JP6674126B2 - 活性エネルギー線硬化性組成物及びそれを用いたフィルム - Google Patents
活性エネルギー線硬化性組成物及びそれを用いたフィルム Download PDFInfo
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- JP6674126B2 JP6674126B2 JP2015153428A JP2015153428A JP6674126B2 JP 6674126 B2 JP6674126 B2 JP 6674126B2 JP 2015153428 A JP2015153428 A JP 2015153428A JP 2015153428 A JP2015153428 A JP 2015153428A JP 6674126 B2 JP6674126 B2 JP 6674126B2
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- acrylate
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- 239000000203 mixture Substances 0.000 title claims description 59
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 114
- 239000011248 coating agent Substances 0.000 claims description 67
- 238000000576 coating method Methods 0.000 claims description 67
- 150000004706 metal oxides Chemical class 0.000 claims description 54
- 229910044991 metal oxide Inorganic materials 0.000 claims description 53
- 239000006185 dispersion Substances 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- -1 acrylate compound Chemical class 0.000 claims description 30
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 28
- 239000003960 organic solvent Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 10
- 229910001887 tin oxide Inorganic materials 0.000 claims description 10
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000010287 polarization Effects 0.000 claims description 9
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 4
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 3
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 2
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 8
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- 239000002585 base Substances 0.000 description 6
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- 238000003860 storage Methods 0.000 description 6
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 5
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
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- 229910003437 indium oxide Inorganic materials 0.000 description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 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 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000002216 antistatic agent Substances 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 3
- 239000012965 benzophenone Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 125000005843 halogen group Chemical group 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 3
- 239000012788 optical film Substances 0.000 description 3
- 125000005702 oxyalkylene group Chemical group 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
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- VVBLNCFGVYUYGU-UHFFFAOYSA-N 4,4'-Bis(dimethylamino)benzophenone Chemical compound C1=CC(N(C)C)=CC=C1C(=O)C1=CC=C(N(C)C)C=C1 VVBLNCFGVYUYGU-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229920008347 Cellulose acetate propionate Polymers 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
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- 229910008051 Si-OH Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
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- 150000001298 alcohols Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 2
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- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 2
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- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
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- 229920001220 nitrocellulos Polymers 0.000 description 1
- ACLZYRNSDLQOIA-UHFFFAOYSA-N o-tolylthiourea Chemical compound CC1=CC=CC=C1NC(N)=S ACLZYRNSDLQOIA-UHFFFAOYSA-N 0.000 description 1
- OTLDLKLSNZMTTA-UHFFFAOYSA-N octahydro-1h-4,7-methanoindene-1,5-diyldimethanol Chemical compound C1C2C3C(CO)CCC3C1C(CO)C2 OTLDLKLSNZMTTA-UHFFFAOYSA-N 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
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- 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
- 238000010979 pH adjustment Methods 0.000 description 1
- HPAFOABSQZMTHE-UHFFFAOYSA-N phenyl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)C1=CC=CC=C1 HPAFOABSQZMTHE-UHFFFAOYSA-N 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920002454 poly(glycidyl methacrylate) polymer Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
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- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- ZKDDJTYSFCWVGS-UHFFFAOYSA-M sodium;diethoxy-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [Na+].CCOP([S-])(=S)OCC ZKDDJTYSFCWVGS-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- MVQLEZWPIWKLBY-UHFFFAOYSA-N tert-butyl 2-benzoylbenzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1C(=O)C1=CC=CC=C1 MVQLEZWPIWKLBY-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
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical class C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-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
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 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
- QNKXRZAXBKSFQC-UHFFFAOYSA-N trimethoxy-[3-[2-(oxiran-2-ylmethoxy)ethoxy]propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCCOCC1CO1 QNKXRZAXBKSFQC-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- JBCJMTUHAXHILC-UHFFFAOYSA-N zinc;octanoic acid Chemical compound [Zn+2].CCCCCCCC(O)=O JBCJMTUHAXHILC-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
- Paints Or Removers (AREA)
Description
まず、前記金属酸化物微粒子の水分散液を調製する。このときの金属酸化物の微粒子水分散液の濃度は特に制限はないが、通常1〜40質量%の範囲が好ましく、10〜40質量%の範囲がより好ましい。
次いで、濃度調整した導電性を有する金属酸化物微粒子の水分散液に前記一般式(1)で表される加水分解性有機ケイ素化合物を加える。このような加水分解性有機ケイ素化合物としては、例えば、テトラメトキシシラン、テトラエトキシシラン等のテトラアルコキシシラン;メチルトリメトキシシラン、メチルトリエトキシシラン、メチルトリアセトキシシラン、メチルトリプロポキシシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリアセトキシシラン、フェニルトリメトキシシラン、フェニルトリメトキシシラン、フェニルトリエトキシシラン、フェニルトリアセトキシシラン、γ−クロロプロピルトリメトキシシラン、γ−クロロプロピルトリエトキシシラン、γ−クロロプロピルトリプロポキシシラン、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トリエトキシシラン、γ−(β−グリシドキシエトキシ)プロピルトリメトキシシラン、γ−メタクリルオキシ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、γ−メルカプトプロピルトリエトキシシラン等のトリアルコキシシラン又はトリアシルオキシシラン;ジメチルジメトキシシラン、ジメチルジエトキシシラン、フェニルメチルジエトキシシラン、γ−グリシドキシプロピルメチルジメトキシシラン、γ−グリシドキシプロピルフェニルジエトキシシラン、γ−クロロプロピルメチルジメトキシシラン、ジメチルジアセトキシシラン、γ−メタクリルオキシプロピルメチルジメトキシシラン、γ−メルカプトプロピルメチルジメトキシシラン、γ−アミノプロピルメチルジメトキシシラン等のジアルコキシシラン又はジアシルシラン;トリメチルクロロシランなどが挙げられる。これらの加水分解性有機ケイ素化合物は、1種で用いることも2種以上併用することもできる。
錫酸カリウム130質量部及び酒石酸アンチモニルカリウム30質量部を純水400質量部に溶解した溶液を、硝酸アンモニウム1.0質量部及び15質量%アンモニア水12質量部を溶解した純水1,000質量部中に添加した後、60℃で12時間、攪拌しながら加水分解を行った。この加水分解の際に、10質量%硝酸溶液を添加してpH9.0に保った。加水分解によって生成した沈殿物を濾別洗浄した後、再び水に分散させて不揮発分20質量%のアンチモンドープ酸化錫前駆体の水酸化物分散液を調製した。この分散液を温度100℃で噴霧乾燥した。得られた粉体を空気雰囲気下、550℃で2時間加熱処理することによりアンチモンドープ酸化錫粉末を得た。この粉末60質量部を4.3質量%水酸化カリウム水溶液140質量部に分散させ、分散液を30℃に保持しながらサンドミルで3時間粉砕してゾルを調製した。
多官能アクリレート混合物(ジペンタエリスリトールヘキサアクリレート64質量%、ジペンタエリスリトールペンタアクリレート17質量%、ジペンタエリスリトールテトラアクリレート19質量%の混合物)13.7質量部、ウレタンアクリレート(ペンタエリスリトールトリアクリレートとイソホロンジイソシアネートとの反応物)1.5質量部、メチルエチルケトン47.11質量部、エタノール5.28質量部、n−プロパノール0.6質量部、メタノール0.3質量部、ダイアセトンアルコール9.28質量部、光重合開始剤0.4質量部(BASFジャパン株式会社製「イルガキュア184」0.09質量部及びBASFジャパン株式会社製「イルガキュア127」0.31質量部の混合物)を均一に混合した後、製造例1で得られた金属酸化物微粒子(1)の分散液21.63質量部(内訳:金属酸化物(1)4.2質量部、エタノール15.13質量部、イソプロピルアルコール1.62質量部及びメタノール0.68質量部)及びレベリング剤(ビックケミー・ジャパン株式会社製「BYK−UV3576」)0.2質量部を混合して、不揮発分20質量%の活性エネルギー線硬化性組成物(1)を得た。
表1〜4に示した配合に変更した以外は、実施例1と同様に行い、不揮発分20質量%の活性エネルギー線硬化性組成物(2)〜(8)及び(R1)〜(R16)を得た。なお、表1〜4中のエタノール、イソプロピルアルコール及びメタノールの配合量は、製造例1で得られた金属酸化物微粒子(1)の分散液に含まれるものも含んだ量となっている。
上記で得られた活性エネルギー線硬化性組成物の外観を目視で観察し、下記の基準にしたがって塗材外観を評価した。
○:ほぼ白濁なし。
△:やや白濁あり。
×:白濁あり。
上記で得られた活性エネルギー線硬化性組成物の調製直後及び25℃で1日放置後の粘度を、E型粘度計(東機産業株式会社「TV−20型」)を用いて、25℃、100rpm、コーンプレートNo.1(1°34’×R24ロータ)の条件で測定し、下記の基準にしたがって塗材の保存安定性を評価した。
○:1日放置後の粘度増加が2mPa・s以下である。
△:1日放置後の粘度増加が2mPa・sを超えて5mPa・s以下である。
×:1日放置後の粘度増加が5mPa・sを超える。
上記で得られた活性エネルギー線硬化性組成物を、ポリエチレンテレフタレート製フィルム(東洋紡株式会社製「コスモシャインA4100」、厚さ100μm)の易接着処理面上にバーコーターを用いて膜厚2.7μmとなるように塗工して、60℃で90秒間乾燥した後、空気雰囲気下で紫外線照射装置(アイグラフィックス株式会社製「MIDN−042−C1」、ランプ:120W/cm、高圧水銀灯)を用いて、照射光量0.3J/cm2で紫外線を照射し、活性エネルギー線硬化性組成物の硬化塗膜を有するフィルムを評価用サンプルとして得た。
上記で得られた評価用サンプルの硬化塗膜の外観を目視で観察し、下記の基準にしたがって塗膜外観を評価した。
○:ほぼ白化なし。
△:やや白化あり。
×:白化あり。
上記で得られた評価用フィルムを温度23℃、湿度50%RHの環境下で18時間保管後、評価用フィルムの硬化塗膜の表面について、高抵抗率計(株式会社三菱化学アナリテック製「ハイレスタ−UP MCP−HT450」)を用いて、印加電圧500V、測定時間10秒で表面抵抗値を測定した。得られた表面抵抗値から、下記の基準にしたがって帯電防止性を評価した。
○:表面抵抗値が7×108Ω/□以下である。
△:表面抵抗値が7×108Ω/□を超えて、10×108Ω/□以下である。
×:表面抵抗値が10×108Ω/□を超える。
Claims (5)
- 活性エネルギー線硬化性化合物(A)、粒子表面に加水分解性有機ケイ素化合物での処理層を有し導電性を有する金属酸化物(B)、及び有機溶剤(C)を含有する活性エネルギー線硬化性組成物であって、
前記活性エネルギー線硬化性化合物(A)が、ウレタン(メタ)アクリレート(A2)と、前記ウレタン(メタ)アクリレート(A2)以外の多官能(メタ)アクリレート化合物(A1)を含むものであり、
前記有機溶剤(C)が、ダイアセトンアルコール、アセチルアセトン、ジメチルカルビトール及びプロピレングリコールモノメチルエーテルアセテートからなる群から選ばれる少なくとも1種と、メタノール、エタノール、n−プロパノール、イソプロピルアルコール及びメチルエチルケトンからなる群から選ばれる少なくとも1種とを含む混合溶剤であり、
前記混合溶剤のハンセン溶解度パラメータでの分散項(δD)が15.6〜16.1MPa 0.5 の範囲であり、分極項(δP)が7.2〜9.8MPa 0.5 の範囲であり、水素結合項(δH)が8.2〜11.4MPa 0.5 の範囲であることを特徴とする活性エネルギー線硬化性組成物。 - 前記ウレタン(メタ)アクリレート(A2)が、ペンタエリスリトールトリアクリレートと、イソホロンジイソシアネートとの反応物である請求項1記載の活性エネルギー線硬化性組成物。
- 前記金属酸化物(B)が、アンチモンドープ酸化錫である請求項1記載の活性エネルギー線硬化性組成物。
- 前記混合溶剤のハンセン溶解度パラメータでの分散項(δD)が15.6〜16.1MPa 0.5 の範囲であり、分極項(δP)が7.2〜9.6MPa 0.5 の範囲であり、水素結合項(δH)が8.2〜11.4MPa 0.5 の範囲である請求項1記載の活性エネルギー線硬化性組成物。
- 請求項1〜4のいずれか1項記載の活性エネルギー線硬化性組成物の硬化塗膜を有することを特徴とするフィルム。
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