JPWO2017104426A1 - 積層フィルム - Google Patents
積層フィルム Download PDFInfo
- Publication number
- JPWO2017104426A1 JPWO2017104426A1 JP2017519028A JP2017519028A JPWO2017104426A1 JP WO2017104426 A1 JPWO2017104426 A1 JP WO2017104426A1 JP 2017519028 A JP2017519028 A JP 2017519028A JP 2017519028 A JP2017519028 A JP 2017519028A JP WO2017104426 A1 JPWO2017104426 A1 JP WO2017104426A1
- Authority
- JP
- Japan
- Prior art keywords
- meth
- acrylate
- film
- layer
- hard coat
- 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
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- -1 acrylate compound Chemical class 0.000 claims abstract description 103
- 239000000203 mixture Substances 0.000 claims abstract description 76
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims abstract description 57
- 239000011347 resin Substances 0.000 claims abstract description 55
- 229920005989 resin Polymers 0.000 claims abstract description 55
- 239000010419 fine particle Substances 0.000 claims abstract description 42
- 229920006255 plastic film Polymers 0.000 claims abstract description 24
- 239000002985 plastic film Substances 0.000 claims abstract description 24
- 239000004925 Acrylic resin Substances 0.000 claims description 23
- 229920000178 Acrylic resin Polymers 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 229920000193 polymethacrylate Polymers 0.000 claims description 7
- 229920002284 Cellulose triacetate Polymers 0.000 claims description 5
- 239000004793 Polystyrene Substances 0.000 claims description 5
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 claims description 5
- 229920002223 polystyrene Polymers 0.000 claims description 5
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims description 3
- 229920006267 polyester film Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920006289 polycarbonate film Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 170
- 239000010408 film Substances 0.000 description 79
- 239000010410 layer Substances 0.000 description 72
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 36
- 239000000178 monomer Substances 0.000 description 33
- 238000004519 manufacturing process Methods 0.000 description 30
- 239000006087 Silane Coupling Agent Substances 0.000 description 25
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 20
- 239000011324 bead Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 17
- 150000001875 compounds Chemical class 0.000 description 17
- 239000006185 dispersion Substances 0.000 description 17
- 238000000576 coating method Methods 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 14
- 239000000377 silicon dioxide Substances 0.000 description 13
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 12
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- 239000000654 additive Substances 0.000 description 12
- 125000000524 functional group Chemical group 0.000 description 11
- 239000003960 organic solvent Substances 0.000 description 11
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 10
- 239000003999 initiator Substances 0.000 description 10
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 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 9
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 229910002012 Aerosil® Inorganic materials 0.000 description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000003963 antioxidant agent Substances 0.000 description 7
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 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 6
- 239000004593 Epoxy Substances 0.000 description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- OTARVPUIYXHRRB-UHFFFAOYSA-N diethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](C)(OCC)CCCOCC1CO1 OTARVPUIYXHRRB-UHFFFAOYSA-N 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 6
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 239000000412 dendrimer Substances 0.000 description 5
- 229920000736 dendritic polymer Polymers 0.000 description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000010954 inorganic particle Substances 0.000 description 5
- 150000002596 lactones Chemical group 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 125000005702 oxyalkylene group Chemical group 0.000 description 5
- 229920005862 polyol Polymers 0.000 description 5
- 239000012508 resin bead Substances 0.000 description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 4
- 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 4
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 description 4
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 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 4
- DOYKFSOCSXVQAN-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CCO[Si](C)(OCC)CCCOC(=O)C(C)=C DOYKFSOCSXVQAN-UHFFFAOYSA-N 0.000 description 4
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 description 4
- LZMNXXQIQIHFGC-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C(C)=C LZMNXXQIQIHFGC-UHFFFAOYSA-N 0.000 description 4
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 4
- URDOJQUSEUXVRP-UHFFFAOYSA-N 3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C URDOJQUSEUXVRP-UHFFFAOYSA-N 0.000 description 4
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 4
- 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 4
- PRKPGWQEKNEVEU-UHFFFAOYSA-N 4-methyl-n-(3-triethoxysilylpropyl)pentan-2-imine Chemical compound CCO[Si](OCC)(OCC)CCCN=C(C)CC(C)C PRKPGWQEKNEVEU-UHFFFAOYSA-N 0.000 description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 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 description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 4
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 4
- 125000003709 fluoroalkyl group Chemical group 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- 238000007756 gravure coating Methods 0.000 description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material 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
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 description 4
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 4
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 4
- 239000005056 polyisocyanate Substances 0.000 description 4
- 229920001228 polyisocyanate Polymers 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- 239000011342 resin composition Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 description 4
- 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 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 4
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 4
- 239000005050 vinyl trichlorosilane Substances 0.000 description 4
- GJKGAPPUXSSCFI-UHFFFAOYSA-N 2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone Chemical compound CC(C)(O)C(=O)C1=CC=C(OCCO)C=C1 GJKGAPPUXSSCFI-UHFFFAOYSA-N 0.000 description 3
- FDSUVTROAWLVJA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OCC(CO)(CO)COCC(CO)(CO)CO FDSUVTROAWLVJA-UHFFFAOYSA-N 0.000 description 3
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- CQHKDHVZYZUZMJ-UHFFFAOYSA-N [2,2-bis(hydroxymethyl)-3-prop-2-enoyloxypropyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(CO)COC(=O)C=C CQHKDHVZYZUZMJ-UHFFFAOYSA-N 0.000 description 3
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000002216 antistatic agent Substances 0.000 description 3
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- FZUGPQWGEGAKET-UHFFFAOYSA-N parbenate Chemical compound CCOC(=O)C1=CC=C(N(C)C)C=C1 FZUGPQWGEGAKET-UHFFFAOYSA-N 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 239000003504 photosensitizing agent Substances 0.000 description 3
- 229920001225 polyester resin Polymers 0.000 description 3
- 239000004645 polyester resin Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical group C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 2
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 2
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 description 2
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 2
- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 2
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical compound CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 description 2
- SVIQBUBNVYWIDV-UHFFFAOYSA-N 2-methoxy-2-(2-methoxyphenyl)-1-phenylethanone Chemical compound C=1C=CC=C(OC)C=1C(OC)C(=O)C1=CC=CC=C1 SVIQBUBNVYWIDV-UHFFFAOYSA-N 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 2
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- 239000009719 polyimide resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
- MUTNCGKQJGXKEM-UHFFFAOYSA-N tamibarotene Chemical compound C=1C=C2C(C)(C)CCC(C)(C)C2=CC=1NC(=O)C1=CC=C(C(O)=O)C=C1 MUTNCGKQJGXKEM-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- 150000003918 triazines Chemical class 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
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 150000007964 xanthones Chemical class 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Laminated Bodies (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Paints Or Removers (AREA)
- Polarising Elements (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Inorganic Chemistry (AREA)
Abstract
Description
粒子径測定装置:大塚電子株式会社製「ELSZ−2」
粒子径測定サンプル:プライマー用組成物(y)を不揮発分1質量%のメチルイソブチルケトン溶液としたもの。
カラム ; 東ソー株式会社製ガードカラムHXL−H
+東ソー株式会社製 TSKgel G5000HXL
+東ソー株式会社製 TSKgel G4000HXL
+東ソー株式会社製 TSKgel G3000HXL
+東ソー株式会社製 TSKgel G2000HXL
検出器 ; RI(示差屈折計)
データ処理:東ソー株式会社製 SC−8010
測定条件: カラム温度 40℃
溶媒 テトラヒドロフラン
流速 1.0ml/分
標準 ;ポリスチレン
試料 ;樹脂固形分換算で0.4質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(100μl)
カラム ; 東ソー株式会社製ガードカラムHXL−H
+東ソー株式会社製 TSKgel G5000HXL
+東ソー株式会社製 TSKgel G4000HXL
+東ソー株式会社製 TSKgel G3000HXL
+東ソー株式会社製 TSKgel G2000HXL
検出器 ; RI(示差屈折計)
データ処理:東ソー株式会社製 SC−8010
測定条件: カラム温度 40℃
溶媒 テトラヒドロフラン
流速 1.0ml/分
標準 ;ポリスチレン
試料 ;樹脂固形分換算で0.4質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(100μl)
粒子径測定装置:大塚電子株式会社製「ELSZ−2」
粒子径測定サンプル:プライマー用組成物(y)を不揮発分1質量%のメチルイソブチルケトン溶液としたもの。
撹拌装置、冷却管、滴下ロートおよび窒素導入管を備えた反応装置に、メチルイソブチルケトン184質量部を仕込み、撹拌しながら系内温度が110℃になるまで昇温した。次いで、グリシジルメタアクリレート221質量部、メチルメタアクリレート52.5質量部、エチルアクリレート2.8質量部およびt−ブチルパーオキシ−2−エチルヘキサノエート(日本乳化剤株式会社製「パーブチルO」)16.6質量部からなる混合液を3時間かけて滴下ロートより滴下し、110℃で15時間保持した。次いで、90℃まで降温した後、メトキノン0.1質量部およびアクリル酸76質量部を仕込み、トリフェニルホスフィン2.0質量部を添加して、100℃で8時間以上反応させた。溶液酸価が4.2mgKOH/g以下になったことを確認した後、メチルイソブチルケトンで希釈を行い、(メタ)アクリロイル基含有アクリル樹脂(B1−1)のメチルイソブチルケトン溶液910質量部(不揮発分50.0質量%)を得た。(メタ)アクリロイル基含有アクリル樹脂(B1−1)の各性状値は以下のようであった。重量平均分子量(Mw)20,000、理論アクリロイル基当量250g/当量、水酸基価224mgKOH/g
[用いた原料]
・「アエロジルR7200」〔無機微粒子(a)に相当〕:日本アエロジル株式会社製「アエロジルR7200」、一次平均粒子径が12nmであり、粒子表面に(メタ)アクリロイル基を有するシリカ微粒子
・「DPA−600」〔その他の硬化性成分(B’)に相当〕:東亞合成株式会社製「DPA−600」、ジペンタエリスリトールペンタアクリレートとジペンタエリスリトールヘキサアクリレートとをモル比40/60で含有する組成物
[製造方法]
前記「アエロジルR7200」53質量部、製造例1で得た(メタ)アクリロイル基含有アクリル樹脂(B1−1)溶液24質量部(樹脂固形分12質量部)、前記「DPA−600」35質量部、メチルイソブチルケトン188質量部を配合し、不揮発分50質量%のスラリーとしたものを、湿式ボールミル(アシザワ株式会社製「スターミルLMZ015」)を用いて混合分散し、分散体を得た。
得られた分散体に、光重合開始剤(チバスペシャルティケミカルズ社製「イルガキュア#184」)2質量部を加え、更にメチルイソブチルケトンを加えて不揮発分率を40質量%に調製し、プライマー用組成物(y−1)を得た。プライマー用組成物(y−1)中のシリカ微粒子の平均粒子径は125nmであった。
メディア:メジアン径100μmのジルコニアビーズ
ミルの内容積に対する樹脂組成物の充填率:70体積%
攪拌翼の先端部の周速:11m/sec
樹脂組成物の流速:200ml/min
分散時間:50分
[用いた原料]
・「アエロジルR7200」〔無機微粒子(a)に相当〕:日本アエロジル株式会社製「アエロジルR7200」、一次平均粒子径が12nmであり、粒子表面に(メタ)アクリロイル基を有するシリカ微粒子
・「Miramer SP-1106」〔デンドリマー型ポリ(メタ)アクリレート(B2)に相当〕:MIWON社製「Miramer SP-1106」、重量平均分子量(Mw)1,630、一分子あたりの平均(メタ)アクリロイル基数18
・「アロニックスM−404」〔その他の硬化性成分(B’)に相当〕:東亞合成株式会社製「アロニックスM−404」、ジペンタエリスリトールペンタアクリレートとジペンタエリスリトールヘキサアクリレートとを質量比30/70〜40/60で含有する混合物
[製造方法]
前記「アエロジルR7200」50質量部、前記「Miramer SP-1106」20質量部、前記「アロニックスM−404」30質量部、メチルイソブチルケトン80質量部及びプロピレングリコールモノメチルエーテル20質量部を配合し、不揮発分50質量%のスラリーとしたものを、湿式ボールミル(アシザワ株式会社製「スターミルLMZ015」)を用いて混合分散し、分散体を得た。
得られた分散体に、光重合開始剤(チバスペシャルティケミカルズ社製「イルガキュア#184」)2質量部を加え、更にメチルイソブチルケトンを加えて不揮発分率を40質量%に調製し、プライマー用組成物(y−2)を得た。プライマー用組成物(y−2)中のシリカ微粒子の平均粒子径は120nmであった。
メディア:メジアン径100μmのジルコニアビーズ
ミルの内容積に対する樹脂組成物の充填率:70体積%
攪拌翼の先端部の周速:11m/sec
樹脂組成物の流速:200ml/min
分散時間:50分
[用いた原料]
・「デュラネート24A−100」:旭化成ケミカルズ株式会社製「デュラネート24A−100」、ヘキサメチレンジイソシアネートのビウレット変性体、イソシアネート基含有量23.5質量%
・「アロニクスM−306」:東亞合成株式会社製「アロニクスM−306」、ペンタエリスリトールジアクリレート、ペンタエリスリトールトリアクリレート、及びペンタエリスリトールテトラアクリレートをモル比5/70/25で含有する組成物
[製造方法]
撹拌装置を備えた反応装置にヘキサメチレンジイソシアネート60質量部、「デュラネート24A−100」70質量部、ジブチル錫ジラウリート0.2質量部及びメトキノン0.2質量部を加え、攪拌しながら60℃まで昇温した。次いで、「アロニクスM−306」424質量部を10回に分けて10分毎に仕込んだ。更に10時間反応させ、赤外線スペクトルで2250cm−1のイソシアネート基の吸収が消失したことを確認して反応を終了し、(メタ)アクリレート化合物(C−1)を得た。該(メタ)アクリレート化合物(C−1)の各性状値は以下のようであった。重量平均分子量(Mw)9,980、理論アクリロイル基当量130g/当量
[用いた原料]
・「アロニクスMT−3533」:東亞合成株式会社製「アロニクスMT−3533」、ペンタエリスリトールジアクリレート、ペンタエリスリトールトリアクリレート、及びペンタエリスリトールテトラアクリレートをモル比22/52/27で含有する組成物
[製造方法]
撹拌装置を備えた反応装置に1,3−ビス(イソシアナトメチル)シクロヘキサン80質量部、ジブチル錫ジラウリート0.2質量部及びメトキノン0.2質量部を加え、攪拌しながら60℃まで昇温した。次いで、「アロニクスMT−3533」245質量部を10回に分けて10分毎に仕込んだ。更に10時間反応させ、赤外線スペクトルで2250cm−1のイソシアネート基の吸収が消失したことを確認して反応を終了し、(メタ)アクリレート化合物(C−2)を得た。該(メタ)アクリレート化合物(C−2)の各性状値は以下のようであった。重量平均分子量(Mw)2,500、理論アクリロイル基当量135g/当量
[用いた原料]
・「アロニクスM−305」:東亞合成株式会社製「アロニクスM−305」、ペンタエリスリトールトリアクリレートとペンタエリスリトールテトラアクリレートとをモル比60/40で含有する組成物
[製造方法]
撹拌装置を備えた反応装置にヘキサメチレンジイソシアネート80質量部、ジブチル錫ジラウリート0.2質量部及びメトキノン0.2質量部を加え、攪拌しながら60℃まで昇温した。次いで、「アロニクスM−305」520質量部を10回に分けて10分毎に仕込んだ。更に10時間反応させ、赤外線スペクトルで2250cm−1のイソシアネート基の吸収が消失したことを確認して反応を終了し、(メタ)アクリレート化合物(C−3)を得た。該(メタ)アクリレート化合物(C−3)の各性状値は以下のようであった。重量平均分子量(Mw)1,500、理論アクリロイル基当量118g/当量
[用いた原料]
・「MT−3533」〔(メタ)アクリレート化合物(C)に相当〕:東亞合成株式会社製「アロニクスMT−3533」、ペンタエリスリトールジアクリレート、ペンタエリスリトールトリアクリレート、及びペンタエリスリトールテトラアクリレートをモル比22/52/27で含有する組成物
・「DPA−600」〔(メタ)アクリレート化合物(C)に相当〕:東亞合成株式会社製「DPA−600」、ジペンタエリスリトールペンタアクリレートとジペンタエリスリトールヘキサアクリレートとをモル比40/60で含有する組成物
[製造方法]
下記表に示す割合で各成分を配合し、樹脂固形分に対して光重合開始剤(チバスペシャルティケミカルズ社製「イルガキュア#184」)を3質量%添加し、メチルイソブチルケトンを用いて不揮発分を40質量%に調整して、ハードコート用組成物(z−1)〜(z−4)を得た。
下記要領で積層フィルムを製造し、各種評価を行った。結果を表2に示す。
◆積層フィルムの製造
プラスチックフィルム層(X)として厚さ60μmのトリアセチルセルロースフィルムを用い、該トリアセチルセルロースフィルム上に製造例2で得たプライマー用組成物(y−1)を硬化後の膜厚が12μmとなるようにバーコーターで塗布し、70℃で1分乾燥させ、窒素雰囲気下で高圧水銀灯を用いて250mJ/cm2の紫外線を照射し、プライマー層(Y)を設けた。
次いで、プライマー層(Y)上に製造例7で得たハードコート用組成物(z−1)を硬化後の膜厚が3μmとなるようにバーコーターで塗布し、70℃で1分乾燥させ、窒素雰囲気下で高圧水銀灯を用いて250mJ/cm2の紫外線を照射し、ハードコート層(Z)を設けた。
先で得た積層フィルムを10cm四方に切り、4角の水平からの浮きを測定し、その合計値で評価した。
スガ試験機株式会社製「ヘーズコンピュータHZ−2」を用いて積層フィルムのヘーズ値を測定した。
スチールウール(日本スチールウール株式会社製「ボンスター#0000」)0.5gで直径2.4センチメートルの円盤状の圧子を包み、該圧子に1kg重の荷重をかけて、積層フィルムのハードコート層(Z)表面を1000往復させる磨耗試験を行った。磨耗試験前後の積層フィルムのヘーズ値をスガ試験機株式会社製「ヘーズコンピュータHZ−2」を用いて測定し、それらの差の値(dH)で耐擦傷性を評価した。また、摩耗試験後にハードコート層(Z)表面に傷が付いたかどうかを目視で評価した。
JIS K5600−5−4に準拠し、前記積層フィルムのハードコート層(Z)表面の鉛筆硬度を750g荷重条件下で測定した。1つの硬度につき5回測定を行い、傷が付かなかった測定が4回以上あった硬度を積層フィルムの表面硬度とした。
マンドレル試験機(TP技研社製「屈曲試験機」)を用いて前記積層フィルムを試験棒に巻きつけ、クラックが生じるか否かを目視確認する試験を行い、クラックが生じない試験棒の最小径を評価結果とした。試験棒は直径5mmから19mmまで1mm刻みのものを用いた。
プライマー用組成物(y)とハードコート用組成物(z)の種類、及びプライマー層(Y)とハードコート層(Z)の膜厚を表2に示す通りに変更した以外は実施例1と同様にして積層フィルムを製造し、各種評価を行った。結果を表2に示す。
Claims (5)
- プラスチックフィルム層(X)と、プライマー層(Y)と、ハードコート層(Z)とを有する積層フィルムであって、前記プライマー層(Y)が、無機微粒子(A)と重量平均分子量(Mw)が1,000以上である(メタ)アクリロイル基含有樹脂(B)とを必須の成分として含有するプライマー用組成物(y)の硬化物であり、前記ハードコート層(Z)が、(メタ)アクリレート化合物(C)を必須の成分として含有するハードコート用組成物(z)の硬化物であることを特徴とする積層フィルム。
- 前記(メタ)アクリロイル基含有樹脂(B)が(メタ)アクリロイル基含有アクリル樹脂(B1)又はデンドリマー型ポリ(メタ)アクリレート(B2)である請求項1記載の積層フィルム。
- 前記プラスチックフィルム層(X)、プライマー層(Y)、ハードコート層(Z)に加え、更に、光反射防止フィルム層、光拡散フィルム層、偏光フィルム層、透明電極フィルム層の何れかを有する請求項1記載の積層フィルム。
- 前記プライマー用組成物(y)中の無機微粒子(A)の平均粒径が80〜250nmの範囲である請求項1記載の積層フィルム。
- 前記プラスチックフィルム層(X)が、トリアセチルセルロースフィルム、ポリエステルフィルム、アクリルフィルム、シクロオレフィンポリマーフィルム、ポリアミドフィルム、ポリイミドフィルム、ポリスチレンフィルム、ポリカーボネートフィルム、ポリプロピレンフィルムの何れかである請求項1記載の積層フィルム。
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Application Number | Priority Date | Filing Date | Title |
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JP2015245284 | 2015-12-16 | ||
JP2015245284 | 2015-12-16 | ||
PCT/JP2016/085718 WO2017104426A1 (ja) | 2015-12-16 | 2016-12-01 | 積層フィルム |
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