製)5重量部、メチルエチルケトン200重量部の混合塗液を使用した。
得られた試料のヘーズをJIS−K−7136に準じ、株式会社村上指色彩技術研究所製ヘーズメーター「HM−150」により、フィルムヘーズを測定した(ヘーズ1)。
次いで、試料の活性エネルギー線硬化樹脂層と反対の面を測定面として、(6)項の方法で加熱した後、上述した方法でヘーズを測定した(ヘーズ2)。
ΔH=(ヘーズ2)−(ヘーズ1)
ΔHが低いほど、高温処理によるエステル環状三量体の析出が少ないことを示し、良好である。
粘着層を加工する前のポリエステルフィルムを空気中、180℃で30分間加熱する。その後、熱処理をした当該フィルムを上部が開いている縦横10cm、高さ3cmになるように、測定面(下引き層)を内面として箱形の形状を作成する。次いで、上記の方法で作成した箱の中にDMFを4ml入れて、3分間放置した後、DMFを回収する。回収したDMFを液体クロマトグラフィー(株式会社島津製作所製:LC−7A)に供給して、DMF中のエステル環状三量体量を求め、この値を、DMFを接触させたフィルム面積で割って、フィルム表面に析出するエステル環状三量体量(mg/m2)とした。なお、DMF中のエステル環状三量体量は上記(3)ポリエステル原料に含有される含有オリゴマー量の測定方法に記載の絶対検量線法に従い算出した。
本発明で得られた粘着フィルムを、窒素雰囲気下、150℃で1時間放置し、熱処理を行った。次いで、80℃で300時間加熱した後、粘着層内に生じた異物を光学顕微鏡下で検査した。検査は、50mm×50mmの面積を、試料の任意の箇所から12箇所選択し、5μm以上の大きさのエステル環状三量体の結晶個数をカウントした。全12箇所の検査範囲のうち、結晶個数が最も多かった2箇所を除き、10箇所の検査範囲内での結晶個数から、以下の基準で判定した。
○:エステル環状三量体の結晶が見つからない
△:エステル環状三量体の結晶が1個以上、3個未満(実用上やや問題になる)
×:エステル環状三量体の結晶が3個以上(実用上問題になる)
本発明で得られた粘着フィルムに対して、粘着層上に辺の長さが20mmになるよう、正方形状の切り傷を付けた。次いで、正方形の中央部をフィルムとは垂直方向から指で押さえた状態で、指を45度回転させた後、粘着層の外観を観察した。観察した外観は以下の基準で判定した。
○:粘着層に変化がない
△:正方形の四つの角の内、1つ剥がれている
×:正方形の四つの角の内、2つ以上剥がれている
<ポリエステル(A)の製造方法>
テレフタル酸ジメチル100重量部とエチレングリコール60重量部とを出発原料とし、触媒として酢酸マグネシウム・四水塩0.09重量部を反応器にとり、反応開始温度を150℃とし、メタノールの留去とともに徐々に反応温度を上昇させ、3時間後に230℃とした。4時間後、実質的にエステル交換反応を終了させた。この反応混合物にエチルアシッドフォスフェート0.04部を添加した後、三酸化アンチモン0.04部を加えて、4時間重縮合反応を行った。すなわち、温度を230℃から徐々に昇温し280℃とした。一方、圧力は常圧より徐々に減じ、最終的には0.3mmHgとした。反応開始後、反応槽の攪拌動力の変化により、極限粘度0.63に相当する時点で反応を停止し、窒素加圧下ポリマーを吐出させた。得られたポリエステル(A)の極限粘度は0.63、エステル環状三量体の含有量は0.97重量%であった。
ポリエステル(A)を、予め160℃で予備結晶化させた後、温度220℃の窒素雰囲気下で固相重合し、極限粘度0.75、エステル環状三量体の含有量が0.46重量%のポリエステル(B)を得た。
テレフタル酸ジメチル100重量部、エチレングリコール60重量部、エチルアシッドフォスフェートを生成ポリエステルに対して30ppm、触媒として酢酸マグネシウム・四水和物を生成ポリエステルに対して100ppmを窒素雰囲気下、260℃でエステル化反応をさせた。引き続いて、テトラブチルチタネートを生成ポリエステルに対して50ppm添加し、2時間30分かけて280℃まで昇温すると共に、絶対圧力0.3kPaまで減圧し、さらに80分、溶融重縮合させ、極限粘度0.61のポリエステル(A)エステル環状三量体の含有量が1.02重量%のポリエステル(C)を得た。
ポリエステル(C)を、予め160℃で予備結晶化させた後、温度210℃の窒素雰囲気下で固相重合し、極限粘度0.72、エステル環状三量体の含有量が0.50重量%のポリエステル(D)を得た。
ポリエステル(A)の製造方法において、エチルアシッドフォスフェート0.04部を添加後、エチレングリコールに分散させた平均粒子径(d50)が1.6μmのシリカ粒子を0.5部、三酸化アンチモン0.04部を加えて、極限粘度0.65に相当する時点で重縮合反応を停止した以外は、ポリエステル1の製造方法と同様の方法を用いてポリエステル(E)を得た。得られたポリエステル(E)は、極限粘度0.65、エステル環状三量体の含有量は0.82重量%であった。
(A1):下記組成で重合したスチレンアクリル共重合体
スチレン/アクリル酸=80/20(モル%)で共重合したスチレンアクリル共重合体。
(A2):下記組成で重合したスチレンアクリル共重合体
スチレン/アクリル酸/ヒドロキシエチルアクリルアミド=70/20/10(モル%)で共重合したスチレンアクリル共重合体
(B1):ヘキサメトキシメチロールメラミン
(B2):オキサゾリン化合物であるエポクロス(株式会社日本触媒製) オキサゾリン基量7.7mmol/g
(B3):オキサゾリン化合物であるエポクロス(株式会社日本触媒製) オキサゾリン基量4.5mmol/g
(B4):ポリグリセロールポリグリシジルエーテル
ヘキサメチレンジイソシアネート1000部を60℃で攪拌し、触媒としてテトラメチルアンモニウム・カプリエート0.1部を加えた。4時間後、リン酸0.2部を添加して反応を停止させ、イソシアヌレート型ポリイソシアネート組成物を得た。得られたイソシアヌレート型ポリイソシアネート組成物100部、数平均分子量400のメトキシポリエチレングリコール42.3部、プロピレングリコールモノメチルエーテルアセテート29.5部を仕込み、80℃で7時間保持した。その後反応液温度を60℃に保持し、イソブタノイル酢酸メチル35.8部、マロン酸ジエチル32.2部、ナトリウムメトキシドの28%メタノール溶液0.88部を添加し、4時間保持した。n−ブタノール58.9部を添加し、反応液温度80℃で2時間保持し、その後、2−エチルヘキシルアシッドホスフェート0.86部を添加して得られたブロックポリイソシアネート
(C1):下記組成で重合したアクリル樹脂の水分散体
エチルアクリレート/n−ブチルアクリレート/メチルメタクリレート/N−メチロールアクリルアミド/アクリル酸=65/21/10/2/2(重量%)の乳化重合体(乳化剤:アニオン系界面活性剤)
(C2):下記組成で重合したスチレン酢酸ビニル共重合体
スチレン/酢酸ビニル/2,2‘−アゾビスイソブチロニトリル=65/35/1(モル%)で共重合したスチレン酢酸ビニル共重合体
(D1):メラミン架橋触媒である、2−アミノ−2−メチルプロパノールハイドロクロライド
(E1):平均粒径0.07μmのシリカ粒子
<粘着剤溶液の調整>
ブチルアクリレート/アクリル酸/2−ヒドロキシエチルアクリレートが重量比で100/6/0.1の共重合体からなる重量平均分子量200万のアクリル系ポリマーの溶液に対して、イソシアネート系架橋剤である日本ポリウレタン工業株式会社製コロネートL、シランカップリング剤である3−グリシドキシプロピルトリメトキシシラン、酢酸エチルを加え、固形分濃度が10%の粘着剤溶液を調製した。溶液中の固形分換算で、アクリル共重合ポリマー/コロネートL/3−グリシドキシプロピルトリメトキシシラン=100/3/0.6とした。
ポリエステル(B)、(E)を重量比で80/20でブレンドしたものを表層、ポリエステル(A)のみのものを中間層の原料として、二台の押出機にそれぞれを供給し、285℃に加熱溶融した後、A層を最外層(表層)、B層を中間層として、2種3層(A/B/A)で厚み構成比がA/B/A=2.5/45/2.5になるよう共押出し、静電密着法を用いて表面温度45℃の鏡面冷却ドラムに密着させながら冷却固化させて、未延伸ポリエチレンテレフタレートフィルムを作成した。このフィルムを85℃の加熱ロール群を通過させながら、ロール周速差を利用して縦方向に3.4倍延伸した後、この縦延伸フィルムの片面に、下記表1に示す水系の塗布液1を塗布し、テンター延伸機に導き、100℃で横方向に4.0倍延伸し、さらに230℃で熱処理を施した後、横方向に2%の弛緩処理を行い、下引き層の膜厚(乾燥後)が0.05μmの下引き層を有するフィルム厚みが50μmの二軸配向ポリエチレンテレフタレートフィルムを得た。さらに、粘着剤溶液を、三菱樹脂株式会社製の離型フィルムMRF38上に、乾燥後の厚さが25μmになるように塗布、乾燥した。この粘着層付きの離型フィルムを、二軸延伸ポリエステルフィルムに貼りあわせて、粘着フィルムを得た。
実施例1において、塗布剤組成を表1および表2に示す塗布剤組成に変更する以外は実施例1と同様にして製造し、粘着フィルムを得た。得られた粘着フィルムは表3に示す特性を有し、加熱処理によるポリエステル表面、および粘着層中へのエステル環状三量体の結晶の析出も抑制され、良好であった。
実施例8において、ポリエステルフィルムの厚みを25μm、厚み構成比をA/B/A=5/15/5に変更した以外は、実施例8と同様の方法で粘着フィルムを得た。得られた粘着フィルムの特性を表3に示す。
実施例8において、ポリエステルフィルムの厚みを125μm、厚み構成比をA/B/A=5/115/5に変更した以外は、実施例8と同様の方法で粘着フィルムを得た。得られた粘着フィルムの特性を表3に示す。
ポリエステル(D)、(E)を重量比で80/20でブレンドしたものを表層、ポリエステル(D)のみのものを中間層の原料として、二台の押出機にそれぞれを供給し、285℃に加熱溶融した後、A層を最外層(表層)、B層を中間層として、2種3層(A/B/A)で厚み構成比がA/B/A=2.5/45/2.5になるよう共押出し、静電密着法を用いて表面温度45℃の鏡面冷却ドラムに密着させながら冷却固化させて、未延伸ポリエチレンテレフタレートフィルムを作成した。このフィルムを85℃の加熱ロール群を通過させながら、ロール周速差を利用して縦方向に3.4倍延伸した後、この縦延伸フィルムの片面に、下記表1に示す水系の塗布液7を塗布し、テンター延伸機に導き、100℃で横方向に4.0倍延伸し、さらに230℃で熱処理を施した後、横方向に2%の弛緩処理を行い、下引き層の膜厚(乾燥後)が0.05μmの下引き層を有するフィルム厚みが50μmの二軸配向ポリエチレンテレフタレートフィルムを得た。なお、粘着層は実施例1と同様にして製造し、粘着フィルムを得た。
実施例8において、粘着層の厚みを5μmに変更した以外は、実施例8と同様の方法で粘着フィルムを得た。得られた粘着フィルムの特性を表3に示す。
実施例1において、塗布剤組成を表1に示す塗布剤組成に変更する以外は実施例1と同様にして製造し、粘着フィルムを得た。得られた粘着フィルムは表3に示す特性を有し、加熱処理によるオリゴマー結晶の析出も抑制され、良好であった。なお、基材であるポリエステルフィルムが粘着層から剥がれにくく、密着性も良好な結果であった。
実施例1において、下引き層を設けないこと以外は実施例1と同様にして製造し、粘着フィルムを得た。でき上がった粘着フィルムを評価したところ、粘着層へのオリゴマー結晶の析出が確認され、密着性も乏しいとなった。
実施例1において、塗布剤組成を表1に示す塗布剤組成に変更する以外は実施例1と同様にして製造し、粘着フィルムを得た。でき上がった粘着フィルムを評価したところ、表3に示すとおり、加熱処理による粘着層へのオリゴマー結晶の析出が確認された。
Claims (1)
- ポリエステルフィルムの少なくとも片面に、下引き層と粘着層とを順次設けたフィルムであって、前記下引き層が、スチレン構造および(メタ)アクリル酸構造を有する樹脂を含有することを特徴とする粘着フィルム。
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